CN109364510B - Device for extracting high-purity methyl formate from by-product of preparing ethylene glycol by dimethyl oxalate hydrogenation - Google Patents
Device for extracting high-purity methyl formate from by-product of preparing ethylene glycol by dimethyl oxalate hydrogenation Download PDFInfo
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- CN109364510B CN109364510B CN201811331028.8A CN201811331028A CN109364510B CN 109364510 B CN109364510 B CN 109364510B CN 201811331028 A CN201811331028 A CN 201811331028A CN 109364510 B CN109364510 B CN 109364510B
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- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 title claims abstract description 108
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 101
- LOMVENUNSWAXEN-UHFFFAOYSA-N Methyl oxalate Chemical compound COC(=O)C(=O)OC LOMVENUNSWAXEN-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000006227 byproduct Substances 0.000 title claims abstract description 28
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 19
- 238000009826 distribution Methods 0.000 claims abstract description 54
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 239000000047 product Substances 0.000 claims abstract description 31
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000010992 reflux Methods 0.000 claims description 20
- 238000012856 packing Methods 0.000 claims description 18
- 239000000945 filler Substances 0.000 claims description 15
- 238000007789 sealing Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000035484 reaction time Effects 0.000 abstract description 4
- 238000012824 chemical production Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- BLLFVUPNHCTMSV-UHFFFAOYSA-N methyl nitrite Chemical compound CON=O BLLFVUPNHCTMSV-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 5
- 238000003860 storage Methods 0.000 description 3
- -1 terylene (dacron) Chemical class 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920000298 Cellophane Polymers 0.000 description 1
- 229920004934 Dacron® Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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Classifications
-
- 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
- B01D3/146—Multiple effect distillation
-
- 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
- B01D3/322—Reboiler specifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a device for extracting high-purity methyl formate from a byproduct in preparation of ethylene glycol by dimethyl oxalate hydrogenation, and relates to the technical field of chemical production. Comprises a rectifying tower and a product tower; wherein the trough-type liquid distributor in the rectifying tower and the product tower comprises: the device comprises a primary tank and a secondary tank, wherein a buffer tank is arranged in the primary tank; the secondary groove comprises a plurality of parallel distribution grooves, and the primary groove and the secondary groove are in a vertical structure; t-shaped baffles are alternately arranged on two side walls in the distribution groove, and transverse baffles of the T-shaped baffles are connected with the inner side wall of the distribution groove. The groove type liquid distributor is characterized in that the two side walls in the distribution groove are alternately provided with the T-shaped baffles, the T-shaped baffles prolong the contact time of gas and liquid, and the reaction time is ensured to achieve the expected separation effect.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a device for extracting high-purity methyl formate from a byproduct generated in preparation of ethylene glycol by hydrogenation of dimethyl oxalate.
Background
The ethylene glycol is commonly named as glycol, has wide application, can be used for synthesizing high molecular compounds such as terylene (dacron), and the like, can also be used as raw materials such as films, rubber, plasticizers, drying agents, brake oil, and the like, is a common high boiling point solvent, has a freezing point of 60 percent of aqueous solution of-40 ℃, and can be used as an anti-freezing agent of an automobile radiator in winter and a refrigerant of an aircraft engine. Ethylene glycol can also be used as a wetting agent for cellophane, fiber, leather, adhesives. The vapor produced by heating ethylene glycol can be used as stage smoke, and the nitrate ester of ethylene glycol is an explosive.
The ethylene glycol production process comprises an ethylene oxide hydration method, oxalate hydrogenation and the like. The method for preparing ethylene glycol by hydrogenating oxalate, particularly preparing ethylene glycol by hydrogenating dimethyl oxalate, is applied more and more in recent years, and comprises the following specific preparation processes: NO with methanol and O2Methyl nitrite is generated through reaction, dimethyl oxalate is synthesized by the methyl nitrite and CO, and then ethylene glycol is prepared through dimethyl oxalate hydrogenation. A certain amount of methyl formate by-product is generated in the process of preparing ethylene glycol, for example, methyl formate by-product with the meaning of about 15% in dimethyl carbonate component separated in the process of synthesizing dimethyl oxalate, and a certain amount of methyl formate by-product is also generated in the process of synthesizing ethylene glycol from dimethyl oxalate.
