CN115350679B - Device and method for preparing dimethyl carbonate by high-speed jet impact tubular reactor - Google Patents
Device and method for preparing dimethyl carbonate by high-speed jet impact tubular reactor Download PDFInfo
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- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 title claims abstract description 226
- 238000000034 method Methods 0.000 title claims abstract description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 780
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 568
- 239000007788 liquid Substances 0.000 claims abstract description 376
- 238000000926 separation method Methods 0.000 claims abstract description 197
- 238000006243 chemical reaction Methods 0.000 claims abstract description 55
- 238000002156 mixing Methods 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000004821 distillation Methods 0.000 claims description 462
- 238000010992 reflux Methods 0.000 claims description 69
- 229910000831 Steel Inorganic materials 0.000 claims description 68
- 238000012856 packing Methods 0.000 claims description 68
- 239000010959 steel Substances 0.000 claims description 68
- 150000002148 esters Chemical class 0.000 claims description 59
- 230000035800 maturation Effects 0.000 claims description 48
- 239000012530 fluid Substances 0.000 claims description 42
- 239000006200 vaporizer Substances 0.000 claims description 29
- 238000003860 storage Methods 0.000 claims description 26
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 22
- 239000003054 catalyst Substances 0.000 claims description 22
- 238000005809 transesterification reaction Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000005265 energy consumption Methods 0.000 abstract description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 2
- 239000000047 product Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- -1 7-7 Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000739 chaotic effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005381 potential energy Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 101001121408 Homo sapiens L-amino-acid oxidase Proteins 0.000 description 1
- 102100026388 L-amino-acid oxidase Human genes 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000006315 carbonylation Effects 0.000 description 1
- 238000005810 carbonylation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/128—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis
- C07C29/1285—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by alcoholysis of esters of organic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
- C07C68/065—Preparation of esters of carbonic or haloformic acids from organic carbonates from alkylene carbonates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
Description
技术领域Technical Field
本发明属于化工技术领域,具体涉及高速喷流撞击管式反应器制备碳酸二甲酯的装置及方法。The invention belongs to the technical field of chemical industry, and particularly relates to a device and a method for preparing dimethyl carbonate by using a high-speed jet impact tubular reactor.
背景技术Background technique
碳酸二甲酯生产方法一般是光气法、甲醇氧化碳基化法和酯交换法。由于光气法是以剧毒的光气为主要原料,现已基本上淘汰,其余两种方法成为合成DMC的主要方法。联产乙二醇的酯交换法合成DMC技术,近年来得到了很快的发展。碳酸二甲酯制备过程一般采用釜式反应器及机械搅拌,这种制备设备存在的弊端是传热、传质效率低,反应周期长,能耗高,能耗的增加导致成本上升,不利于工业化生产。The production methods of dimethyl carbonate are generally phosgene method, methanol oxidation carbonylation method and ester exchange method. Since the phosgene method uses highly toxic phosgene as the main raw material, it has been basically eliminated, and the other two methods have become the main methods for synthesizing DMC. The technology of synthesizing DMC by ester exchange method with co-production of ethylene glycol has developed rapidly in recent years. The preparation process of dimethyl carbonate generally adopts a kettle reactor and mechanical stirring. The disadvantages of this preparation equipment are low heat and mass transfer efficiency, long reaction cycle, high energy consumption, and increased energy consumption leads to rising costs, which is not conducive to industrial production.
本领域急于寻找一种低能耗、环境友好型制备碳酸二甲酯的工艺及设备,以克服上述技术问题。The art is eager to find a low-energy consumption, environmentally friendly process and equipment for preparing dimethyl carbonate to overcome the above technical problems.
发明内容Summary of the invention
本发明提出高速喷流撞击管式反应器制备碳酸二甲酯的装置及方法,其目的在于解决现有制备碳酸二甲酯的设备和工艺存在传热、传质效率低,反应周期长,能耗高、反应速率和产品收率低等问题。The invention provides a device and a method for preparing dimethyl carbonate by using a high-speed jet impact tubular reactor, and aims to solve the problems of low heat and mass transfer efficiency, long reaction cycle, high energy consumption, low reaction rate and product yield in the existing equipment and process for preparing dimethyl carbonate.
为实现上述目的,本发明采用以下技术方案:To achieve the above object, the present invention adopts the following technical solutions:
高速喷流撞击管式反应器制备碳酸二甲酯的装置,该装置包括依次连通的配料罐、第一高速喷流撞击管式反应器、汽液分离罐、第二高速喷流撞击管式反应器、熟化罐、轻组分分离塔系统、甲醇精馏塔系统和碳酸二甲酯精馏塔系统;同时,配料罐与乙二醇精馏塔系统连通,甲醇精馏塔系统分别与第一高速喷流撞击管式反应器和第二高速喷流撞击管式反应器连通,汽液分离罐与轻组分分离塔系统连通,轻组分分离塔系统与乙二醇精馏塔系统连通。The invention discloses a device for preparing dimethyl carbonate by using a high-speed jet impingement tubular reactor, which comprises a batching tank, a first high-speed jet impingement tubular reactor, a vapor-liquid separation tank, a second high-speed jet impingement tubular reactor, a maturation tank, a light component separation tower system, a methanol distillation tower system and a dimethyl carbonate distillation tower system which are connected in sequence; at the same time, the batching tank is connected to the ethylene glycol distillation tower system, the methanol distillation tower system is connected to the first high-speed jet impingement tubular reactor and the second high-speed jet impingement tubular reactor respectively, the vapor-liquid separation tank is connected to the light component separation tower system, and the light component separation tower system is connected to the ethylene glycol distillation tower system.
进一步的,所述配料罐、汽液分离罐和熟化罐结构一致,均为外周圈设置有热媒,内部设置有机械搅拌器的罐体结构;所述配料罐顶部进液口连接乙二醇精馏塔系统的乙二醇精馏塔塔底泵出口端;配料罐底部出液口通过第一动力流体泵连通第一高速喷流撞击管式反应器的两个第一拉瓦尔喷管的管口;Furthermore, the batching tank, the vapor-liquid separation tank and the maturation tank have the same structure, and are all tank structures with a heat medium arranged on the outer circumference and a mechanical agitator arranged inside; the liquid inlet on the top of the batching tank is connected to the outlet end of the bottom pump of the ethylene glycol distillation tower of the ethylene glycol distillation tower system; the liquid outlet at the bottom of the batching tank is connected to the outlets of the two first Laval nozzles of the first high-speed jet impact tubular reactor through the first power fluid pump;
所述汽液分离罐上端的入口端与第一高速喷流撞击管式反应器的第一管式反应器的出口端连通,汽液分离罐上端的汽体出口端通过分离罐冷凝器与轻组分分离塔系统的汽体入口端连通,汽液分离罐底端的出口端通过第二动力流体泵连通第二高速喷流撞击管式反应器的两个第二拉瓦尔喷管的管口;The inlet end of the upper end of the vapor-liquid separation tank is connected to the outlet end of the first tubular reactor of the first high-speed jet impact tubular reactor, the vapor outlet end of the upper end of the vapor-liquid separation tank is connected to the vapor inlet end of the light component separation tower system through the separation tank condenser, and the outlet end of the bottom end of the vapor-liquid separation tank is connected to the orifices of the two second Laval nozzles of the second high-speed jet impact tubular reactor through the second power fluid pump;
所述熟化罐顶端进液口连接第二高速喷流撞击管式反应器的第二管式反应器出口端,熟化罐的上部溢流口连接轻组分分离塔系统的轻组分分离塔塔釜顶部进液口。The top liquid inlet of the maturation tank is connected to the outlet end of the second tubular reactor of the second high-speed jet impact tubular reactor, and the upper overflow port of the maturation tank is connected to the top liquid inlet of the light component separation tower kettle of the light component separation tower system.
进一步的,所述第一高速喷流撞击管式反应器与第二高速喷流撞击管式反应器结构一致,所述第一高速喷流撞击管式反应器包括第一拉瓦尔喷管、第一混合腔、第一高速喷流撞击腔、第一管式反应器和第一加热器;第一拉瓦尔喷管、第一混合腔、第一高速喷流撞击腔和第一管式反应器均设置在第一加热器内部,两个第一拉瓦尔喷管相向设置并连通,中间连通部位形成的腔体为第一混合腔,第一混合腔中部的垂直方向上连通第一高速喷流撞击腔,第一高速喷流撞击腔连通第一管式反应器的一端,第一管式反应器的另一端连通汽液分离罐顶部进液口,两个第一拉瓦尔喷管的管口处开设有进汽口,进汽口与甲醇精馏塔系统的甲醇汽化器出口端连通;Further, the first high-speed jet impact tubular reactor has the same structure as the second high-speed jet impact tubular reactor, and the first high-speed jet impact tubular reactor includes a first Laval nozzle, a first mixing chamber, a first high-speed jet impact chamber, a first tubular reactor and a first heater; the first Laval nozzle, the first mixing chamber, the first high-speed jet impact chamber and the first tubular reactor are all arranged inside the first heater, the two first Laval nozzles are arranged opposite to each other and connected, and the cavity formed at the middle connecting part is the first mixing chamber, the first high-speed jet impact chamber is connected in the vertical direction of the middle of the first mixing chamber, the first high-speed jet impact chamber is connected to one end of the first tubular reactor, and the other end of the first tubular reactor is connected to the liquid inlet at the top of the vapor-liquid separation tank, and steam inlets are opened at the nozzles of the two first Laval nozzles, and the steam inlets are connected to the outlet end of the methanol vaporizer of the methanol distillation tower system;
第二高速喷流撞击管式反应器包括第二拉瓦尔喷管,第二混合腔,第二高速喷流撞击腔,第二管式反应器,第二加热器;第二拉瓦尔喷管、第二混合腔、第二高速喷流撞击腔和第二管式反应器均设置在第二加热器内部,两个第二拉瓦尔喷管相向设置并连通,中间连通部位形成的腔体为第二混合腔,第二混合腔中部的垂直方向上连通第二高速喷流撞击腔,第二高速喷流撞击腔连通第二管式反应器的一端,第二管式反应器的另一端连通熟化罐顶部的进液口;两个第二拉瓦尔喷管的管口通过第二动力流体泵与汽液分离罐底部的出液口连通,两个第二拉瓦尔喷管的管口处开设有进汽口,进汽口与甲醇精馏塔系统的甲醇汽化器出口端连通。进一步的,第一管式反应器长径比为1000,第二管式反应器长径比为1000。The second high-speed jet impact tubular reactor includes a second Laval nozzle, a second mixing chamber, a second high-speed jet impact chamber, a second tubular reactor, and a second heater; the second Laval nozzle, the second mixing chamber, the second high-speed jet impact chamber, and the second tubular reactor are all arranged inside the second heater, the two second Laval nozzles are arranged opposite to each other and connected, the cavity formed by the middle connecting part is the second mixing chamber, the second high-speed jet impact chamber is connected in the vertical direction of the middle of the second mixing chamber, the second high-speed jet impact chamber is connected to one end of the second tubular reactor, and the other end of the second tubular reactor is connected to the liquid inlet at the top of the maturation tank; the nozzles of the two second Laval nozzles are connected to the liquid outlet at the bottom of the vapor-liquid separation tank through the second power fluid pump, and the nozzles of the two second Laval nozzles are provided with steam inlets, which are connected to the outlet end of the methanol vaporizer of the methanol distillation tower system. Further, the length-to-diameter ratio of the first tubular reactor is 1000, and the length-to-diameter ratio of the second tubular reactor is 1000.
进一步的,所述轻组分分离塔系统包括轻组分分离塔塔釜、轻组分白钢规整填料塔、轻组分冷凝器、轻组分接收罐、轻组分液泵和轻组分分离塔塔底泵;轻组分分离塔塔釜为外周圈设置有热媒的结构,所述轻组分分离塔塔釜顶部进液口与熟化罐的上部溢流口连通,轻组分分离塔塔釜底部的出液口与轻组分分离塔塔底泵的进液口连通,轻组分分离塔塔底泵的出口连通轻组分分离塔塔釜塔釜液回流进液口,轻组分分离塔塔底泵的出口端连接乙二醇精馏塔系统的进液口;轻组分分离塔塔釜上端与轻组分白钢规整填料塔连通并一体设置,轻组分白钢规整填料塔的蒸汽入口端连通分离罐冷凝器的出口端,轻组分白钢规整填料塔的蒸汽出口端连通轻组分冷凝器的入口端,轻组分冷凝器的出口端连通轻组分接收罐的入口端,轻组分接收罐的出口端连通轻组分液泵的出口端,轻组分液泵的出口端连通轻组分白钢规整填料塔上部回流进液口,轻组分液泵的出口端还连通甲醇精馏塔系统进液口。Furthermore, the light component separation tower system includes a light component separation tower kettle, a light component white steel structured packing tower, a light component condenser, a light component receiving tank, a light component liquid pump and a light component separation tower bottom pump; the light component separation tower kettle is a structure with a heat medium arranged on the outer circumference, the liquid inlet at the top of the light component separation tower kettle is connected with the upper overflow port of the maturation tank, the liquid outlet at the bottom of the light component separation tower kettle is connected with the liquid inlet of the light component separation tower bottom pump, the outlet of the light component separation tower bottom pump is connected with the liquid reflux inlet of the light component separation tower kettle, and the outlet end of the light component separation tower bottom pump is connected to the second The liquid inlet of the alcohol distillation tower system; the upper end of the light component separation tower kettle is connected to the light component white steel structured packing tower and is integrally arranged, the steam inlet end of the light component white steel structured packing tower is connected to the outlet end of the separation tank condenser, the steam outlet end of the light component white steel structured packing tower is connected to the inlet end of the light component condenser, the outlet end of the light component condenser is connected to the inlet end of the light component receiving tank, the outlet end of the light component receiving tank is connected to the outlet end of the light component liquid pump, the outlet end of the light component liquid pump is connected to the upper reflux liquid inlet of the light component white steel structured packing tower, and the outlet end of the light component liquid pump is also connected to the liquid inlet of the methanol distillation tower system.