The traditional treatment method for methyl formate in the byproduct of ethylene glycol preparation by hydrogenation of dimethyl ester is mainly incineration treatment, although medium-pressure steam of 4.0MPa can be generated. However, the treatment method does not effectively recycle the methyl formate, which results in resource waste.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a device for extracting high-purity methyl formate from a byproduct in the process of preparing ethylene glycol by hydrogenating dimethyl oxalate, and solves the problem of resource waste caused by the fact that the byproduct methyl formate in the process of preparing ethylene glycol by hydrogenating dimethyl oxalate cannot be effectively recycled.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
a device for extracting high-purity methyl formate from a byproduct of ethylene glycol preparation by dimethyl oxalate hydrogenation comprises a rectifying tower and a product tower;
the rectifying tower is sequentially provided with a reflux distributor, a groove type liquid distributor, a filler section, a groove type liquid distributor with a collecting function, a filler section, a first feeding distribution pipe, a groove type liquid distributor with a collecting function, a filler section, a second feeding distribution pipe, a tower tray, a liquid sealing cover and a gas distributor from top to bottom;
the product tower is sequentially provided with a reflux distributor, a groove type liquid distributor, a filler section, a groove type liquid distributor with a collecting function, a filler section, a first feeding distribution pipe, a groove type liquid distributor with a collecting function, a filler section, a second feeding distribution pipe, a tower tray, a second feeding distribution pipe, a liquid sealing cover and a gas distributor from top to bottom;
the groove type liquid distributor and the liquid distributor with the collecting groove are structurally different only in that whether the collecting groove type liquid distributor has a collecting function or not is judged, and other structures are the same;
the trough-type liquid distributor comprises: the device comprises a primary tank and a secondary tank, wherein a buffer tank is arranged in the primary tank; the secondary groove comprises a plurality of parallel distribution grooves, and the primary groove and the secondary groove are in a vertical structure;
t-shaped baffles are alternately arranged on two side walls in the distribution groove, and the transverse baffles of the T-shaped baffles are connected with the inner side wall of the distribution groove.
Preferably, the packing section sequentially comprises a packing pressing ring, regular packing and a packing support from top to bottom.
Preferably, a baffle plate is arranged at the lower end position of the outer side wall of the distribution groove.
Preferably, the gas distributor comprises a main pipe, a plurality of branch pipes are distributed on the side wall of the main pipe, and through holes are uniformly distributed on the upper walls of the main pipe and the branch pipes.
Preferably, the upper end or/and the lower end of the distribution groove is/are provided with a V-shaped through groove.
Preferably, the side wall or the bottom plate of the primary groove is provided with distribution holes, and the position of the opening hole corresponds to the secondary groove; and the side part of the lower end position of the side part of the secondary groove is provided with distribution holes.
(III) advantageous effects
The invention provides a device for extracting high-purity methyl formate from a byproduct in preparation of ethylene glycol by dimethyl oxalate hydrogenation. Compared with the prior art, the method has the following beneficial effects:
the invention adopts the two-tower process design to purify the methyl formate in the ethylene glycol byproduct prepared by dimethyl oxalate hydrogenation, fully ensures the recovery rate of resources, avoids the problem that the methyl formate cannot be effectively recycled due to the mixed components of the byproduct, has the recovery rate of over 99 percent, increases the economic benefit of enterprises, and can save the cost of the enterprises for treating the byproduct.
The groove type liquid distributor is characterized in that the two side walls in the distribution groove are alternately provided with the T-shaped baffles, the T-shaped baffles prolong the contact time of gas and liquid, and the reaction time is ensured to achieve the expected separation effect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram showing the overall structure of a rectifying column according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the overall structure of a product tower according to an embodiment of the present invention;
FIG. 3 is a top view of an integral trough liquid distributor of an embodiment of the present invention;
FIG. 4 is a schematic view of the overall structure of a gas distributor according to an embodiment of the present invention;
fig. 5 is a first structural view of a distribution groove according to an embodiment of the present invention;
fig. 6 is a second structural view of the distribution groove according to the embodiment of the present invention;
FIG. 7 is a schematic structural view of an integral trough-type liquid distributor according to an embodiment of the present invention;
FIG. 8 is a flow chart of a process for extracting high purity methyl formate from a byproduct generated in the preparation of ethylene glycol by hydrogenation of dimethyl oxalate according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Because methyl formate is a light component and is volatile, the methyl formate meets high requirements on collection and storage of raw materials and rectification separation, and in order to solve the problem, the embodiment of the invention provides a device for extracting high-purity methyl formate from a byproduct in the process of preparing ethylene glycol by hydrogenating dimethyl oxalate,
as shown in fig. 1 to 8, a device for extracting high-purity methyl formate from a byproduct generated in the preparation of ethylene glycol by dimethyl oxalate hydrogenation comprises a rectifying tower A and a product tower B; the outlet of the rectifying tower A is divided into a tower bottom heavy component liquid phase outlet and a tower top light component gas phase outlet, and the outlet liquid phase at the bottom of the rectifying tower A enters the inlet in the middle of the product tower B and is connected with the inlet through a pipeline.
As shown in fig. 1 and 2, the rectifying tower a is provided with a reflux distributor 1, a trough type liquid distributor 2, a packing section, a trough type liquid distributor with collection 6, a packing section, a first feeding distributor 7, a trough type liquid distributor with collection 8, a packing section, a second feeding distributor 10, a tray 9, a liquid cover 11, and a gas distributor 13 in sequence from top to bottom;
wherein, the groove type liquid distributor 2 and the groove type liquid distributor with collection 6 are different in structure only in that whether a collection function is provided or not, and other structures are the same.
The first feeding distribution pipe 7 distributes coarse methyl formate, and the coarse methyl formate enters the first feeding distribution pipe 7 to be distributed; the second feeding distribution pipe 10 is distributed with alcohol-containing wastewater;
the product tower B is sequentially provided with a reflux distributor 1, a groove type liquid distributor 2, a filler section, a groove type liquid distributor with a collection function 6, a filler section, a first feeding distribution pipe 7, a groove type liquid distributor with a collection function 6, a filler section, a second feeding distribution pipe 10, a tower tray 9, a second feeding distribution pipe 10, a liquid seal cover 11 and a gas distributor 13 from top to bottom;
the structures in the rectifying columns a and a product column B, such as the reflux distributor 1, the groove-type liquid distributor 2, the packing section, the groove-type liquid distributor with collection 6, the first feeding distributor 7, the groove-type liquid distributor with collection 8, the tray 9, the second feeding distributor 10, the liquid seal cover 11, the gas distributor 13, and the like, are the same in specific structure, and only have differences in size.
With reference to fig. 1 and 2, the reflux distributor 1 is fixed on a reflux distribution pipe support 1-1, the trough liquid distributor 2 is fixed on a trough liquid distributor support 2-1, wherein the packing section comprises a packing clamping ring 3, a structured packing 4 and a packing support 5 from top to bottom, and the packing section is arranged in the tower through a packing support welding part 3-1; the first feeding distribution pipe 7 is fixed on the first feeding distribution pipe support 5-1, and the second feeding distribution pipe 10 is fixed on the second feeding distribution pipe support 6-1; the tray 9 is fixed on the tray welding piece 7-1, and the liquid sealing cover 11 is fixed on the liquid sealing tray welding piece 9-1.
As shown in fig. 3, the trough type liquid distributor 2 includes: the device comprises a primary tank 201 and a secondary tank, wherein a buffer tank 203 is arranged in the primary tank 201; the secondary groove comprises a plurality of parallel distribution grooves 202, and the primary groove 201 and the secondary groove are in a vertical structure;
t-shaped baffles 2023 are alternately distributed on two side walls in the distribution groove 202, and transverse baffles of the T-shaped baffles are connected with the inner side walls of the distribution groove 202. The T-shaped baffle 2023 plays a certain role in stopping in the operation process of the device, so that the contact time of gas and liquid is prolonged, and the reaction time is ensured to achieve the expected separation effect.
In the specific implementation, the baffle 2024 is disposed at the lower end of the outer sidewall of the distribution groove 202, so as to ensure the reaction time to reach the desired separation effect.
In a specific implementation process, as shown in fig. 4, the gas distributor 13 includes a main pipe 1301, a plurality of branch pipes 1302 are distributed on a side wall of the main pipe 1301, and through holes 1303 are uniformly distributed on upper walls of the main pipe and the branch pipes. After the gas enters the main pipe 1301, part of the gas flows out from the through holes 1303 in the main pipe 1301, part of the gas enters the branch pipe 1302, and then the gas flows out from the through holes 1303 in the branch pipe 1302.
In a specific implementation process, a V-shaped through groove 2021 is arranged at the upper end or/and the lower end of the distribution groove 202. The V-shaped through groove 2021 is connected to the distribution groove 202 as shown in fig. 5 and 6, and is used for stabilizing the flow distribution, so that the fluid flows through the channel and the turbulent flow and the uneven distribution are prevented.
In a specific implementation process, the side wall or the bottom plate of the primary groove 201 is provided with distribution holes, and the position of the distribution holes corresponds to the secondary groove; and the side part of the lower end position of the side part of the secondary groove is provided with distribution holes.