进一步的,所述甲醇精馏塔系统包括甲醇精馏塔再沸器、甲醇精馏塔白钢规整填料塔、甲醇精馏塔冷凝器、甲醇精馏塔共沸液接收罐、甲醇精馏塔共沸液泵、甲醇汽化器和甲醇精馏塔塔底泵;所述甲醇精馏塔系统中部进液口连通轻组分分离塔系统的轻组分液泵出口端还连通碳酸二甲酯精馏塔系统的碳酸二甲酯精馏塔共沸液泵出口端;甲醇精馏塔白钢规整填料塔顶部蒸汽出口连通甲醇精馏塔冷凝器的入口端,甲醇精馏塔冷凝器的出口端连通甲醇精馏塔共沸液接收罐顶部的入口端,甲醇精馏塔共沸液接收罐底部的出口端连通甲醇精馏塔共沸液泵的入口端,甲醇精馏塔共沸液泵的出口端连通甲醇精馏塔白钢规整填料塔上部回流液进液口还连通碳酸二甲酯精馏塔系统中部的进液口;甲醇精馏塔白钢规整填料塔底部出液口连通甲醇精馏塔塔底泵的入口端,甲醇精馏塔塔底泵的出口端连通甲醇精馏塔再沸器入口端,甲醇精馏塔再沸器为设置有热媒的结构,甲醇精馏塔再沸器出口端连通甲醇精馏塔白钢规整填料塔的再沸液回流口;甲醇精馏塔塔底泵的出口端还连通甲醇汽化器入口端,甲醇汽化器入口端还连通新鲜甲醇入口端,甲醇汽化器出口端分别连通第一拉瓦尔喷管和第二拉瓦尔喷管的进汽口。Furthermore, the methanol distillation tower system includes a methanol distillation tower reboiler, a methanol distillation tower white steel structured packing tower, a methanol distillation tower condenser, a methanol distillation tower azeotropic liquid receiving tank, a methanol distillation tower azeotropic liquid pump, a methanol vaporizer and a methanol distillation tower bottom pump; the middle liquid inlet of the methanol distillation tower system is connected to the outlet end of the light component liquid pump of the light component separation tower system and is also connected to the outlet end of the dimethyl carbonate distillation tower azeotropic liquid pump of the dimethyl carbonate distillation tower system; the steam outlet at the top of the methanol distillation tower white steel structured packing tower is connected to the inlet end of the methanol distillation tower condenser, the outlet end of the methanol distillation tower condenser is connected to the inlet end of the top of the methanol distillation tower azeotropic liquid receiving tank, and the outlet end of the bottom of the methanol distillation tower azeotropic liquid receiving tank is connected to the inlet end of the methanol distillation tower azeotropic liquid pump The outlet end of the methanol distillation tower azeotropic liquid pump is connected to the upper reflux liquid inlet of the white steel structured packing tower of the methanol distillation tower and is also connected to the liquid inlet in the middle of the dimethyl carbonate distillation tower system; the bottom liquid outlet of the white steel structured packing tower of the methanol distillation tower is connected to the inlet end of the bottom pump of the methanol distillation tower, and the outlet end of the bottom pump of the methanol distillation tower is connected to the inlet end of the reboiler of the methanol distillation tower. The reboiler of the methanol distillation tower is a structure provided with a heat medium, and the outlet end of the reboiler of the methanol distillation tower is connected to the reboiled liquid reflux port of the white steel structured packing tower of the methanol distillation tower; the outlet end of the bottom pump of the methanol distillation tower is also connected to the inlet end of the methanol vaporizer, and the inlet end of the methanol vaporizer is also connected to the inlet end of fresh methanol, and the outlet end of the methanol vaporizer is respectively connected to the steam inlets of the first Laval nozzle and the second Laval nozzle.
进一步的,所述碳酸二甲酯精馏塔系统包括碳酸二甲酯精馏塔再沸器、碳酸二甲酯精馏塔白钢规整填料塔、碳酸二甲酯精馏塔冷凝器、碳酸二甲酯精馏塔共沸液接收罐、碳酸二甲酯精馏塔共沸液泵、碳酸二甲酯储罐和碳酸二甲酯精馏塔塔底泵;所述碳酸二甲酯精馏塔白钢规整填料塔中部进液口连通甲醇精馏塔共沸液泵的出口端;碳酸二甲酯精馏塔白钢规整填料塔顶部蒸汽出口连通碳酸二甲酯精馏塔冷凝器的入口端,碳酸二甲酯精馏塔冷凝器的出口端连接碳酸二甲酯精馏塔共沸液接收罐顶部的入口端,碳酸二甲酯精馏塔共沸液接收罐底部的出口端连通碳酸二甲酯精馏塔共沸液泵的入口端,碳酸二甲酯精馏塔共沸液泵的出口端连通碳酸二甲酯精馏塔白钢规整填料塔上部回流液进液口,碳酸二甲酯精馏塔共沸液泵的出口端还连通甲醇精馏塔系统中部的进液口;碳酸二甲酯精馏塔白钢规整填料塔底部出液口连通碳酸二甲酯精馏塔塔底泵的入口端,碳酸二甲酯精馏塔塔底泵的出口端连通碳酸二甲酯精馏塔再沸器入口端,碳酸二甲酯精馏塔再沸器为设置有热媒的结构,碳酸二甲酯精馏塔再沸器出口端连通碳酸二甲酯精馏塔白钢规整填料塔再沸液回流口;碳酸二甲酯精馏塔塔底泵的出口端还连接碳酸二甲酯储罐顶部入口端。Furthermore, the dimethyl carbonate distillation tower system comprises a dimethyl carbonate distillation tower reboiler, a dimethyl carbonate distillation tower white steel structured packing tower, a dimethyl carbonate distillation tower condenser, a dimethyl carbonate distillation tower azeotropic liquid receiving tank, a dimethyl carbonate distillation tower azeotropic liquid pump, a dimethyl carbonate storage tank and a dimethyl carbonate distillation tower bottom pump; the liquid inlet in the middle of the dimethyl carbonate distillation tower white steel structured packing tower is connected to the outlet end of the azeotropic liquid pump of the methanol distillation tower; the steam outlet at the top of the white steel structured packing tower of the dimethyl carbonate distillation tower is connected to the inlet end of the dimethyl carbonate distillation tower condenser, the outlet end of the dimethyl carbonate distillation tower condenser is connected to the inlet end of the top of the dimethyl carbonate distillation tower azeotropic liquid receiving tank, and the outlet end at the bottom of the dimethyl carbonate distillation tower azeotropic liquid receiving tank is connected to the dimethyl carbonate distillation tower azeotropic liquid receiving tank. The inlet end of the azeotropic liquid pump of the ester distillation tower and the outlet end of the azeotropic liquid pump of the dimethyl carbonate distillation tower are connected to the reflux liquid inlet of the upper part of the white steel structured packing tower of the dimethyl carbonate distillation tower, and the outlet end of the azeotropic liquid pump of the dimethyl carbonate distillation tower is also connected to the liquid inlet in the middle of the methanol distillation tower system; the bottom liquid outlet of the white steel structured packing tower of the dimethyl carbonate distillation tower is connected to the inlet end of the bottom pump of the dimethyl carbonate distillation tower, and the outlet end of the bottom pump of the dimethyl carbonate distillation tower is connected to the inlet end of the reboiler of the dimethyl carbonate distillation tower, the reboiler of the dimethyl carbonate distillation tower is a structure provided with a heat medium, and the outlet end of the reboiler of the dimethyl carbonate distillation tower is connected to the reboiled liquid reflux port of the white steel structured packing tower of the dimethyl carbonate distillation tower; the outlet end of the bottom pump of the dimethyl carbonate distillation tower is also connected to the top inlet end of the dimethyl carbonate storage tank.
进一步的,所述乙二醇精馏塔系统包括乙二醇精馏塔再沸器、乙二醇精馏塔白钢规整填料塔、乙二醇精馏塔冷凝器、乙二醇接收罐、乙二醇泵、乙二醇储罐和乙二醇精馏塔塔底泵;所述乙二醇精馏塔系统中部进液口连通轻组分分离塔塔底泵的出口端;乙二醇精馏塔白钢规整填料塔顶部蒸汽出口连通乙二醇精馏塔冷凝器的入口端,乙二醇精馏塔冷凝器的出口端连通乙二醇接收罐顶部的入口端,乙二醇接收罐底部的出口端连通乙二醇泵的入口端,乙二醇泵的出口端连通乙二醇精馏塔白钢规整填料塔上部回流液进液口,乙二醇泵的出口端还连通乙二醇储罐顶部入口端;乙二醇精馏塔白钢规整填料塔底部出液口连通乙二醇精馏塔塔底泵的入口端,乙二醇精馏塔塔底泵的出口端连通乙二醇精馏塔再沸器入口端,乙二醇精馏塔再沸器为设置有热媒的结构,乙二醇精馏塔再沸器出口端连通乙二醇精馏塔白钢规整填料塔再沸液回流口;乙二醇精馏塔塔底泵的出口端还连通配料罐顶部入口端。Furthermore, the ethylene glycol distillation tower system includes an ethylene glycol distillation tower reboiler, an ethylene glycol distillation tower white steel structured packing tower, an ethylene glycol distillation tower condenser, an ethylene glycol receiving tank, an ethylene glycol pump, an ethylene glycol storage tank and an ethylene glycol distillation tower bottom pump; the middle liquid inlet of the ethylene glycol distillation tower system is connected to the outlet end of the light component separation tower bottom pump; the steam outlet at the top of the ethylene glycol distillation tower white steel structured packing tower is connected to the inlet end of the ethylene glycol distillation tower condenser, the outlet end of the ethylene glycol distillation tower condenser is connected to the inlet end of the top of the ethylene glycol receiving tank, and the outlet end at the bottom of the ethylene glycol receiving tank is connected to the inlet end of the ethylene glycol pump. The outlet end of the ethylene glycol pump is connected to the reflux liquid inlet of the upper part of the white steel structured packing tower of the ethylene glycol distillation tower, and the outlet end of the ethylene glycol pump is also connected to the top inlet end of the ethylene glycol storage tank; the bottom liquid outlet of the white steel structured packing tower of the ethylene glycol distillation tower is connected to the inlet end of the bottom pump of the ethylene glycol distillation tower, and the outlet end of the bottom pump of the ethylene glycol distillation tower is connected to the inlet end of the reboiler of the ethylene glycol distillation tower. The reboiler of the ethylene glycol distillation tower is a structure provided with a heat medium, and the outlet end of the reboiler of the ethylene glycol distillation tower is connected to the reboiled liquid reflux port of the white steel structured packing tower of the ethylene glycol distillation tower; the outlet end of the bottom pump of the ethylene glycol distillation tower is also connected to the top inlet end of the batching tank.
一种高速喷流撞击管式反应器制备碳酸二甲酯的装置的方法,具体包括如下步骤:A method for preparing dimethyl carbonate by using a high-speed jet impinging tubular reactor comprises the following steps:
步骤1.原料碳酸乙烯酯、催化剂进入到配料罐内搅拌混合均匀得到混合液,催化剂用量为碳酸乙烯酯质量的0.15%~0.25%;混合液在热媒的加热下达到反应温度,通过第一动力流体泵连续进入到第一高速喷流撞击管式反应器;Step 1. The raw material ethylene carbonate and the catalyst are put into a batching tank and stirred and mixed to obtain a mixed liquid, wherein the amount of the catalyst is 0.15% to 0.25% of the mass of the ethylene carbonate; the mixed liquid reaches the reaction temperature under the heating of the heat medium, and continuously enters the first high-speed jet impact tubular reactor through the first power fluid pump;
步骤2.配料罐的混合液通过动力流体泵泵入两个相向的第一拉瓦尔喷管,同时吸入甲醇蒸汽,甲醇与碳酸乙烯酯的摩尔比为4~4.4:1,两股从第一拉瓦尔管喷出的高速喷流,在高速喷流撞击腔中相互撞击,然后进入第一管式反应器进行酯交换反应得到碳酸二甲酯蒸汽与酯交换液,甲醇蒸汽、反应生成的碳酸二甲酯蒸汽与酯交换液连续进入到汽液分离罐;Step 2. The mixed liquid in the batching tank is pumped into two opposing first Laval nozzles through a power fluid pump, and methanol vapor is sucked in at the same time. The molar ratio of methanol to ethylene carbonate is 4 to 4.4:1. The two high-speed jets ejected from the first Laval tube collide with each other in the high-speed jet impact chamber, and then enter the first tubular reactor for ester exchange reaction to obtain dimethyl carbonate vapor and ester exchange liquid. The methanol vapor, dimethyl carbonate vapor generated by the reaction, and the ester exchange liquid continuously enter the vapor-liquid separation tank;
步骤3.汽液分离罐将甲醇蒸汽、反应生成的碳酸二甲酯蒸汽与酯交换液分离,分离出的甲醇蒸汽和反应生成的碳酸二甲酯蒸汽进入到轻组分分离塔系统;分离出轻组分的酯交换液通过第二动力流体泵连续进入到第二高速喷流撞击管式反应器;Step 3. The vapor-liquid separation tank separates the methanol vapor, the dimethyl carbonate vapor generated by the reaction and the transesterification liquid, and the separated methanol vapor and the dimethyl carbonate vapor generated by the reaction enter the light component separation tower system; the transesterification liquid with the separated light component continuously enters the second high-speed jet impact tubular reactor through the second power fluid pump;
步骤4.汽液分离罐中的酯交换液通过第二动力流体泵泵入两个相向的第二拉瓦尔喷管,同时吸入甲醇蒸汽,甲醇的添加量与步骤2中一致,两股从第二拉瓦尔管喷出的高速喷流,在高速喷流撞击腔中相互撞击,然后进入第二管式反应器进行酯交换反应,从第二高速喷流撞击管式反应器出来的甲醇蒸汽、反应生成的碳酸二甲酯蒸汽与酯交换液连续进入到熟化罐;Step 4. The transesterification liquid in the vapor-liquid separation tank is pumped into two opposing second Laval nozzles through a second power fluid pump, and methanol vapor is sucked in at the same time. The amount of methanol added is the same as that in step 2. The two high-speed jets ejected from the second Laval tubes collide with each other in the high-speed jet impact chamber, and then enter the second tubular reactor for transesterification reaction. The methanol vapor from the second high-speed jet impact tubular reactor, the dimethyl carbonate vapor generated by the reaction, and the transesterification liquid continuously enter the maturation tank;
步骤5.酯交换液在熟化罐里继续进行补充酯交换反应;从熟化罐里溢流出来的熟化液进入到轻组分分离塔系统;Step 5. The ester exchange liquid continues to undergo supplementary ester exchange reaction in the aging tank; the aging liquid overflowing from the aging tank enters the light component separation tower system;
步骤6.来自汽液分离罐的甲醇蒸汽和反应生成的碳酸二甲酯蒸汽和熟化罐的熟化液连续进入到轻组分分离塔系统,轻组分分离塔系统分离出的轻组分汽体经冷凝器冷凝进入轻组分液接收罐,轻组分分离塔系统分离出的轻组分液部分作为轻组分分离塔系统的回流,部分进入到甲醇精馏塔系统;轻组分分离塔系统的塔釜液通过分离塔塔底泵连续进入到乙二醇精馏塔系统;Step 6. The methanol vapor from the vapor-liquid separation tank, the dimethyl carbonate vapor generated by the reaction, and the mature liquid from the mature tank continuously enter the light component separation tower system, the light component vapor separated by the light component separation tower system is condensed by the condenser and enters the light component liquid receiving tank, part of the light component liquid separated by the light component separation tower system is used as the reflux of the light component separation tower system, and part of it enters the methanol distillation tower system; the bottom liquid of the light component separation tower system continuously enters the ethylene glycol distillation tower system through the bottom pump of the separation tower;
步骤7.来自轻组分分离塔系统的轻组分液及来自碳酸二甲酯精馏塔共沸液接收罐的共沸液连续进入到甲醇精馏塔系统,甲醇精馏塔系统塔顶分离出的共沸物蒸汽经甲醇精馏塔冷凝器冷凝进入到共沸液接收罐得到共沸液,部分作为甲醇精馏塔系统的回流,部分进入到碳酸二甲酯精馏塔系统;甲醇精馏塔系统塔釜液经甲醇精馏塔塔底泵进入到甲醇汽化器,汽化的甲醇继续用于酯交换反应;Step 7. The light component liquid from the light component separation tower system and the azeotropic liquid from the azeotropic liquid receiving tank of the dimethyl carbonate distillation tower continuously enter the methanol distillation tower system, the azeotropic vapor separated from the top of the methanol distillation tower system is condensed by the methanol distillation tower condenser and enters the azeotropic liquid receiving tank to obtain the azeotropic liquid, part of which is used as the reflux of the methanol distillation tower system, and part of which enters the dimethyl carbonate distillation tower system; the bottom liquid of the methanol distillation tower system enters the methanol vaporizer through the bottom pump of the methanol distillation tower, and the vaporized methanol is continuously used for the transesterification reaction;
步骤8.来自甲醇精馏塔系统共沸液接收罐的共沸液连续进入到碳酸二甲酯精馏塔系统,碳酸二甲酯精馏塔系统塔顶分离出的共沸物蒸汽经碳酸二甲酯精馏塔冷凝器冷凝进入到碳酸二甲酯精馏塔共沸液接收罐得到共沸液,部分作为碳酸二甲酯精馏塔系统的回流,部分作为进料返回到甲醇精馏塔系统;碳酸二甲酯精馏塔系统塔釜液经碳酸二甲酯精馏塔塔底泵进入到碳酸二甲酯储罐;Step 8. The azeotropic liquid from the azeotropic liquid receiving tank of the methanol distillation tower system continuously enters the dimethyl carbonate distillation tower system, the azeotropic product vapor separated from the top of the dimethyl carbonate distillation tower system is condensed by the dimethyl carbonate distillation tower condenser and enters the azeotropic liquid receiving tank of the dimethyl carbonate distillation tower to obtain the azeotropic liquid, part of which is used as reflux of the dimethyl carbonate distillation tower system, and part of which is returned to the methanol distillation tower system as feed; the bottom liquid of the dimethyl carbonate distillation tower system enters the dimethyl carbonate storage tank through the bottom pump of the dimethyl carbonate distillation tower;
步骤9.来自轻组分分离塔系统的塔釜液连续进入到乙二醇精馏塔系统,乙二醇精馏塔系统塔顶分离出的乙二醇蒸汽经乙二醇精馏塔冷凝器冷凝进入到乙二醇接收罐得到乙二醇,部分作为乙二醇精馏塔系统的回流,部分进料进入到乙二醇储罐;乙二醇精馏塔系统的塔釜液经乙二醇精馏塔塔底泵部分进入乙二醇精馏塔再沸器加热后返回乙二醇精馏塔系统,部分作为回收催化剂连续进入到配料罐。Step 9. The bottom liquid from the light component separation tower system continuously enters the ethylene glycol distillation tower system, and the ethylene glycol vapor separated from the top of the ethylene glycol distillation tower system is condensed by the ethylene glycol distillation tower condenser and enters the ethylene glycol receiving tank to obtain ethylene glycol, part of which is used as reflux of the ethylene glycol distillation tower system, and part of which is fed into the ethylene glycol storage tank; the bottom liquid of the ethylene glycol distillation tower system is partially pumped into the ethylene glycol distillation tower reboiler for heating and then returned to the ethylene glycol distillation tower system, and part of which is continuously entered into the batching tank as a recovered catalyst.