In the specific implementation of the above device, since methyl formate is a light component and is volatile, high requirements are put on the collection and storage of raw materials and the rectification separation, and to solve the problem, the embodiment of the present invention provides a method for extracting high purity methyl formate from a byproduct of ethylene glycol preparation by dimethyl oxalate hydrogenation, which includes the following steps:
s1: the method takes a byproduct of preparing the ethylene glycol by hydrogenating dimethyl oxalate as a raw material, and the raw material comprises a dimethyl carbonate crude substance separated in the process of synthesizing the dimethyl oxalate and the byproduct of synthesizing the ethylene glycol by using the dimethyl oxalate.
The raw material is sent to a rectifying tower A through a rectifying tower feed pump 1003 to remove methyl nitrite, a mixture of methyl formate and methyl nitrite is discharged from the top of the rectifying tower A, a mixture of methyl formate and a heavy component is discharged from the bottom of the rectifying tower A, and the main component of the heavy component is methanol;
in the step S1, the pressure of the rectifying tower is controlled to be 0.5-1 MPaG, the top of the rectifying tower is provided with a tower top rectifying tower condenser 1004, a rectifying tower reflux tank 1002 and a rectifying tower reflux pump 1005, and the bottom of the rectifying tower is provided with a thermosiphon rectifying tower reboiler 1001; in the specific implementation, in the step S1, the top temperature of the rectifying tower is 50 to 60 ℃, the bottom temperature of the rectifying tower is 100 to 110 ℃, and the reflux ratio is 30 to 31.
S2: sending a mixture of methyl formate and heavy components from the bottom of the tower to the lower part of a methyl formate product tower B, sending methyl formate from the top of the methyl formate product tower B, and outputting the heavy components containing the methyl formate from the bottom of the tower through a product tower bottom pump 2022, wherein the main component of the heavy components is methanol; in the step S2, the pressure of the methyl formate product column B is controlled to 0.07 to 0.12MPaG, the top of the methyl formate product column B is provided with a top product column condenser 2005, a product column reflux tank 2003 and a product column reflux pump 204, and the bottom of the methyl formate product column B is provided with a thermosiphon product column reboiler 201. In the specific implementation, in the step S2, the top temperature of the methyl formate product tower is 50-55 ℃, the bottom temperature of the methyl formate product tower is 70-75 ℃, and the reflux ratio is 3-4.
In specific implementation, the raw material feeding temperature is 35-45 ℃.
In specific implementation, the by-product of preparing ethylene glycol by dimethyl oxalate hydrogenation is collected and stored in a low-temperature pressurizing mode, so that the volatilization of methyl formate components in the raw materials is avoided.
In specific implementation, the low-temperature pressurized storage conditions are as follows: the temperature is below 20 ℃ and the pressure is above 0.3 MPa.
The methyl nitrite product is removed by adopting a two-tower flow design and the rectifying tower A. The mixed raw material crude methyl formate is sent to the upper part of a rectifying tower A through a rectifying tower feed pump 103, and is in countercurrent contact with ascending light components in the tower, the heavy components descend, the light components ascend, a mixture of methyl formate and methyl nitrite is discharged from the top of the rectifying tower A, the mixture enters a tower top condenser and is condensed by circulating water, condensate enters a reflux tank, a part of condensate returns to the tower through a reflux pump and flows back, and the rest is sent to the outside for recovery; the bottom of the rectifying tower A is provided with a thermosyphon reboiler which provides a heat source for rectification, and the bottom of the tower produces a mixture of methyl formate and heavy components. The rectifying tower A is operated at high pressure.
And the product at the bottom of the rectifying tower A is sent to the lower part of a methyl formate product tower B by the self pressure, and the methyl formate product tower B realizes the rectification and purification of the methyl formate product. Qualified methyl formate is discharged from the tower top of the methyl formate product tower B, enters a tower top condenser and is condensed by circulating water, condensate enters a reflux tank, a part of condensate returns to the tower through a reflux pump for reflux, and the rest is sent to the outside for recovery; the bottom of the rectifying tower is provided with a thermosyphon reboiler which provides a heat source for rectification. Heavy components containing methyl formate are discharged from the bottom of the tower.