进一步的,步骤1中配料罐内温度为70℃~75℃,压力为常压,物料的停留时间为0.5h~0.75h;Furthermore, in step 1, the temperature in the batching tank is 70°C to 75°C, the pressure is normal pressure, and the residence time of the material is 0.5h to 0.75h;
步骤2中第一高速喷流撞击管式反应器内温度为80℃~85℃,压力为0.2MPa~0.25MPa;In step 2, the temperature in the first high-speed jet impact tubular reactor is 80° C. to 85° C., and the pressure is 0.2 MPa to 0.25 MPa;
步骤3中汽液分离罐内温度为70℃~75℃,压力为常压,物料的停留时间为0.5h~0.75h;In step 3, the temperature in the vapor-liquid separation tank is 70°C to 75°C, the pressure is normal pressure, and the residence time of the material is 0.5h to 0.75h;
步骤4中第二高速喷流撞击管式反应器内温度为80℃~85℃,压力为0.2MPa~0.25MPa:In step 4, the temperature in the second high-speed jet impact tubular reactor is 80° C. to 85° C., and the pressure is 0.2 MPa to 0.25 MPa:
步骤5中熟化罐内温度为80℃~85℃,压力为0.2MPa~0.25MPa,物料的停留时间为1.5h~2h;In step 5, the temperature in the aging tank is 80°C to 85°C, the pressure is 0.2MPa to 0.25MPa, and the residence time of the material is 1.5h to 2h;
步骤6中轻组分分离塔系统塔釜温度为75℃~78℃,塔顶温度为64℃~66℃,回流比为3~4,压力为常压;In step 6, the kettle temperature of the light component separation tower system is 75°C to 78°C, the tower top temperature is 64°C to 66°C, the reflux ratio is 3 to 4, and the pressure is normal pressure;
步骤7中甲醇精馏塔系统塔底温度为70℃,塔底压力为0.13MPa;塔顶温度为64℃,塔顶压力为常压,回流比为2;In step 7, the bottom temperature of the methanol distillation tower system is 70° C., the bottom pressure is 0.13 MPa; the top temperature is 64° C., the top pressure is normal pressure, and the reflux ratio is 2;
步骤8中碳酸二甲酯精馏塔系统塔底温度为183℃,塔底压力为1.33MPa;塔顶温度为147℃,塔顶压力为1.30MPa,回流比为1.2;In step 8, the bottom temperature of the dimethyl carbonate distillation tower system is 183° C., the bottom pressure is 1.33 MPa; the top temperature is 147° C., the top pressure is 1.30 MPa, and the reflux ratio is 1.2;
步骤9中乙二醇精馏塔系统塔顶温度为150℃,塔顶压力为0.02MPa;塔底温度为178℃,回流比为1.5。In step 9, the top temperature of the ethylene glycol distillation tower system is 150° C., and the top pressure is 0.02 MPa; the bottom temperature is 178° C., and the reflux ratio is 1.5.
本发明的高速喷流撞击管式反应器制备碳酸二甲酯的装置及方法,与现有技术相比,有益效果为:Compared with the prior art, the device and method for preparing dimethyl carbonate by using a high-speed jet impingement tubular reactor of the present invention have the following beneficial effects:
1、采用高速喷流撞击管式反应器进行酯交换反应,两股非均相流体相向高速流动,通过撞击形成一个高度湍动的撞击区,撞击流有效改善了反应器内的混合及传质效果,提高了反应速率和产品收率;1. The high-speed jet impact tubular reactor is used for transesterification reaction. Two heterogeneous fluids flow toward each other at high speed, forming a highly turbulent impact zone through impact. The impact flow effectively improves the mixing and mass transfer effect in the reactor, and increases the reaction rate and product yield.
2、缩短了反应时间,节能,提高了生产效率,绿色环保,环境友好;2. Shortened the reaction time, saved energy, improved production efficiency, green and environmentally friendly;
3、本装置在生产碳酸二甲酯的同时副产乙二醇,提高了装置的经济效益;3. This device produces ethylene glycol as a by-product while producing dimethyl carbonate, which improves the economic benefits of the device;
4、碳酸二甲酯收率大于95%,碳酸二甲酯质量优于工业级国标;本发明工艺成熟,设备先进,连续操作,自动化程度高。4. The yield of dimethyl carbonate is greater than 95%, and the quality of dimethyl carbonate is better than the national industrial standard; the process of the present invention is mature, the equipment is advanced, the operation is continuous, and the degree of automation is high.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1为本发明高速喷流撞击管式反应器制备碳酸二甲酯的装置示意图;FIG1 is a schematic diagram of a device for preparing dimethyl carbonate using a high-speed jet impingement tubular reactor according to the present invention;
附图标记:1、配料罐,1-1、机械搅拌器,1-2、第一动力流体泵;2、第一高速喷流撞击管式反应器,2-1、第一拉瓦尔喷管,2-2、混合腔,2-3、第一高速喷流撞击腔,2-4、第一管式反应器,2-5、第一加热器;3、汽液分离罐,3-1、分离罐机械搅拌器,3-2、分离罐冷凝器,3-3、第二动力流体泵;4、第二高速喷流撞击管式反应器,4-1、第二拉瓦尔喷管,4-2、混合腔,4-3、第二高速喷流撞击腔,4-4、第二管式反应器,4-5、第二加热器;5、熟化罐,5-1、熟化罐机械搅拌器;6、轻组分分离塔,6-1、轻组分分离塔塔釜,6-2、轻组分白钢规整填料,6-3、轻组分冷凝器,6-4、轻组分接收罐,6-5、轻组分液泵,6-6、轻组分分离塔塔底泵;7、甲醇精馏塔,7-1、甲醇精馏塔再沸器,7-2、甲醇精馏塔白钢规整填料,7-3、甲醇精馏塔冷凝器,7-4、甲醇精馏塔共沸液接收罐,7-5、甲醇精馏塔共沸液泵,7-6、甲醇汽化器,7-7、甲醇精馏塔塔底泵;8、碳酸二甲酯精馏塔,8-1、碳酸二甲酯精馏塔再沸器,8-2、碳酸二甲酯精馏塔白钢规整填料,8-3、碳酸二甲酯精馏塔冷凝器,8-4、碳酸二甲酯精馏塔共沸液接收罐,8-5、碳酸二甲酯精馏塔共沸液泵,8-6、碳酸二甲酯储罐,8-7、碳酸二甲酯精馏塔塔底泵;9、乙二醇精馏塔,9-1、乙二醇精馏塔再沸器,9-2、乙二醇精馏塔白钢规整填料,9-3、乙二醇精馏塔冷凝器,9-4、乙二醇接收罐,9-5、乙二醇泵,9-6、乙二醇储罐,9-7、乙二醇精馏塔塔底泵。Figure numerals: 1, batching tank, 1-1, mechanical stirrer, 1-2, first power fluid pump; 2, first high-speed jet impact tubular reactor, 2-1, first Laval nozzle, 2-2, mixing chamber, 2-3, first high-speed jet impact chamber, 2-4, first tubular reactor, 2-5, first heater; 3, vapor-liquid separation tank, 3-1, separation tank mechanical stirrer, 3-2, separation tank condenser, 3-3, second power fluid pump; 4, second high-speed jet impact tubular reactor reactor, 4-1, second Laval nozzle, 4-2, mixing chamber, 4-3, second high-speed jet impact chamber, 4-4, second tubular reactor, 4-5, second heater; 5, maturation tank, 5-1, maturation tank mechanical agitator; 6, light component separation tower, 6-1, light component separation tower kettle, 6-2, light component white steel structured packing, 6-3, light component condenser, 6-4, light component receiving tank, 6-5, light component liquid pump, 6-6, light component separation tower bottom pump; 7, Methanol distillation tower, 7-1, methanol distillation tower reboiler, 7-2, methanol distillation tower white steel structured packing, 7-3, methanol distillation tower condenser, 7-4, methanol distillation tower azeotropic liquid receiving tank, 7-5, methanol distillation tower azeotropic liquid pump, 7-6, methanol vaporizer, 7-7, methanol distillation tower bottom pump; 8, dimethyl carbonate distillation tower, 8-1, dimethyl carbonate distillation tower reboiler, 8-2, dimethyl carbonate distillation tower white steel structured packing, 8-3, dimethyl carbonate distillation tower condenser , 8-4, azeotropic liquid receiving tank for dimethyl carbonate distillation tower, 8-5, azeotropic liquid pump for dimethyl carbonate distillation tower, 8-6, dimethyl carbonate storage tank, 8-7, bottom pump for dimethyl carbonate distillation tower; 9, ethylene glycol distillation tower, 9-1, reboiler for ethylene glycol distillation tower, 9-2, white steel structured packing for ethylene glycol distillation tower, 9-3, condenser for ethylene glycol distillation tower, 9-4, ethylene glycol receiving tank, 9-5, ethylene glycol pump, 9-6, ethylene glycol storage tank, 9-7, bottom pump for ethylene glycol distillation tower.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.
针对工程问题和市场需求,为了克服现有技术中存在的问题,本发明提供一种工艺成熟,连续操作,自动化程度高,反应器技术先进,反应效率高,节能、环境友好;采用先进的高速喷流撞击管式反应器进行酯交换反应,由于混合液经拉瓦尔管高速喷出,会在汽体吸入口产生负压区,致使汽体被吸入,并在负压区迅速膨胀并被动力流体打成微小气泡,进入混合腔;此时,在混合腔中,汽体、液体在混合腔中充分混合,并且由于能量交换而加速排出,速度可以达到音速,混合液的势能增加到最大,更加强了传质、传热的效果;两股流体相向高速流动,通过撞击形成一个高度湍动的撞击区,大大强化了过程热、质传递;撞击流其强烈的微观混合以及压力波动特性可以使化学反应快速进行,瞬间产生有效均匀的过饱和度;而且由于混沌流动状态使混合尺度迅速减小,不同尺度漩涡及彼此折叠碰撞增强了湍动强度和能量扩散,促使分子在发生化学反应时达到更有效的高能级碰撞,撞击流强化了传热、传质,提高了反应速率和产品收率,制备的碳酸二甲酯质量高于工业级国标,提高了反应速率和产品收率。In view of engineering problems and market demands, in order to overcome the problems existing in the prior art, the present invention provides a method with mature process, continuous operation, high degree of automation, advanced reactor technology, high reaction efficiency, energy saving and environmental friendliness; an advanced high-speed jet impact tubular reactor is adopted for ester exchange reaction, and since the mixed liquid is ejected at high speed through the Laval tube, a negative pressure zone will be generated at the gas suction port, causing the gas to be sucked in, and rapidly expand in the negative pressure zone and be beaten into tiny bubbles by the power fluid, and enter the mixing chamber; at this time, in the mixing chamber, the gas and liquid are fully mixed in the mixing chamber, and are accelerated to be discharged due to energy exchange, and the speed can reach the speed of sound, and the potential energy of the mixed liquid is increased to the maximum, which is more The mass transfer and heat transfer effects are enhanced; two fluids flow towards each other at high speed, and a highly turbulent collision zone is formed through collision, which greatly enhances the process heat and mass transfer; the strong microscopic mixing and pressure fluctuation characteristics of the impact flow can make the chemical reaction proceed rapidly and instantly produce effective and uniform supersaturation; and because the chaotic flow state rapidly reduces the mixing scale, vortices of different scales and folding collisions with each other enhance the turbulence intensity and energy diffusion, prompting molecules to reach more effective high-energy level collisions when chemical reactions occur. The impact flow enhances heat and mass transfer, improves the reaction rate and product yield, and the quality of the prepared dimethyl carbonate is higher than the industrial grade national standard, which improves the reaction rate and product yield.
如图1所示,高速喷流撞击管式反应器制备碳酸二甲酯的装置,包括依次连通的配料罐1、第一高速喷流撞击管式反应器2、汽液分离罐3、第二高速喷流撞击管式反应器4、熟化罐5、轻组分分离塔系统6、甲醇精馏塔系统7和碳酸二甲酯精馏塔系统8;同时,配料罐1还与乙二醇精馏塔系统9连通,甲醇精馏塔系统7还分别与第一高速喷流撞击管式反应器2和第二高速喷流撞击管式反应器4连通,汽液分离罐3还与轻组分分离塔系统6连通,轻组分分离塔系统6还与乙二醇精馏塔系统9连通。As shown in Figure 1, the device for preparing dimethyl carbonate by using a high-speed jet impinging tubular reactor comprises a batching tank 1, a first high-speed jet impinging tubular reactor 2, a vapor-liquid separation tank 3, a second high-speed jet impinging tubular reactor 4, a maturation tank 5, a light component separation tower system 6, a methanol distillation tower system 7 and a dimethyl carbonate distillation tower system 8 which are connected in sequence; at the same time, the batching tank 1 is also connected to the ethylene glycol distillation tower system 9, the methanol distillation tower system 7 is also connected to the first high-speed jet impinging tubular reactor 2 and the second high-speed jet impinging tubular reactor 4, respectively, the vapor-liquid separation tank 3 is also connected to the light component separation tower system 6, and the light component separation tower system 6 is also connected to the ethylene glycol distillation tower system 9.
所述配料罐1为外周圈设置有热媒,内部设置有机械搅拌器1-1的罐体结构,配料罐1顶部开设有催化剂、碳酸乙烯酯进液口,配料罐1顶部进液口连接乙二醇精馏塔系统9的乙二醇精馏塔塔底泵9-7出口端;配料罐1底部出液口连接第一动力流体泵1-2的入口端,第一动力流体泵1-2的出口端连接第一高速喷流撞击管式反应器2的第一拉瓦尔喷管2-1液体入口端;配料罐1用于碳酸乙烯酯、催化剂配料,同时在搅拌的作用下将碳酸乙烯酯、催化剂混合均匀;混合液在热媒的加热下达到反应温度,通过动力流体泵1-2进入到第一高速喷流撞击管式反应器2。The batching tank 1 is a tank structure with a heat medium arranged on the outer circumference and a mechanical stirrer 1-1 arranged inside. The top of the batching tank 1 is provided with catalyst and ethylene carbonate liquid inlets, and the top liquid inlet of the batching tank 1 is connected to the outlet end of the ethylene glycol distillation tower bottom pump 9-7 of the ethylene glycol distillation tower system 9; the bottom liquid outlet of the batching tank 1 is connected to the inlet end of the first power fluid pump 1-2, and the outlet end of the first power fluid pump 1-2 is connected to the liquid inlet end of the first Laval nozzle 2-1 of the first high-speed jet impact tubular reactor 2; the batching tank 1 is used for batching ethylene carbonate and catalyst, and at the same time, ethylene carbonate and catalyst are evenly mixed under the action of stirring; the mixed liquid reaches the reaction temperature under the heating of the heat medium, and enters the first high-speed jet impact tubular reactor 2 through the power fluid pump 1-2.
所述第一高速喷流撞击管式反应器2包括第一拉瓦尔喷管2-1、第一混合腔2-2、第一高速喷流撞击腔2-3、第一管式反应器2-4和第一加热器2-5;第一拉瓦尔喷管2-1、第一混合腔2-2、第一高速喷流撞击腔2-3和第一管式反应器2-4均设置在第一加热器2-5内部,两个第一拉瓦尔喷管2-1相向设置并连通,中间连通部位形成的腔体为第一混合腔2-2,第一混合腔2-2中部的垂直方向上连通第一高速喷流撞击腔2-3,第一高速喷流撞击腔2-3连通第一管式反应器2-4的一端,第一管式反应器2-4的另一端连通汽液分离罐3顶部进液口,第一管式反应器2-4为长径比大于1000的管子,可以是Φ75mm或Φ100mm,可以设置为往复型或弹簧型。The first high-speed jet impact tubular reactor 2 includes a first Laval nozzle 2-1, a first mixing chamber 2-2, a first high-speed jet impact chamber 2-3, a first tubular reactor 2-4 and a first heater 2-5; the first Laval nozzle 2-1, the first mixing chamber 2-2, the first high-speed jet impact chamber 2-3 and the first tubular reactor 2-4 are all arranged inside the first heater 2-5, the two first Laval nozzles 2-1 are arranged opposite to each other and connected, and the cavity formed at the middle connecting part is the first mixing chamber 2-2, the first high-speed jet impact chamber 2-3 is connected in the vertical direction of the middle of the first mixing chamber 2-2, the first high-speed jet impact chamber 2-3 is connected to one end of the first tubular reactor 2-4, and the other end of the first tubular reactor 2-4 is connected to the liquid inlet at the top of the vapor-liquid separation tank 3, the first tubular reactor 2-4 is a tube with a length-to-diameter ratio greater than 1000, which can be Φ75mm or Φ100mm, and can be set to a reciprocating type or a spring type.
两个第一拉瓦尔喷管2-1的管口处开设有进汽口,进汽口与甲醇精馏塔系统7的甲醇汽化器7-6出口端连通。所述第一高速喷流撞击管式反应器2用于酯交换反应;两个相向的第一拉瓦尔喷管2-1通过第一动力流体泵1-2与配料罐1连通,并与甲醇精馏塔系统7的甲醇汽化器7-6出口端连通,配料罐1的混合液通过第一动力流体泵1-2泵入两个相向的第一拉瓦尔喷管2-1,两个相向的第一拉瓦尔喷管2-1的进气口同时吸入甲醇精馏塔系统7的甲醇汽化器7-6出口端汽化的甲醇蒸汽,两股从第一拉瓦尔喷管2-1喷出的高速喷流(配料罐1的混合液和甲醇精馏塔系统7的甲醇蒸汽),通过第一混合腔2-2在高速喷流撞击腔2-3中相互撞击,然后进入第一管式反应器2-4进行酯交换反应,酯交换液连续进入到汽液分离罐3。Steam inlets are provided at the orifices of the two first Laval nozzles 2 - 1 , and the steam inlets are connected to the outlet end of the methanol vaporizer 7 - 6 of the methanol distillation tower system 7 . The first high-speed jet impact tubular reactor 2 is used for ester exchange reaction; the two opposing first Laval nozzles 2-1 are connected to the batching tank 1 through the first power fluid pump 1-2, and are connected to the outlet end of the methanol vaporizer 7-6 of the methanol distillation tower system 7, the mixed liquid in the batching tank 1 is pumped into the two opposing first Laval nozzles 2-1 through the first power fluid pump 1-2, and the air inlets of the two opposing first Laval nozzles 2-1 simultaneously inhale the methanol vapor vaporized at the outlet end of the methanol vaporizer 7-6 of the methanol distillation tower system 7, and the two high-speed jets ejected from the first Laval nozzles 2-1 (the mixed liquid in the batching tank 1 and the methanol vapor of the methanol distillation tower system 7) collide with each other in the high-speed jet impact chamber 2-3 through the first mixing chamber 2-2, and then enter the first tubular reactor 2-4 for ester exchange reaction, and the ester exchange liquid continuously enters the vapor-liquid separation tank 3.
具体为,由于配料罐1的原料混合液经第一拉瓦尔喷管2-1高速喷出,会在第一拉瓦尔喷管2-1的进汽口产生负压区,致使甲醇精馏塔系统7的甲醇蒸汽被吸入,并在其负压区迅速膨胀并被动力流体打成微小气泡,进入第一拉瓦尔喷管2-1的第一混合腔2-2;此时,在第一混合腔2-2中,甲醇蒸汽和混合液充分混合,并且由于能量交换而加速排出,速度可以达到音速,再经过第一拉瓦尔喷管2-1的第一混合腔2-2将混合液的势能增加到最大,更加强了传质、传热的效果;来自第一拉瓦尔喷管2-1两股流体相向高速流动,通过撞击形成一个高度湍动的撞击区,大大强化了过程热、质传递;撞击流其强烈的微观混合以及压力波动特性可以使化学反应快速进行,瞬间产生有效均匀的过饱和度;而且由于混沌流动状态使混合尺度迅速减小,不同尺度漩涡及彼此折叠碰撞增强了湍动强度和能量扩散,促使分子在发生化学反应时达到更有效的高能级碰撞,撞击流有效改善了反应器内的混合及传质效果,提高了反应速率和产品收率。Specifically, since the raw material mixed liquid in the batching tank 1 is ejected at high speed through the first Laval nozzle 2-1, a negative pressure zone will be generated at the steam inlet of the first Laval nozzle 2-1, causing the methanol vapor of the methanol distillation tower system 7 to be sucked in, and rapidly expand in its negative pressure zone and be beaten into tiny bubbles by the power fluid, and enter the first mixing chamber 2-2 of the first Laval nozzle 2-1; at this time, in the first mixing chamber 2-2, the methanol vapor and the mixed liquid are fully mixed, and are accelerated to be discharged due to energy exchange, and the speed can reach the speed of sound, and then the potential energy of the mixed liquid is increased to the maximum through the first mixing chamber 2-2 of the first Laval nozzle 2-1, which further enhances the mass transfer. , heat transfer effect; the two fluids from the first Laval nozzle 2-1 flow towards each other at high speed, forming a highly turbulent impact zone through collision, which greatly enhances the process heat and mass transfer; the strong micro-mixing and pressure fluctuation characteristics of the impact flow can make the chemical reaction proceed rapidly and instantly produce effective and uniform supersaturation; and due to the chaotic flow state, the mixing scale is rapidly reduced, and the vortices of different scales and the folding collisions with each other enhance the turbulence intensity and energy diffusion, which promotes the molecules to reach more effective high-energy level collisions when chemical reactions occur. The impact flow effectively improves the mixing and mass transfer effects in the reactor, and increases the reaction rate and product yield.
所述汽液分离罐3为外周圈设置有热媒,内部设置有分离罐机械搅拌器3-1的罐体结构,汽液分离罐3上端的入口端与第一管式反应器2-4的出口端连通,汽液分离罐3上端的汽体出口端通过分离罐冷凝器3-2与轻组分分离塔系统6的汽体入口端连通,汽液分离罐3底端的出口端通过第二动力流体泵3-3与第二高速喷流撞击管式反应器4的两个第二拉瓦尔喷管4-1连通。所述汽液分离罐3用于甲醇蒸汽、反应生成的碳酸二甲酯蒸汽与酯交换液分离;从第一高速喷流撞击管式反应器2出来的酯交换液连续进入到汽液分离罐3上端的进液口,汽液分离罐3将甲醇蒸汽、反应生成的碳酸二甲酯蒸汽与酯交换液分离,分离出的汽体通过分离罐冷凝器3-2进入到轻组分分离塔系统6,分离出轻组分的酯交换液通过动力流体泵3-3进入到第二高速喷流撞击管式反应器4。The vapor-liquid separation tank 3 is a tank structure with a heat medium arranged on the outer circumference and a separation tank mechanical agitator 3-1 arranged inside. The inlet end of the upper end of the vapor-liquid separation tank 3 is connected to the outlet end of the first tubular reactor 2-4, and the vapor outlet end of the upper end of the vapor-liquid separation tank 3 is connected to the vapor inlet end of the light component separation tower system 6 through the separation tank condenser 3-2. The outlet end of the bottom end of the vapor-liquid separation tank 3 is connected to the two second Laval nozzles 4-1 of the second high-speed jet impact tubular reactor 4 through the second power fluid pump 3-3. The vapor-liquid separation tank 3 is used to separate methanol vapor, dimethyl carbonate vapor generated by the reaction from the ester exchange liquid; the ester exchange liquid coming out of the first high-speed jet impact tubular reactor 2 continuously enters the liquid inlet at the upper end of the vapor-liquid separation tank 3, and the vapor-liquid separation tank 3 separates the methanol vapor, dimethyl carbonate vapor generated by the reaction from the ester exchange liquid, and the separated vapor enters the light component separation tower system 6 through the separation tank condenser 3-2, and the ester exchange liquid separated from the light component enters the second high-speed jet impact tubular reactor 4 through the power fluid pump 3-3.
第二高速喷流撞击管式反应器4结构与第一高速喷流撞击管式反应器2一致,第二高速喷流撞击管式反应器4包括第二拉瓦尔喷管4-1,第二混合腔4-2,第二高速喷流撞击腔4-3,第二管式反应器4-4,第二加热器4-5;第二拉瓦尔喷管4-1、第二混合腔4-2、第二高速喷流撞击腔4-3和第二管式反应器4-4均设置在第二加热器4-5内部,两个第二拉瓦尔喷管4-1相向设置并连通,中间连通部位形成的腔体为第二混合腔4-2,第二混合腔4-2中部的垂直方向上连通第二高速喷流撞击腔4-3,第二高速喷流撞击腔4-3连通第二管式反应器4-4的一端,第二管式反应器4-4的另一端连通熟化罐5顶部的进液口。两个第二拉瓦尔喷管4-1的管口通过第二动力流体泵3-3与汽液分离罐3底部的出液口连通,两个第二拉瓦尔喷管4-1的管口处开设有进汽口,进汽口与甲醇精馏塔系统7的甲醇汽化器7-6出口端连通。所述第二高速喷流撞击管式反应器4用于酯交换反应。The structure of the second high-speed jet impact tubular reactor 4 is consistent with that of the first high-speed jet impact tubular reactor 2. The second high-speed jet impact tubular reactor 4 includes a second Laval nozzle 4-1, a second mixing chamber 4-2, a second high-speed jet impact chamber 4-3, a second tubular reactor 4-4, and a second heater 4-5; the second Laval nozzle 4-1, the second mixing chamber 4-2, the second high-speed jet impact chamber 4-3 and the second tubular reactor 4-4 are all arranged inside the second heater 4-5, the two second Laval nozzles 4-1 are arranged opposite to each other and connected, and the cavity formed at the middle connecting part is the second mixing chamber 4-2, the middle part of the second mixing chamber 4-2 is connected to the second high-speed jet impact chamber 4-3 in the vertical direction, the second high-speed jet impact chamber 4-3 is connected to one end of the second tubular reactor 4-4, and the other end of the second tubular reactor 4-4 is connected to the liquid inlet at the top of the maturation tank 5. The pipe openings of the two second Laval nozzles 4-1 are connected to the liquid outlet at the bottom of the vapor-liquid separation tank 3 through the second power fluid pump 3-3, and the pipe openings of the two second Laval nozzles 4-1 are provided with steam inlets, which are connected to the outlet end of the methanol vaporizer 7-6 of the methanol distillation tower system 7. The second high-speed jet impact tubular reactor 4 is used for transesterification reaction.
两个第二拉瓦尔喷管4-1通过第二动力流体泵3-3与汽液分离罐3底部的出液口连通,并与甲醇精馏塔系统7的甲醇汽化器7-6出口端连通,汽液分离罐3的混合液通过第二动力流体泵3-3泵入两个相向的第二拉瓦尔喷管4-1,两个相向的第二拉瓦尔喷管4-1进汽口同时吸入甲醇精馏塔系统7的甲醇汽化器7-6出口端汽化的甲醇蒸汽,两股从第二拉瓦尔喷管4-1喷出的高速喷流(汽液分离罐3的酯交换液和甲醇精馏塔系统7的甲醇蒸汽),通过第二混合腔4-2在高速喷流撞击腔4-3中相互撞击,然后进入第二管式反应器4-4进行酯交换反应,酯交换液连续进入到熟化罐5。The two second Laval nozzles 4-1 are connected to the liquid outlet at the bottom of the vapor-liquid separation tank 3 through the second power fluid pump 3-3, and are connected to the outlet end of the methanol vaporizer 7-6 of the methanol distillation tower system 7. The mixed liquid in the vapor-liquid separation tank 3 is pumped into the two opposing second Laval nozzles 4-1 through the second power fluid pump 3-3. The steam inlets of the two opposing second Laval nozzles 4-1 simultaneously inhale the methanol vapor vaporized at the outlet end of the methanol vaporizer 7-6 of the methanol distillation tower system 7. The two high-speed jets ejected from the second Laval nozzles 4-1 (the ester exchange liquid in the vapor-liquid separation tank 3 and the methanol vapor in the methanol distillation tower system 7) collide with each other in the high-speed jet impact chamber 4-3 through the second mixing chamber 4-2, and then enter the second tubular reactor 4-4 for ester exchange reaction, and the ester exchange liquid continuously enters the maturation tank 5.