The device is used for extracting high-purity methyl formate from a byproduct of ethylene glycol preparation by dimethyl oxalate hydrogenation, the product quality meets the requirement of superior products in GB/T33105-2016 methyl formate for industrial use, and the recovery rate of methyl formate is over 99 percent.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. A device for extracting high-purity methyl formate from a byproduct of ethylene glycol preparation by dimethyl oxalate hydrogenation is characterized by comprising a rectifying tower and a product tower;
the rectifying tower is sequentially provided with a reflux distributor, a groove type liquid distributor, a filler section, a groove type liquid distributor with a collecting groove, a filler section, a first feeding distribution pipe, a groove type liquid distributor with a collecting groove, a filler section, a second feeding distribution pipe, a tower tray, a liquid sealing cover and a gas distributor from top to bottom;
the product tower is sequentially provided with a reflux distributor, a groove type liquid distributor, a filler section, a groove type liquid distributor with a collecting function, a filler section, a first feeding distribution pipe, a groove type liquid distributor with a collecting function, a filler section, a second feeding distribution pipe, a tower tray, a second feeding distribution pipe, a liquid sealing cover and a gas distributor from top to bottom;
the trough-type liquid distributor comprises: the device comprises a primary tank and a secondary tank, wherein a buffer tank is arranged in the primary tank; the secondary groove comprises a plurality of parallel distribution grooves, and the primary groove and the secondary groove are in a vertical structure;
the groove type liquid distributor and the liquid distributor with the collecting groove are structurally different only in that whether the collecting groove type liquid distributor has a collecting function or not is judged, and other structures are the same;
t-shaped baffles are alternately arranged on two side walls in the distribution groove, and the transverse baffles of the T-shaped baffles are connected with the inner side wall of the distribution groove.
2. The apparatus for extracting high-purity methyl formate from the by-product of ethylene glycol preparation by dimethyl oxalate hydrogenation according to claim 1, wherein the packing section comprises a packing pressing ring, a structured packing and a packing support from top to bottom in sequence.
3. The apparatus for extracting high-purity methyl formate from the by-product of ethylene glycol preparation by hydrogenation of dimethyl oxalate as claimed in claim 1, wherein a baffle is provided at a lower end position of the outer sidewall of the distribution tank.
4. The apparatus according to claim 1, wherein the gas distributor comprises a main pipe, a plurality of branch pipes are arranged on the side wall of the main pipe, and through holes are uniformly distributed on the upper walls of the main pipe and the branch pipes.
5. The apparatus for extracting high-purity methyl formate from the by-product of ethylene glycol preparation by dimethyl oxalate hydrogenation according to claim 1, wherein the upper end or/and the lower end of the distribution groove is/are provided with a V-shaped through groove.
6. The device for extracting high-purity methyl formate from the by-product of preparing ethylene glycol by hydrogenating dimethyl oxalate according to claim 1, wherein the side wall or the bottom plate of the primary tank is provided with distribution holes, and the positions of the distribution holes correspond to those of the secondary tank; and the side part of the lower end position of the side part of the secondary groove is provided with distribution holes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811331028.8A CN109364510B (en) | 2018-11-09 | 2018-11-09 | Device for extracting high-purity methyl formate from by-product of preparing ethylene glycol by dimethyl oxalate hydrogenation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811331028.8A CN109364510B (en) | 2018-11-09 | 2018-11-09 | Device for extracting high-purity methyl formate from by-product of preparing ethylene glycol by dimethyl oxalate hydrogenation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109364510A CN109364510A (en) | 2019-02-22 |
| CN109364510B true CN109364510B (en) | 2020-09-25 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9457291B2 (en) * | 2013-06-21 | 2016-10-04 | Praxair Technology, Inc. | Combined collector and distributor |
| CN206081707U (en) * | 2016-10-12 | 2017-04-12 | 宁夏佰斯特医药化工有限公司 | Methyl alcohol rectifying column |
| CN206342938U (en) * | 2016-12-31 | 2017-07-21 | 山东飞源科技有限公司 | Continuous rectification apparatus for preparing high-purity Nitrogen trifluoride |
| CN207525007U (en) * | 2017-09-30 | 2018-06-22 | 江苏迈克化工机械有限公司 | A kind of low-concentration ammonia-nitrogen removes equipment |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9457291B2 (en) * | 2013-06-21 | 2016-10-04 | Praxair Technology, Inc. | Combined collector and distributor |
| CN206081707U (en) * | 2016-10-12 | 2017-04-12 | 宁夏佰斯特医药化工有限公司 | Methyl alcohol rectifying column |
| CN206342938U (en) * | 2016-12-31 | 2017-07-21 | 山东飞源科技有限公司 | Continuous rectification apparatus for preparing high-purity Nitrogen trifluoride |
| CN207525007U (en) * | 2017-09-30 | 2018-06-22 | 江苏迈克化工机械有限公司 | A kind of low-concentration ammonia-nitrogen removes equipment |
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| CN109364510A (en) | 2019-02-22 |
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