所述熟化罐5为外周圈设置有热媒,内部设置有熟化罐机械搅拌器5-1的罐体结构;所述熟化罐5顶端进液口连接第二高速喷流撞击管式反应器4的第二管式反应器4-4出口端,熟化罐5的上部溢流口连接轻组分分离塔塔釜6-1顶部进液口;所述熟化罐5用于继续进行补充酯交换反应;从第二高速喷流撞击管式反应器4出来的酯交换液连续进入到熟化罐5,在熟化罐5里继续进行补充酯交换反应;从熟化罐5里溢流出来的酯交换物料进入到轻组分分离塔系统6塔釜。The maturation tank 5 is a tank structure with a heat medium arranged on the outer circumference and a mechanical stirrer 5-1 arranged inside the maturation tank; the top liquid inlet of the maturation tank 5 is connected to the outlet end of the second tubular reactor 4-4 of the second high-speed jet impact tubular reactor 4, and the upper overflow port of the maturation tank 5 is connected to the top liquid inlet of the light component separation tower kettle 6-1; the maturation tank 5 is used to continue to carry out supplementary ester exchange reaction; the ester exchange liquid coming out of the second high-speed jet impact tubular reactor 4 continuously enters the maturation tank 5, and the supplementary ester exchange reaction continues in the maturation tank 5; the ester exchange material overflowing from the maturation tank 5 enters the light component separation tower system 6 kettle.
所述轻组分分离塔系统6包括轻组分分离塔塔釜6-1、轻组分白钢规整填料塔6-2、轻组分冷凝器6-3、轻组分接收罐6-4、轻组分液泵6-5和轻组分分离塔塔底泵6-6;轻组分分离塔塔釜6-1为外周圈设置有热媒的结构,所述轻组分分离塔塔釜6-1顶部进液口与熟化罐5的上部溢流口连通,轻组分分离塔塔釜6-1底部的出液口与轻组分分离塔塔底泵6-6的进液口连通,轻组分分离塔塔底泵6-6的出口连通轻组分分离塔塔釜6-1塔釜液回流进液口,轻组分分离塔塔底泵6-6的出口端连接乙二醇精馏塔系统9的进液口;轻组分分离塔塔釜6-1上端与轻组分白钢规整填料塔6-2连通一体设置,轻组分白钢规整填料塔6-2的蒸汽入口端连通分离罐冷凝器3-2的出口端,轻组分白钢规整填料塔6-2的蒸汽出口端连通轻组分冷凝器6-3的入口端,轻组分冷凝器6-3的出口端连通轻组分接收罐6-4的入口端,轻组分接收罐6-4的出口端连通轻组分液泵6-5的出口端,轻组分液泵6-5的出口端连通轻组分白钢规整填料塔6-2上部回流进液口,轻组分液泵6-5的出口端还连通甲醇精馏塔系统7进液口。所述轻组分分离塔系统6用于汽液分离罐3、熟化罐5里酯交换液轻组分的分离;轻组分分离塔系统6分离出的轻组分汽体经冷凝器6-3冷凝进入轻组分液接收罐6-4,部分作为轻组分分离塔系统6的回流,部分进入到甲醇精馏塔系统7;轻组分分离塔系统6的塔釜液通过轻组分分离塔塔底泵6-6连续进入到乙二醇精馏塔系统9。The light component separation tower system 6 comprises a light component separation tower kettle 6-1, a light component white steel structured packing tower 6-2, a light component condenser 6-3, a light component receiving tank 6-4, a light component liquid pump 6-5 and a light component separation tower bottom pump 6-6; the light component separation tower kettle 6-1 is a structure with a heat medium arranged on the outer circumference, the top liquid inlet of the light component separation tower kettle 6-1 is connected with the upper overflow port of the maturation tank 5, the bottom liquid outlet of the light component separation tower kettle 6-1 is connected with the liquid inlet of the light component separation tower bottom pump 6-6, the outlet of the light component separation tower bottom pump 6-6 is connected with the liquid reflux inlet of the light component separation tower kettle 6-1, and the outlet end of the light component separation tower bottom pump 6-6 is connected with the ethylene glycol fine The liquid inlet of the distillation tower system 9; the upper end of the light component separation tower kettle 6-1 is connected to the light component white steel structured packing tower 6-2, the steam inlet end of the light component white steel structured packing tower 6-2 is connected to the outlet end of the separation tank condenser 3-2, the steam outlet end of the light component white steel structured packing tower 6-2 is connected to the inlet end of the light component condenser 6-3, the outlet end of the light component condenser 6-3 is connected to the inlet end of the light component receiving tank 6-4, the outlet end of the light component receiving tank 6-4 is connected to the outlet end of the light component liquid pump 6-5, the outlet end of the light component liquid pump 6-5 is connected to the upper reflux liquid inlet of the light component white steel structured packing tower 6-2, and the outlet end of the light component liquid pump 6-5 is also connected to the liquid inlet of the methanol distillation tower system 7. The light component separation tower system 6 is used for separating the light components of the ester exchange liquid in the vapor-liquid separation tank 3 and the maturation tank 5; the light component vapor separated by the light component separation tower system 6 is condensed by the condenser 6-3 and enters the light component liquid receiving tank 6-4, part of which is used as the reflux of the light component separation tower system 6, and part of which enters the methanol distillation tower system 7; the bottom liquid of the light component separation tower system 6 continuously enters the ethylene glycol distillation tower system 9 through the light component separation tower bottom pump 6-6.
所述甲醇精馏塔系统7包括甲醇精馏塔再沸器7-1,甲醇精馏塔白钢规整填料塔7-2,甲醇精馏塔冷凝器7-3,甲醇精馏塔共沸液接收罐7-4,甲醇精馏塔共沸液泵7-5,甲醇汽化器7-6,甲醇精馏塔塔底泵7-7;所述甲醇精馏塔系统7中部进液口连通轻组分分离塔系统6的轻组分液泵6-5出口端还连通碳酸二甲酯精馏塔系统8的碳酸二甲酯精馏塔共沸液泵8-5出口端;甲醇精馏塔白钢规整填料塔7-2顶部蒸汽出口连通甲醇精馏塔冷凝器7-3的入口端,甲醇精馏塔冷凝器7-3的出口端连通甲醇精馏塔共沸液接收罐7-4顶部的入口端,甲醇精馏塔共沸液接收罐7-4底部的出口端连通甲醇精馏塔共沸液泵7-5的入口端,甲醇精馏塔共沸液泵7-5的出口端连通甲醇精馏塔白钢规整填料塔7-2上部回流液进液口还连接碳酸二甲酯精馏塔系统8中部的进液口;甲醇精馏塔白钢规整填料塔7-2底部出液口连接甲醇精馏塔塔底泵7-7的入口端,甲醇精馏塔塔底泵7-7的出口端连接甲醇精馏塔再沸器7-1入口端,甲醇精馏塔再沸器7-1为设置有热媒的结构,甲醇精馏塔再沸器7-1出口端连接甲醇精馏塔白钢规整填料塔7-2的再沸液回流口;甲醇精馏塔塔底泵7-7的出口端还连接甲醇汽化器7-6入口端,甲醇汽化器7-6入口端还连接新鲜甲醇入口端,甲醇汽化器7-6出口端分别连接第一拉瓦尔喷管2-1、第二拉瓦尔喷管4-1的汽体入口端;所述甲醇精馏塔系统7用于共沸液精馏出甲醇;甲醇精馏塔系统7塔顶分离出的共沸物蒸汽经甲醇精馏塔冷凝器7-3冷凝进入到甲醇精馏塔共沸液接收罐7-4,部分作为甲醇精馏塔系统7的回流,部分进入到碳酸二甲酯精馏塔系统8;甲醇精馏塔系统7塔釜液经甲醇精馏塔塔底泵7-7进入到甲醇汽化器7-6,汽化的甲醇继续用于第一高速喷流撞击管式反应器2和第二高速喷流撞击管式反应器4的酯交换反应。The methanol distillation tower system 7 comprises a methanol distillation tower reboiler 7-1, a methanol distillation tower white steel structured packing tower 7-2, a methanol distillation tower condenser 7-3, a methanol distillation tower azeotropic liquid receiving tank 7-4, a methanol distillation tower azeotropic liquid pump 7-5, a methanol vaporizer 7-6, and a methanol distillation tower bottom pump 7-7; the middle liquid inlet of the methanol distillation tower system 7 is connected to the outlet end of the light component liquid pump 6-5 of the light component separation tower system 6 and is also connected to the outlet end of the dimethyl carbonate distillation tower azeotropic liquid pump 8-5 of the dimethyl carbonate distillation tower system 8; the top of the methanol distillation tower white steel structured packing tower 7-2 is connected to the outlet end of the dimethyl carbonate distillation tower azeotropic liquid pump 8-5 of the dimethyl carbonate distillation tower system 8; The steam outlet is connected to the inlet end of the methanol distillation tower condenser 7-3, the outlet end of the methanol distillation tower condenser 7-3 is connected to the inlet end of the top of the methanol distillation tower azeotropic liquid receiving tank 7-4, the outlet end of the methanol distillation tower azeotropic liquid receiving tank 7-4 at the bottom is connected to the inlet end of the methanol distillation tower azeotropic liquid pump 7-5, the outlet end of the methanol distillation tower azeotropic liquid pump 7-5 is connected to the upper reflux liquid inlet of the methanol distillation tower white steel structured packing tower 7-2 is also connected to the liquid inlet in the middle of the dimethyl carbonate distillation tower system 8; the bottom liquid outlet of the methanol distillation tower white steel structured packing tower 7-2 is connected to the bottom of the methanol distillation tower The inlet end of the methanol distillation tower bottom pump 7-7 and the outlet end of the methanol distillation tower bottom pump 7-7 are connected to the inlet end of the methanol distillation tower reboiler 7-1, the methanol distillation tower reboiler 7-1 is a structure provided with a heat medium, and the outlet end of the methanol distillation tower reboiler 7-1 is connected to the reboiled liquid reflux port of the methanol distillation tower white steel structured packing tower 7-2; the outlet end of the methanol distillation tower bottom pump 7-7 is also connected to the inlet end of the methanol vaporizer 7-6, the inlet end of the methanol vaporizer 7-6 is also connected to the inlet end of the fresh methanol, and the outlet end of the methanol vaporizer 7-6 is respectively connected to the first Laval nozzle 2-1 and the second Laval nozzle 4-1 Gas inlet end; the methanol distillation tower system 7 is used to distill methanol from the azeotropic liquid; the azeotropic vapor separated from the top of the methanol distillation tower system 7 is condensed by the methanol distillation tower condenser 7-3 and enters the methanol distillation tower azeotropic liquid receiving tank 7-4, part of which is used as the reflux of the methanol distillation tower system 7, and part of which enters the dimethyl carbonate distillation tower system 8; the bottom liquid of the methanol distillation tower system 7 enters the methanol vaporizer 7-6 through the methanol distillation tower bottom pump 7-7, and the vaporized methanol is continuously used for the ester exchange reaction of the first high-speed jet impact tubular reactor 2 and the second high-speed jet impact tubular reactor 4.
所述碳酸二甲酯精馏塔系统8包括碳酸二甲酯精馏塔再沸器8-1、碳酸二甲酯精馏塔白钢规整填料塔8-2、碳酸二甲酯精馏塔冷凝器8-3、碳酸二甲酯精馏塔共沸液接收罐8-4、碳酸二甲酯精馏塔共沸液泵8-5、碳酸二甲酯储罐8-6和碳酸二甲酯精馏塔塔底泵8-7;所述碳酸二甲酯精馏塔白钢规整填料塔8-2中部进液口连通甲醇精馏塔共沸液泵7-5的出口端;碳酸二甲酯精馏塔白钢规整填料塔8-2顶部蒸汽出口连通碳酸二甲酯精馏塔冷凝器8-3的入口端,碳酸二甲酯精馏塔冷凝器8-3的出口端连接碳酸二甲酯精馏塔共沸液接收罐8-4顶部的入口端,碳酸二甲酯精馏塔共沸液接收罐8-4底部的出口端连通碳酸二甲酯精馏塔共沸液泵8-5的入口端,碳酸二甲酯精馏塔共沸液泵8-5的出口端连通碳酸二甲酯精馏塔白钢规整填料塔8-2上部回流液进液口,碳酸二甲酯精馏塔共沸液泵8-5的出口端还连通甲醇精馏塔系统7中部的进液口;碳酸二甲酯精馏塔白钢规整填料塔8-2底部出液口连通碳酸二甲酯精馏塔塔底泵8-7的入口端,碳酸二甲酯精馏塔塔底泵8-7的出口端连通碳酸二甲酯精馏塔再沸器8-1入口端,碳酸二甲酯精馏塔再沸器8-1为设置有热媒的结构,碳酸二甲酯精馏塔再沸器8-1出口端连通碳酸二甲酯精馏塔白钢规整填料塔8-2再沸液回流口;碳酸二甲酯精馏塔塔底泵8-7的出口端还连接碳酸二甲酯储罐8-6顶部入口端;所述碳酸二甲酯精馏塔系统8用于共沸液精馏出碳酸二甲酯;碳酸二甲酯精馏塔系统8塔顶分离出的共沸物蒸汽经碳酸二甲酯精馏塔冷凝器8-3冷凝进入到碳酸二甲酯精馏塔共沸液接收罐8-4,部分作为碳酸二甲酯精馏塔系统8的回流,部分作为进料返回到甲醇精馏塔系统7;碳酸二甲酯精馏塔系统8塔釜液经碳酸二甲酯精馏塔塔底泵8-7进入到碳酸二甲酯储罐8-6。The dimethyl carbonate distillation tower system 8 comprises a dimethyl carbonate distillation tower reboiler 8-1, a dimethyl carbonate distillation tower white steel structured packing tower 8-2, a dimethyl carbonate distillation tower condenser 8-3, a dimethyl carbonate distillation tower azeotropic liquid receiving tank 8-4, a dimethyl carbonate distillation tower azeotropic liquid pump 8-5, a dimethyl carbonate storage tank 8-6 and a dimethyl carbonate distillation tower bottom pump 8-7; the middle liquid inlet of the dimethyl carbonate distillation tower white steel structured packing tower 8-2 is connected to the outlet end of the methanol distillation tower azeotropic liquid pump 7-5; the dimethyl carbonate distillation tower white steel structured packing tower 8- The top steam outlet of the dimethyl carbonate distillation tower is connected to the inlet end of the condenser 8-3 of the dimethyl carbonate distillation tower, the outlet end of the condenser 8-3 of the dimethyl carbonate distillation tower is connected to the inlet end of the top of the azeotropic liquid receiving tank 8-4 of the dimethyl carbonate distillation tower, the outlet end of the azeotropic liquid receiving tank 8-4 of the dimethyl carbonate distillation tower is connected to the inlet end of the azeotropic liquid pump 8-5 of the dimethyl carbonate distillation tower, the outlet end of the azeotropic liquid pump 8-5 of the dimethyl carbonate distillation tower is connected to the upper reflux liquid inlet of the white steel structured packing tower 8-2 of the dimethyl carbonate distillation tower, and the outlet end of the azeotropic liquid pump 8-5 of the dimethyl carbonate distillation tower is also connected to the top of the reflux liquid inlet of the white steel structured packing tower 8-2 of the dimethyl carbonate distillation tower. The liquid inlet in the middle of the methanol distillation tower system 7 is connected; the bottom liquid outlet of the white steel structured packing tower 8-2 of the dimethyl carbonate distillation tower is connected to the inlet end of the bottom pump 8-7 of the dimethyl carbonate distillation tower, and the outlet end of the bottom pump 8-7 of the dimethyl carbonate distillation tower is connected to the inlet end of the reboiler 8-1 of the dimethyl carbonate distillation tower. The reboiler 8-1 of the dimethyl carbonate distillation tower is a structure provided with a heat medium, and the outlet end of the reboiler 8-1 of the dimethyl carbonate distillation tower is connected to the reboiled liquid reflux port of the white steel structured packing tower 8-2 of the dimethyl carbonate distillation tower; the outlet end of the bottom pump 8-7 of the dimethyl carbonate distillation tower It is also connected to the top inlet end of the dimethyl carbonate storage tank 8-6; the dimethyl carbonate distillation tower system 8 is used to distill dimethyl carbonate from the azeotropic liquid; the azeotropic vapor separated from the top of the dimethyl carbonate distillation tower system 8 is condensed by the dimethyl carbonate distillation tower condenser 8-3 and enters the dimethyl carbonate distillation tower azeotropic liquid receiving tank 8-4, part of which is used as reflux of the dimethyl carbonate distillation tower system 8, and part of which is returned to the methanol distillation tower system 7 as feed; the bottom liquid of the dimethyl carbonate distillation tower system 8 enters the dimethyl carbonate storage tank 8-6 through the dimethyl carbonate distillation tower bottom pump 8-7.
所述乙二醇精馏塔系统9包括乙二醇精馏塔再沸器9-1、乙二醇精馏塔白钢规整填料塔9-2、乙二醇精馏塔冷凝器9-3、乙二醇接收罐9-4、乙二醇泵9-5、乙二醇储罐9-6和乙二醇精馏塔塔底泵9-7。所述乙二醇精馏塔系统9中部进液口连通轻组分分离塔塔底泵6-6的出口端;乙二醇精馏塔白钢规整填料塔9-2顶部蒸汽出口连通乙二醇精馏塔冷凝器9-3的入口端,乙二醇精馏塔冷凝器9-3的出口端连通乙二醇接收罐9-4顶部的入口端,乙二醇接收罐9-4底部的出口端连通乙二醇泵9-5的入口端,乙二醇泵9-5的出口端连通乙二醇精馏塔白钢规整填料塔9-2上部回流液进液口,乙二醇泵9-5的出口端还连通乙二醇储罐9-6顶部入口端;乙二醇精馏塔白钢规整填料塔9-2底部出液口连通乙二醇精馏塔塔底泵9-7的入口端,乙二醇精馏塔塔底泵9-7的出口端连通乙二醇精馏塔再沸器9-1入口端,乙二醇精馏塔再沸器9-1为设置有热媒的结构,乙二醇精馏塔再沸器9-1出口端连通乙二醇精馏塔白钢规整填料塔9-2再沸液回流口;乙二醇精馏塔塔底泵9-7的出口端还连通配料罐1顶部入口端;所述乙二醇精馏塔系统9用于轻组分分离塔系统6的塔釜液精馏出乙二醇;轻组分分离塔系统6的塔釜液通过轻组分分离塔塔底泵6-6连续泵入乙二醇精馏塔系统9,乙二醇精馏塔系统9塔顶分离出的乙二醇蒸汽经乙二醇精馏塔冷凝器9-3冷凝进入到乙二醇接收罐9-4,部分作为乙二醇精馏塔系统9的回流,部分进料进入到乙二醇储罐9-6;乙二醇精馏塔系统9的塔釜液经乙二醇精馏塔塔底泵9-7部分进入乙二醇精馏塔再沸器9-1加热后返回乙二醇精馏塔系统9,部分作为回收催化剂连续进入到配料罐1。The ethylene glycol distillation tower system 9 includes an ethylene glycol distillation tower reboiler 9-1, an ethylene glycol distillation tower white steel structured packing tower 9-2, an ethylene glycol distillation tower condenser 9-3, an ethylene glycol receiving tank 9-4, an ethylene glycol pump 9-5, an ethylene glycol storage tank 9-6 and an ethylene glycol distillation tower bottom pump 9-7. The liquid inlet in the middle of the ethylene glycol distillation tower system 9 is connected to the outlet end of the light component separation tower bottom pump 6-6; the top steam outlet of the ethylene glycol distillation tower white steel structured packing tower 9-2 is connected to the inlet end of the ethylene glycol distillation tower condenser 9-3, the outlet end of the ethylene glycol distillation tower condenser 9-3 is connected to the inlet end of the top of the ethylene glycol receiving tank 9-4, the outlet end of the bottom of the ethylene glycol receiving tank 9-4 is connected to the inlet end of the ethylene glycol pump 9-5, and the outlet end of the ethylene glycol pump 9-5 is connected to the outlet end of the ethylene glycol pump 9-5. The upper reflux liquid inlet of the white steel structured packing tower 9-2 of the ethylene glycol distillation tower is connected, and the outlet end of the ethylene glycol pump 9-5 is also connected to the top inlet end of the ethylene glycol storage tank 9-6; the bottom liquid outlet of the white steel structured packing tower 9-2 of the ethylene glycol distillation tower is connected to the inlet end of the bottom pump 9-7 of the ethylene glycol distillation tower, and the outlet end of the bottom pump 9-7 of the ethylene glycol distillation tower is connected to the inlet end of the reboiler 9-1 of the ethylene glycol distillation tower, and the reboiler 9-1 of the ethylene glycol distillation tower is a structure provided with a heat medium The outlet end of the reboiler 9-1 of the ethylene glycol distillation tower is connected to the reboiled liquid reflux port of the white steel structured packing tower 9-2 of the ethylene glycol distillation tower; the outlet end of the bottom pump 9-7 of the ethylene glycol distillation tower is also connected to the top inlet end of the batching tank 1; the ethylene glycol distillation tower system 9 is used to distill ethylene glycol from the bottom liquid of the light component separation tower system 6; the bottom liquid of the light component separation tower system 6 is continuously pumped into the ethylene glycol distillation tower system 9 through the bottom pump 6-6 of the light component separation tower, and the ethylene glycol distillation tower The ethylene glycol vapor separated from the top of system 9 is condensed by the ethylene glycol distillation tower condenser 9-3 and enters the ethylene glycol receiving tank 9-4, part of which is used as reflux of the ethylene glycol distillation tower system 9, and part of which is fed into the ethylene glycol storage tank 9-6; the bottom liquid of the ethylene glycol distillation tower system 9 is partially fed into the ethylene glycol distillation tower reboiler 9-1 through the ethylene glycol distillation tower bottom pump 9-7, and then returns to the ethylene glycol distillation tower system 9 after heating, and part of which is continuously fed into the batching tank 1 as a recovered catalyst.
本发明采用的原料为工业品碳酸乙烯酯(质量含量大于99.5%)、工业品甲醇(质量含量大于99.5%)、催化剂等;所用公用工程水蒸汽为0.4MPa,290℃的过热水蒸汽;公用工程水蒸汽主要为配料罐1的热媒、第一高速喷流撞击管式反应器2的第一加热器2-5、汽液分离罐3的热媒、第二高速喷流撞击管式反应器4的第二加热器4-5、熟化罐5的热媒、轻组分分离塔系统6的热媒、甲醇精馏塔系统7的热媒、碳酸二甲酯精馏塔系统8的热媒、乙二醇精馏塔系统9的热媒提供热源;装置各设备通过相应的管线连接,附图1中管线在图上发生交叉而实际并不相交时,按照竖断横不断的原则绘制。热媒结构为现有的夹套结构;塔釜的热媒结构为现有的再沸器结构。The raw materials used in the present invention are industrial ethylene carbonate (mass content greater than 99.5%), industrial methanol (mass content greater than 99.5%), catalysts, etc.; the public engineering water vapor used is 0.4MPa, 290°C superheated water vapor; the public engineering water vapor is mainly used as the heat medium of the batching tank 1, the first heater 2-5 of the first high-speed jet impact tubular reactor 2, the heat medium of the vapor-liquid separation tank 3, the second heater 4-5 of the second high-speed jet impact tubular reactor 4, the heat medium of the maturation tank 5, the heat medium of the light component separation tower system 6, the heat medium of the methanol distillation tower system 7, the heat medium of the dimethyl carbonate distillation tower system 8, and the heat medium of the ethylene glycol distillation tower system 9 to provide heat sources; the various devices of the device are connected by corresponding pipelines. When the pipelines in Figure 1 cross on the figure but do not actually intersect, they are drawn according to the principle of vertical and horizontal interruption. The heat medium structure is the existing jacket structure; the heat medium structure of the tower kettle is the existing reboiler structure.
一种基于上述装置的碳酸二甲酯生产方法,具体包括如下步骤:A method for producing dimethyl carbonate based on the above device specifically comprises the following steps:
(1)将原料碳酸乙烯酯、催化剂填入到配料罐1内,配料罐1内温度为70℃~75℃,压力为常压,同时在机械搅拌器1-1搅拌的作用下将碳酸乙烯酯、催化剂混合均匀得到混合液;混合液在热媒的加热下达到反应温度,物料的停留时间为0.5h~0.75h;通过动力流体泵1-2连续进入到第一高速喷流撞击管式反应器2;(1) Adding raw materials of ethylene carbonate and catalyst into a batching tank 1, wherein the temperature in the batching tank 1 is 70° C. to 75° C. and the pressure is normal pressure, and the ethylene carbonate and catalyst are uniformly mixed under the stirring action of a mechanical stirrer 1-1 to obtain a mixed liquid; the mixed liquid reaches the reaction temperature under the heating of a heat medium, and the residence time of the materials is 0.5 h to 0.75 h; and the mixed liquid continuously enters the first high-speed jet impact tubular reactor 2 through a power fluid pump 1-2;
(2)配料罐1内的混合液通过动力流体泵1-2泵入两个相向的第一拉瓦尔喷管2-1,第一拉瓦尔喷管2-1进汽口同时吸入甲醇精馏塔系统7的甲醇蒸汽,两股从第一拉瓦尔喷管2-1喷出的高速喷流,在高速喷流撞击腔中相互撞击,然后进入管式反应器2-4进行酯交换反应得到酯交换液,酯交换液连续进入到汽液分离罐3;第一高速喷流撞击管式反应器2内温度为80℃~85℃,压力为0.2MPa~0.25MPa;(2) The mixed liquid in the batching tank 1 is pumped into two opposing first Laval nozzles 2-1 through a power fluid pump 1-2. The steam inlet of the first Laval nozzle 2-1 simultaneously inhales methanol vapor from the methanol distillation tower system 7. The two high-speed jets ejected from the first Laval nozzle 2-1 collide with each other in the high-speed jet impact chamber and then enter the tubular reactor 2-4 for ester exchange reaction to obtain ester exchange liquid. The ester exchange liquid continuously enters the vapor-liquid separation tank 3. The temperature in the first high-speed jet impact tubular reactor 2 is 80° C. to 85° C. and the pressure is 0.2 MPa to 0.25 MPa.
(3)汽液分离罐3将未反应的甲醇蒸汽、反应生成的碳酸二甲酯蒸汽与酯交换液分离,分离出的汽体进入到轻组分分离塔系统6;分离出轻组分的酯交换液通过第二动力流体泵3-3连续进入到第二高速喷流撞击管式反应器4的两个相向的第二拉瓦尔喷管4-1;汽液分离罐3内温度为70℃~75℃,压力为常压,物料的停留时间为0.5h~0.75h;(3) The vapor-liquid separation tank 3 separates the unreacted methanol vapor, the dimethyl carbonate vapor generated by the reaction and the transesterification liquid, and the separated vapor enters the light component separation tower system 6; the transesterification liquid with separated light components continuously enters the two opposite second Laval nozzles 4-1 of the second high-speed jet impact tubular reactor 4 through the second power fluid pump 3-3; the temperature in the vapor-liquid separation tank 3 is 70°C to 75°C, the pressure is normal pressure, and the residence time of the material is 0.5h to 0.75h;
(4)第二拉瓦尔喷管4-1进汽口同时吸入甲醇精馏塔系统7的甲醇蒸汽,两股从第二拉瓦尔喷管4-1喷出的高速喷流,在高速喷流撞击腔中相互撞击,然后进入第二管式反应器4-4进行酯交换反应,从第二高速喷流撞击管式反应器4出来的酯交换液连续进入到熟化罐5;第二高速喷流撞击管式反应器4内温度为80℃~85℃,压力为0.2MPa~0.25MPa:(4) The steam inlet of the second Laval nozzle 4-1 simultaneously sucks in methanol vapor from the methanol distillation tower system 7. The two high-speed jets ejected from the second Laval nozzle 4-1 collide with each other in the high-speed jet impact chamber and then enter the second tubular reactor 4-4 for transesterification reaction. The transesterification liquid from the second high-speed jet impact tubular reactor 4 continuously enters the maturation tank 5. The temperature in the second high-speed jet impact tubular reactor 4 is 80° C. to 85° C., and the pressure is 0.2 MPa to 0.25 MPa.
(5)酯交换液在熟化罐5里继续进行补充酯交换反应;从熟化罐5里溢流出来的熟化液进入到轻组分分离塔系统6塔釜;熟化罐5内温度为80℃~85℃,压力为0.2MPa~0.25MPa,物料的停留时间为1.5h~2h;(5) The ester exchange liquid continues to undergo supplementary ester exchange reaction in the maturation tank 5; the aging liquid overflowing from the maturation tank 5 enters the kettle of the light component separation tower system 6; the temperature in the maturation tank 5 is 80°C to 85°C, the pressure is 0.2MPa to 0.25MPa, and the residence time of the material is 1.5h to 2h;
(6)来自汽液分离罐3、熟化罐5的物料连续进入到轻组分分离塔系统6,轻组分分离塔系统6分离出的轻组分汽体经冷凝器6-3冷凝进入轻组分液接收罐6-4,得到的轻组分液分别作为轻组分分离塔系统6的回流,以及进入到甲醇精馏塔系统7;轻组分分离塔系统6的塔釜液通过轻组分分离塔塔底泵6-6连续进入到乙二醇精馏塔系统9;轻组分分离塔系统6塔釜温度为75℃~78℃,塔顶温度为64℃~66℃,回流比为3~4,压力为常压;(6) The materials from the vapor-liquid separation tank 3 and the maturation tank 5 continuously enter the light component separation tower system 6. The light component vapor separated by the light component separation tower system 6 is condensed by the condenser 6-3 and enters the light component liquid receiving tank 6-4. The obtained light component liquid is used as the reflux of the light component separation tower system 6 and enters the methanol distillation tower system 7; the bottom liquid of the light component separation tower system 6 continuously enters the ethylene glycol distillation tower system 9 through the light component separation tower bottom pump 6-6; the bottom temperature of the light component separation tower system 6 is 75°C to 78°C, the top temperature is 64°C to 66°C, the reflux ratio is 3 to 4, and the pressure is normal pressure;
(7)来自轻组分分离塔系统6的轻组分液连续进入到甲醇精馏塔系统7,甲醇精馏塔系统7塔顶分离出的共沸物蒸汽经甲醇精馏塔冷凝器7-3冷凝进入到甲醇精馏塔共沸液接收罐7-4,得到的共沸液分别作为甲醇精馏塔系统7的回流,以及进入到碳酸二甲酯精馏塔系统8;甲醇精馏塔系统7塔釜液经甲醇精馏塔塔底泵7-7进入到甲醇汽化器7-6,汽化的甲醇分别进入第一拉瓦尔喷管2-1、第二拉瓦尔喷管4-1的汽体入口继续用于酯交换反应;甲醇精馏塔系统7塔底温度为70℃,塔底压力为0.13MPa;塔顶温度为64℃,塔顶压力为常压,回流比为2;(7) The light component liquid from the light component separation tower system 6 continuously enters the methanol distillation tower system 7, and the azeotropic vapor separated from the top of the methanol distillation tower system 7 is condensed by the methanol distillation tower condenser 7-3 and enters the methanol distillation tower azeotropic liquid receiving tank 7-4. The obtained azeotropic liquid is used as the reflux of the methanol distillation tower system 7 and enters the dimethyl carbonate distillation tower system 8; the bottom liquid of the methanol distillation tower system 7 enters the methanol vaporizer 7-6 through the methanol distillation tower bottom pump 7-7, and the vaporized methanol enters the gas inlet of the first Laval nozzle 2-1 and the second Laval nozzle 4-1 to continue to be used for the ester exchange reaction; the bottom temperature of the methanol distillation tower system 7 is 70°C, and the bottom pressure is 0.13MPa; the top temperature is 64°C, the top pressure is normal pressure, and the reflux ratio is 2;
(8)来自甲醇精馏塔系统7的共沸液连续进入到碳酸二甲酯精馏塔系统8,碳酸二甲酯精馏塔系统8塔顶分离出的共沸物蒸汽经碳酸二甲酯精馏塔冷凝器8-3冷凝进入到碳酸二甲酯精馏塔共沸液接收罐8-4,得到的共沸液分别作为碳酸二甲酯精馏塔系统8的回流,以及作为进料返回到甲醇精馏塔系统7;碳酸二甲酯精馏塔系统8塔釜液经碳酸二甲酯精馏塔塔底泵8-7进入到碳酸二甲酯储罐8-6;碳酸二甲酯精馏塔系统8塔底温度为183℃,塔底压力为1.33MPa;塔顶温度为147℃,塔顶压力为1.30MPa,回流比为1.2;(8) The azeotropic liquid from the methanol distillation tower system 7 continuously enters the dimethyl carbonate distillation tower system 8, and the azeotropic liquid vapor separated from the top of the dimethyl carbonate distillation tower system 8 is condensed by the dimethyl carbonate distillation tower condenser 8-3 and enters the dimethyl carbonate distillation tower azeotropic liquid receiving tank 8-4, and the obtained azeotropic liquid is used as the reflux of the dimethyl carbonate distillation tower system 8 and as the feed to return to the methanol distillation tower system 7; the bottom liquid of the dimethyl carbonate distillation tower system 8 enters the dimethyl carbonate storage tank 8-6 through the dimethyl carbonate distillation tower bottom pump 8-7; the bottom temperature of the dimethyl carbonate distillation tower system 8 is 183°C, the bottom pressure is 1.33MPa; the top temperature is 147°C, the top pressure is 1.30MPa, and the reflux ratio is 1.2;
(9)来自轻组分分离塔系统6的塔釜液连续进入到乙二醇精馏塔系统9,乙二醇精馏塔系统9塔顶分离出的乙二醇蒸汽经乙二醇精馏塔冷凝器9-3冷凝进入到乙二醇接收罐9-4,得到的乙二醇分别作为乙二醇精馏塔系统9的回流,以及进料进入到乙二醇储罐9-6;乙二醇精馏塔系统9的塔釜液经乙二醇精馏塔塔底泵9-7分别进入乙二醇精馏塔再沸器9-1加热后返回乙二醇精馏塔系统9,以及作为回收催化剂连续进入到配料罐1。乙二醇精馏塔系统9塔顶温度为150℃,塔顶压力为0.02MPa;塔底温度为178℃,回流比为1.5。(9) The bottom liquid from the light component separation tower system 6 continuously enters the ethylene glycol distillation tower system 9. The ethylene glycol vapor separated from the top of the ethylene glycol distillation tower system 9 is condensed by the ethylene glycol distillation tower condenser 9-3 and enters the ethylene glycol receiving tank 9-4. The obtained ethylene glycol is used as the reflux of the ethylene glycol distillation tower system 9 and the feed to the ethylene glycol storage tank 9-6. The bottom liquid of the ethylene glycol distillation tower system 9 enters the ethylene glycol distillation tower reboiler 9-1 through the ethylene glycol distillation tower bottom pump 9-7 and returns to the ethylene glycol distillation tower system 9 after heating, and continuously enters the batching tank 1 as a recovered catalyst. The top temperature of the ethylene glycol distillation tower system 9 is 150°C, the top pressure is 0.02MPa; the bottom temperature is 178°C, and the reflux ratio is 1.5.
实施例1Example 1
基于高速喷流撞击管式反应器制备碳酸二甲酯的装置的碳酸二甲酯生产方法,包括如下步骤:The method for producing dimethyl carbonate based on a device for preparing dimethyl carbonate using a high-speed jet impingement tubular reactor comprises the following steps:
所述步骤(1)原料工业级碳酸乙烯酯(质量含量大于99.5%)176kg/h、催化剂0.44kg/h进入到配料罐1内,同时在搅拌的作用下将碳酸乙烯酯、催化剂混合均匀;混合液在热媒的加热下达到反应温度,通过第一动力流体泵1-2进入到第一高速喷流撞击管式反应器2;所述配料罐1内温度为70℃,压力为常压,催化剂用量为碳酸乙烯酯质量的0.25%,物料的停留时间为0.75h;In the step (1), 176 kg/h of industrial-grade ethylene carbonate (mass content greater than 99.5%) and 0.44 kg/h of catalyst are introduced into a batching tank 1, and the ethylene carbonate and the catalyst are uniformly mixed under stirring; the mixed liquid reaches the reaction temperature under the heating of a heat medium, and enters the first high-speed jet impact tubular reactor 2 through a first power fluid pump 1-2; the temperature in the batching tank 1 is 70° C., the pressure is normal pressure, the amount of catalyst is 0.25% of the mass of the ethylene carbonate, and the residence time of the material is 0.75 h;
所述步骤(2)来自配料罐1的混合液连续进入到第一高速喷流撞击管式反应器2;配料罐1的混合液通过第一动力流体泵1-2泵入两个相向的第一拉瓦尔喷管2-1,进汽口同时吸入甲醇(质量含量大于99.5%)蒸汽,两股从拉瓦尔管喷出的高速喷流,在高速喷流撞击腔中相互撞击,然后进入第一管式反应器2-4进行酯交换反应,酯交换液连续进入到汽液分离罐3;所述第一高速喷流撞击管式反应器2内温度为80℃,压力为0.2MPa,第一管式反应器2-4长径比为1000,碳酸乙烯酯:甲醇为1:4.4(摩尔比),甲醇282kg/h;In the step (2), the mixed liquid from the batching tank 1 continuously enters the first high-speed jet impact tubular reactor 2; the mixed liquid from the batching tank 1 is pumped into two opposing first Laval nozzles 2-1 by the first power fluid pump 1-2, and the steam inlet simultaneously sucks methanol (mass content greater than 99.5%) vapor, and the two high-speed jets ejected from the Laval tubes collide with each other in the high-speed jet impact chamber, and then enter the first tubular reactor 2-4 for ester exchange reaction, and the ester exchange liquid continuously enters the vapor-liquid separation tank 3; the temperature in the first high-speed jet impact tubular reactor 2 is 80° C., the pressure is 0.2 MPa, the length-to-diameter ratio of the first tubular reactor 2-4 is 1000, the ethylene carbonate:methanol ratio is 1:4.4 (molar ratio), and the methanol is 282 kg/h;
所述步骤(3)来自第一高速喷流撞击管式反应器2酯交换液连续进入到汽液分离罐3,汽液分离罐3将甲醇蒸汽、反应生成的碳酸二甲酯蒸汽与酯交换液分离,分离出的汽体进入到轻组分分离塔系统6;分离出轻组分的酯交换液通过第二动力流体泵3-3进入到第二高速喷流撞击管式反应器4;所述汽液分离罐3内温度为70℃,压力为常压,物料的停留时间为0.75h;In the step (3), the ester exchange liquid from the first high-speed jet impact tubular reactor 2 continuously enters the vapor-liquid separation tank 3, and the vapor-liquid separation tank 3 separates the methanol vapor and the dimethyl carbonate vapor generated by the reaction from the ester exchange liquid, and the separated vapor enters the light component separation tower system 6; the ester exchange liquid with the separated light component enters the second high-speed jet impact tubular reactor 4 through the second power fluid pump 3-3; the temperature in the vapor-liquid separation tank 3 is 70° C., the pressure is normal pressure, and the residence time of the material is 0.75h;
所述步骤(4)来自汽液分离罐3分离出轻组分的酯交换液连续进入到第二高速喷流撞击管式反应器4;汽液分离罐3里分离汽体后的酯交换液通过第二动力流体泵3-3泵入两个相向的第二拉瓦尔喷管4-1,进汽口同时吸入甲醇蒸汽,两股从第二拉瓦尔管4-1喷出的高速喷流,在高速喷流撞击腔中相互撞击,然后进入第二管式反应器4-4进行酯交换反应,从第二高速喷流撞击管式反应器4出来的酯交换液连续进入到熟化罐5;所述第二高速喷流撞击管式反应器4内温度为80℃,压力为0.2MPa,第二管式反应器4-4长径比为1000,碳酸乙烯酯:甲醇为1:4.4(摩尔比),甲醇282kg/h;In the step (4), the ester exchange liquid from which the light components are separated from the vapor-liquid separation tank 3 continuously enters the second high-speed jet impact tubular reactor 4; the ester exchange liquid after the vapor is separated in the vapor-liquid separation tank 3 is pumped into two opposing second Laval nozzles 4-1 through the second power fluid pump 3-3, and the steam inlet simultaneously sucks methanol vapor, and the two high-speed jets ejected from the second Laval tube 4-1 collide with each other in the high-speed jet impact chamber, and then enter the second tubular reactor 4-4 for ester exchange reaction, and the ester exchange liquid from the second high-speed jet impact tubular reactor 4 continuously enters the maturation tank 5; the temperature in the second high-speed jet impact tubular reactor 4 is 80° C., the pressure is 0.2 MPa, the length-to-diameter ratio of the second tubular reactor 4-4 is 1000, the ethylene carbonate:methanol ratio is 1:4.4 (molar ratio), and the methanol is 282 kg/h;
所述步骤(5)来自第二高速喷流撞击管式反应器4的酯交换液连续进入到熟化罐5,在熟化罐5里继续进行补充酯交换反应;从熟化罐5里溢流出来的熟化液进入到轻组分分离塔系统6塔釜;所述熟化罐5内温度为80℃,压力为0.2MPa,物料的停留时间为2h;In the step (5), the ester exchange liquid from the second high-speed jet impact tubular reactor 4 continuously enters the maturation tank 5, and the supplementary ester exchange reaction continues in the maturation tank 5; the aging liquid overflowing from the maturation tank 5 enters the kettle of the light component separation tower system 6; the temperature in the maturation tank 5 is 80° C., the pressure is 0.2 MPa, and the residence time of the material is 2 hours;
所述步骤(6)来自汽液分离罐3、熟化罐5的物料连续进入到轻组分分离塔系统6,轻组分分离塔系统6分离出的轻组分汽体经轻组分冷凝器6-3冷凝进入轻组分液接收罐6-4,部分作为轻组分分离塔系统6的回流,部分进入到甲醇精馏塔系统7;轻组分分离塔系统6的塔釜液通过轻组分分离塔塔底泵6-6连续进入到乙二醇精馏塔系统9;轻组分分离塔系统6塔釜温度为75℃,塔顶温度为64℃,回流比为3,压力为常压;In the step (6), the materials from the vapor-liquid separation tank 3 and the maturation tank 5 continuously enter the light component separation tower system 6, and the light component vapor separated by the light component separation tower system 6 is condensed by the light component condenser 6-3 and enters the light component liquid receiving tank 6-4, part of which is used as the reflux of the light component separation tower system 6, and part of which enters the methanol distillation tower system 7; the bottom liquid of the light component separation tower system 6 continuously enters the ethylene glycol distillation tower system 9 through the light component separation tower bottom pump 6-6; the bottom temperature of the light component separation tower system 6 is 75°C, the top temperature is 64°C, the reflux ratio is 3, and the pressure is normal pressure;
所述步骤(7)来自轻组分分离塔系统6的共沸液连续进入到甲醇精馏塔系统7,甲醇精馏塔系统7塔顶分离出的共沸物蒸汽经甲醇精馏塔冷凝器7-3冷凝进入到甲醇精馏塔共沸液接收罐7-4,部分作为甲醇精馏塔系统7的回流,部分进入到碳酸二甲酯精馏塔系统8;甲醇精馏塔系统7塔釜液经甲醇精馏塔塔底泵7-7进入到甲醇汽化器7-6,汽化的甲醇继续用于酯交换反应;甲醇精馏塔系统7塔底温度为70℃,塔底压力为0.13MPa;塔顶温度为64℃,塔顶压力为常压,回流比为2;In the step (7), the azeotropic liquid from the light component separation tower system 6 continuously enters the methanol distillation tower system 7, and the azeotropic vapor separated from the top of the methanol distillation tower system 7 is condensed by the methanol distillation tower condenser 7-3 and enters the methanol distillation tower azeotropic liquid receiving tank 7-4, part of which is used as the reflux of the methanol distillation tower system 7, and part of which enters the dimethyl carbonate distillation tower system 8; the bottom liquid of the methanol distillation tower system 7 enters the methanol vaporizer 7-6 through the methanol distillation tower bottom pump 7-7, and the vaporized methanol is continuously used for the transesterification reaction; the bottom temperature of the methanol distillation tower system 7 is 70°C, and the bottom pressure is 0.13MPa; the top temperature is 64°C, the top pressure is normal pressure, and the reflux ratio is 2;
所述步骤(8)来自甲醇精馏塔系统7的共沸液连续进入到碳酸二甲酯精馏塔系统8,碳酸二甲酯精馏塔系统8塔顶分离出的共沸物蒸汽经碳酸二甲酯精馏塔冷凝器8-3冷凝进入到碳酸二甲酯精馏塔共沸液接收罐8-4,部分作为碳酸二甲酯精馏塔系统8的回流,部分作为进料返回到甲醇精馏塔系统7;碳酸二甲酯精馏塔系统8塔釜液经碳酸二甲酯精馏塔塔底泵8-7进入到碳酸二甲酯储罐8-6;碳酸二甲酯精馏塔系统8塔底温度为183℃,塔底压力为1.33MPa;塔顶温度为147℃,塔顶压力为1.30MPa,回流比为1.2;碳酸二甲酯采出172kg/h;In the step (8), the azeotropic liquid from the methanol distillation tower system 7 continuously enters the dimethyl carbonate distillation tower system 8, the azeotropic liquid vapor separated from the top of the dimethyl carbonate distillation tower system 8 is condensed by the dimethyl carbonate distillation tower condenser 8-3 and enters the dimethyl carbonate distillation tower azeotropic liquid receiving tank 8-4, part of which is used as reflux of the dimethyl carbonate distillation tower system 8, and part of which is returned to the methanol distillation tower system 7 as feed; the bottom liquid of the dimethyl carbonate distillation tower system 8 enters the dimethyl carbonate storage tank 8-6 through the dimethyl carbonate distillation tower bottom pump 8-7; the bottom temperature of the dimethyl carbonate distillation tower system 8 is 183° C., and the bottom pressure is 1.33 MPa; the top temperature is 147° C., the top pressure is 1.30 MPa, and the reflux ratio is 1.2; 172 kg/h of dimethyl carbonate is produced;
所述步骤(9)来自轻组分分离塔系统6的塔釜液连续进入到乙二醇精馏塔系统9,乙二醇精馏塔系统9塔顶分离出的乙二醇蒸汽经冷凝器9-3冷凝进入到乙二醇接收罐9-4,部分作为乙二醇精馏塔系统9的回流,部分进料进入到乙二醇储罐9-6;乙二醇精馏塔系统9的塔釜液经乙二醇精馏塔塔底泵9-7部分进入乙二醇精馏塔再沸器9-1加热后返回乙二醇精馏塔系统9,部分作为回收催化剂连续进入到配料罐1;乙二醇精馏塔系统9塔顶温度为150℃,塔顶压力为0.02MPa;塔底温度为178℃,回流比为1.5。In the step (9), the bottom liquid from the light component separation tower system 6 continuously enters the ethylene glycol distillation tower system 9, and the ethylene glycol vapor separated from the top of the ethylene glycol distillation tower system 9 is condensed by the condenser 9-3 and enters the ethylene glycol receiving tank 9-4, part of which is used as reflux of the ethylene glycol distillation tower system 9, and part of which is fed into the ethylene glycol storage tank 9-6; the bottom liquid of the ethylene glycol distillation tower system 9 is partially entered into the ethylene glycol distillation tower reboiler 9-1 through the ethylene glycol distillation tower bottom pump 9-7, and then returns to the ethylene glycol distillation tower system 9 after heating, and part of which is continuously entered into the batching tank 1 as a recovered catalyst; the top temperature of the ethylene glycol distillation tower system 9 is 150°C, and the top pressure is 0.02MPa; the bottom temperature is 178°C, and the reflux ratio is 1.5.
本实施例1中碳酸二甲酯收率大于95%。In this embodiment 1, the yield of dimethyl carbonate is greater than 95%.
实施例2Example 2
基于所述高速喷流撞击管式反应器制备碳酸二甲酯的装置的碳酸二甲酯生产方法,包括如下步骤:The method for producing dimethyl carbonate based on the device for preparing dimethyl carbonate using the high-speed jet impingement tubular reactor comprises the following steps:
所述步骤(1)原料工业级碳酸乙烯酯(质量含量大于99.5%)176kg/h、催化剂0.27kg/h进入到配料罐1内,同时在搅拌的作用下将碳酸乙烯酯、催化剂混合均匀;混合液在热媒的加热下达到反应温度,通过第一动力流体泵1-2进入到第一高速喷流撞击管式反应器2;所述配料罐1内温度为75℃,压力为常压,催化剂用量为碳酸乙烯酯质量的0.15%,物料的停留时间为0.5h;In the step (1), 176 kg/h of industrial-grade ethylene carbonate (mass content greater than 99.5%) and 0.27 kg/h of catalyst are introduced into a batching tank 1, and the ethylene carbonate and the catalyst are uniformly mixed under stirring; the mixed liquid reaches the reaction temperature under the heating of a heat medium, and enters the first high-speed jet impact tubular reactor 2 through a first power fluid pump 1-2; the temperature in the batching tank 1 is 75° C., the pressure is normal pressure, the amount of catalyst is 0.15% of the mass of the ethylene carbonate, and the residence time of the material is 0.5 h;
所述步骤(2)来自配料罐1的混合液连续进入到第一高速喷流撞击管式反应器2;配料罐1的混合液通过第一动力流体泵1-2泵入两个相向的第一拉瓦尔喷管2-1,同时吸入甲醇(质量含量大于99.5%)蒸汽,两股从第一拉瓦尔管2-1喷出的高速喷流,在高速喷流撞击腔中相互撞击,然后进入第一管式反应器2-4进行酯交换反应,酯交换液连续进入到汽液分离罐3;所述第一高速喷流撞击管式反应器2内温度为85℃,压力为0.25MPa,第一管式反应器2-4长径比为1000,碳酸乙烯酯:甲醇为1:4(摩尔比),甲醇256kg/h;In the step (2), the mixed liquid from the batching tank 1 continuously enters the first high-speed jet impact tubular reactor 2; the mixed liquid from the batching tank 1 is pumped into two opposing first Laval nozzles 2-1 by the first power fluid pump 1-2, and methanol (mass content greater than 99.5%) vapor is sucked in at the same time, and the two high-speed jets ejected from the first Laval tube 2-1 collide with each other in the high-speed jet impact chamber, and then enter the first tubular reactor 2-4 for ester exchange reaction, and the ester exchange liquid continuously enters the vapor-liquid separation tank 3; the temperature in the first high-speed jet impact tubular reactor 2 is 85° C., the pressure is 0.25 MPa, the length-to-diameter ratio of the first tubular reactor 2-4 is 1000, the ethylene carbonate:methanol ratio is 1:4 (molar ratio), and the methanol is 256 kg/h;
所述步骤(3)来自第一高速喷流撞击管式反应器2酯交换液连续进入到汽液分离罐3,汽液分离罐3将甲醇蒸汽、反应生成的碳酸二甲酯蒸汽与酯交换液分离,分离出的汽体进入到轻组分分离塔系统6;分离出轻组分的酯交换液通过第二动力流体泵3-3进入到第二高速喷流撞击管式反应器4;所述汽液分离罐3内温度为75℃,压力为常压,物料的停留时间为0.5h;In the step (3), the ester exchange liquid from the first high-speed jet impact tubular reactor 2 continuously enters the vapor-liquid separation tank 3, and the vapor-liquid separation tank 3 separates the methanol vapor and the dimethyl carbonate vapor generated by the reaction from the ester exchange liquid, and the separated vapor enters the light component separation tower system 6; the ester exchange liquid with the separated light component enters the second high-speed jet impact tubular reactor 4 through the second power fluid pump 3-3; the temperature in the vapor-liquid separation tank 3 is 75° C., the pressure is normal pressure, and the residence time of the material is 0.5h;
所述步骤(4)来自汽液分离罐3分离出轻组分的酯交换液连续进入到第二高速喷流撞击管式反应器4;汽液分离罐3里分离汽体后的酯交换液通过第二动力流体泵3-3泵入两个相向的第二拉瓦尔喷管4-1,同时吸入甲醇蒸汽,两股从第二拉瓦尔管4-1喷出的高速喷流,在高速喷流撞击腔中相互撞击,然后进入第二管式反应器4-4进行酯交换反应,从第二高速喷流撞击管式反应器4出来的酯交换液连续进入到熟化罐5;所述第二高速喷流撞击管式反应器4内温度为85℃,压力为0.25MPa,第二管式反应器4-4长径比为1000,碳酸乙烯酯:甲醇为1:4(摩尔比),甲醇256kg/h;In the step (4), the ester exchange liquid from which the light components are separated from the vapor-liquid separation tank 3 continuously enters the second high-speed jet impact tubular reactor 4; the ester exchange liquid after the vapor is separated in the vapor-liquid separation tank 3 is pumped into two opposing second Laval nozzles 4-1 through the second power fluid pump 3-3, and methanol vapor is sucked in at the same time, and the two high-speed jets ejected from the second Laval tube 4-1 collide with each other in the high-speed jet impact chamber, and then enter the second tubular reactor 4-4 for ester exchange reaction, and the ester exchange liquid from the second high-speed jet impact tubular reactor 4 continuously enters the maturation tank 5; the temperature in the second high-speed jet impact tubular reactor 4 is 85° C., the pressure is 0.25 MPa, the length-to-diameter ratio of the second tubular reactor 4-4 is 1000, the ethylene carbonate:methanol ratio is 1:4 (molar ratio), and the methanol is 256 kg/h;
所述步骤(5)来自第二高速喷流撞击管式反应器4的酯交换液连续进入到熟化罐5,在熟化罐5里继续进行补充酯交换反应;从熟化罐5里溢流出来的熟化液进入到轻组分分离塔系统6塔釜;所述熟化罐5内温度为85℃,压力为0.25MPa,物料的停留时间为1.5h;In the step (5), the ester exchange liquid from the second high-speed jet impact tubular reactor 4 continuously enters the maturation tank 5, and the supplementary ester exchange reaction continues in the maturation tank 5; the aging liquid overflowing from the maturation tank 5 enters the kettle of the light component separation tower system 6; the temperature in the maturation tank 5 is 85° C., the pressure is 0.25 MPa, and the residence time of the material is 1.5 h;
所述步骤(6)来自汽液分离罐3、熟化罐5的物料连续进入到轻组分分离塔系统6,轻组分分离塔系统6分离出的轻组分汽体经轻组分冷凝器6-3冷凝进入轻组分接收罐6-4,部分作为轻组分分离塔系统6的回流,部分进入到甲醇精馏塔系统7;轻组分分离塔系统6的塔釜液通过分离塔塔底泵连续进入到乙二醇精馏塔系统9;轻组分分离塔系统6塔釜温度为78℃,塔顶温度为66℃,回流比为4,压力为常压;In the step (6), the materials from the vapor-liquid separation tank 3 and the maturation tank 5 continuously enter the light component separation tower system 6, and the light component vapor separated by the light component separation tower system 6 is condensed by the light component condenser 6-3 and enters the light component receiving tank 6-4, part of which is used as the reflux of the light component separation tower system 6, and part of which enters the methanol distillation tower system 7; the bottom liquid of the light component separation tower system 6 continuously enters the ethylene glycol distillation tower system 9 through the bottom pump of the separation tower; the bottom temperature of the light component separation tower system 6 is 78° C., the top temperature is 66° C., the reflux ratio is 4, and the pressure is normal pressure;
所述步骤(7)来自轻组分分离塔系统6的共沸液连续进入到甲醇精馏塔系统7,甲醇精馏塔系统7塔顶分离出的共沸物蒸汽经甲醇精馏塔冷凝器7-3冷凝进入到甲醇精馏塔共沸液接收罐7-4,部分作为甲醇精馏塔系统7的回流,部分进入到碳酸二甲酯精馏塔系统8;甲醇精馏塔系统7塔釜液经甲醇精馏塔塔底泵7-7进入到甲醇汽化器,汽化的甲醇继续用于酯交换反应;甲醇精馏塔系统7塔底温度为70℃,塔底压力为0.13MPa;塔顶温度为64℃,塔顶压力为常压,回流比为2;In the step (7), the azeotropic liquid from the light component separation tower system 6 continuously enters the methanol distillation tower system 7, and the azeotropic vapor separated from the top of the methanol distillation tower system 7 is condensed by the methanol distillation tower condenser 7-3 and enters the methanol distillation tower azeotropic liquid receiving tank 7-4, part of which is used as the reflux of the methanol distillation tower system 7, and part of which enters the dimethyl carbonate distillation tower system 8; the bottom liquid of the methanol distillation tower system 7 enters the methanol vaporizer through the methanol distillation tower bottom pump 7-7, and the vaporized methanol is continuously used for the transesterification reaction; the bottom temperature of the methanol distillation tower system 7 is 70°C, and the bottom pressure is 0.13MPa; the top temperature is 64°C, the top pressure is normal pressure, and the reflux ratio is 2;
所述步骤(8)来自甲醇精馏塔系统7的共沸液连续进入到碳酸二甲酯精馏塔系统8,碳酸二甲酯精馏塔系统8塔顶分离出的共沸物蒸汽经碳酸二甲酯精馏塔冷凝器8-3冷凝进入到碳酸二甲酯精馏塔共沸液接收罐8-4,部分作为碳酸二甲酯精馏塔系统8的回流,部分作为进料返回到甲醇精馏塔系统7;碳酸二甲酯精馏塔系统8塔釜液经碳酸二甲酯精馏塔塔底泵8-7进入到碳酸二甲酯储罐8-6;碳酸二甲酯精馏塔系统8塔底温度为183℃,塔底压力为1.33MPa;塔顶温度为147℃,塔顶压力为1.30MPa,回流比为1.2;碳酸二甲酯采出171.5kg/h;In the step (8), the azeotropic liquid from the methanol distillation tower system 7 continuously enters the dimethyl carbonate distillation tower system 8, the azeotropic liquid vapor separated from the top of the dimethyl carbonate distillation tower system 8 is condensed by the dimethyl carbonate distillation tower condenser 8-3 and enters the dimethyl carbonate distillation tower azeotropic liquid receiving tank 8-4, part of which is used as reflux of the dimethyl carbonate distillation tower system 8, and part of which is returned to the methanol distillation tower system 7 as feed; the bottom liquid of the dimethyl carbonate distillation tower system 8 enters the dimethyl carbonate storage tank 8-6 through the dimethyl carbonate distillation tower bottom pump 8-7; the bottom temperature of the dimethyl carbonate distillation tower system 8 is 183° C., and the bottom pressure is 1.33 MPa; the top temperature is 147° C., the top pressure is 1.30 MPa, and the reflux ratio is 1.2; 171.5 kg/h of dimethyl carbonate is produced;
所述步骤(9)来自轻组分分离塔系统6的塔釜液连续进入到乙二醇精馏塔系统9,乙二醇精馏塔系统9塔顶分离出的乙二醇蒸汽经乙二醇精馏塔冷凝器9-3冷凝进入到乙二醇接收罐9-4,部分作为乙二醇精馏塔系统9的回流,部分进料进入到乙二醇储罐9-6;乙二醇精馏塔系统9的塔釜液经乙二醇精馏塔塔底泵9-7部分进入乙二醇精馏塔再沸器9-1加热后返回乙二醇精馏塔系统9,部分作为回收催化剂连续进入到配料罐1;乙二醇精馏塔系统9塔顶温度为150℃,塔顶压力为0.02MPa;塔底温度为178℃,回流比为1.5。In the step (9), the bottom liquid from the light component separation tower system 6 continuously enters the ethylene glycol distillation tower system 9, and the ethylene glycol vapor separated from the top of the ethylene glycol distillation tower system 9 is condensed by the ethylene glycol distillation tower condenser 9-3 and enters the ethylene glycol receiving tank 9-4, part of which is used as reflux of the ethylene glycol distillation tower system 9, and part of which is fed into the ethylene glycol storage tank 9-6; the bottom liquid of the ethylene glycol distillation tower system 9 is partially entered into the ethylene glycol distillation tower reboiler 9-1 through the ethylene glycol distillation tower bottom pump 9-7, and then returns to the ethylene glycol distillation tower system 9 after heating, and part of which is continuously entered into the batching tank 1 as a recovered catalyst; the top temperature of the ethylene glycol distillation tower system 9 is 150°C, and the top pressure is 0.02MPa; the bottom temperature is 178°C, and the reflux ratio is 1.5.
本实施例中碳酸二甲酯收率大于95%。In this embodiment, the yield of dimethyl carbonate is greater than 95%.
本发明的高速喷流撞击管式反应器制备碳酸二甲酯的生产方法;碳酸二甲酯质量高于HG/T 5391-2018工业级碳酸二甲酯的标准。The invention discloses a production method for preparing dimethyl carbonate by using a high-speed jet impact tubular reactor; the quality of dimethyl carbonate is higher than the standard of HG/T 5391-2018 industrial-grade dimethyl carbonate.
以上技术方案阐述了本发明的技术思路,不能以此限定本发明的保护范围,凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上技术方案所作的任何改动及修饰,均属于本发明技术方案的保护范围。The above technical scheme illustrates the technical idea of the present invention, but cannot be used to limit the protection scope of the present invention. Any changes and modifications made to the above technical scheme based on the technical essence of the present invention without departing from the content of the technical scheme of the present invention shall fall within the protection scope of the technical scheme of the present invention.
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