CN118026803B - Crude benzene hydrofining device and method - Google Patents
Crude benzene hydrofining device and method Download PDFInfo
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- CN118026803B CN118026803B CN202410443533.0A CN202410443533A CN118026803B CN 118026803 B CN118026803 B CN 118026803B CN 202410443533 A CN202410443533 A CN 202410443533A CN 118026803 B CN118026803 B CN 118026803B
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 title claims abstract description 205
- 238000000034 method Methods 0.000 title claims abstract description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 95
- 238000000605 extraction Methods 0.000 claims abstract description 45
- 239000007788 liquid Substances 0.000 claims abstract description 35
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000008096 xylene Substances 0.000 claims abstract description 33
- 238000011084 recovery Methods 0.000 claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- 239000000203 mixture Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 claims abstract description 13
- 238000005194 fractionation Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 20
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 18
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000005711 Benzoic acid Substances 0.000 claims description 9
- 235000010233 benzoic acid Nutrition 0.000 claims description 9
- 210000003437 trachea Anatomy 0.000 claims 4
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 10
- 238000007670 refining Methods 0.000 abstract description 9
- 230000001976 improved effect Effects 0.000 abstract description 7
- 239000007789 gas Substances 0.000 description 24
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 15
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 9
- 238000000895 extractive distillation Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- JYFHYPJRHGVZDY-UHFFFAOYSA-N Dibutyl phosphate Chemical compound CCCCOP(O)(=O)OCCCC JYFHYPJRHGVZDY-UHFFFAOYSA-N 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 230000001737 promoting effect Effects 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008093 supporting effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- 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
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/38—Steam 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
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive distillation
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/34—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of chromium, molybdenum or tungsten
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
- C07C7/163—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound by hydrogenation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention is applicable to the technical field of crude benzene hydrogenation, and provides a crude benzene hydrofining device and a crude benzene hydrofining method, wherein the method comprises the following steps: step one: heating crude benzene by a heater, and fractionating the heated crude benzene in a fractionating tower through a crude benzene inlet pipe; step two: introducing the benzene fraction obtained after fractionation into an extraction rectifying tower for extraction and rectification; step three: the mixture extracted from the bottom of the extraction rectifying tower enters an extractant recovery tower, and pure benzene is obtained from the top of the recovery tower; step four: the mixture of toluene and xylene is obtained at the bottom of the fractionating tower, the mixture is introduced into a stripping tower, toluene is obtained at the top of the stripping tower, xylene is obtained at the middle part of the stripping tower, and the xylene sequentially passes through a third condenser and a third gas-liquid separator to reach a xylene collecting tank; step five: the catalyst at the bottom of the stripping tower sequentially passes through the water absorption tower, the filter and the filter centrifuge and returns to the fractionating tower, so that the temperature of the fractionating tower is controlled by matching the circulating pump with the radiator, and the refining effect is improved.
Description
Technical Field
The invention is suitable for the technical field of crude benzene hydrogenation, and provides a crude benzene hydrofining device and a crude benzene hydrofining method.
Background
At present, crude benzene hydrofining is a main means for refining crude benzene instead of the traditional acid washing process, and the technology is mainly characterized in that the process is environment-friendly, the content of sulfur and nitrogen impurities in the obtained hydrogenation product is low, and low-sulfur and low-nitrogen pure benzene, toluene and mixed xylene products can be obtained after subsequent refining. The hydrogenated product is mainly benzene, toluene and xylene and contains a large amount of non-aromatic hydrocarbons which are close to the boiling point of aromatic hydrocarbons or form azeotropes. In order to remove non-aromatic hydrocarbons in hydrogenated oil and obtain various aromatic hydrocarbon products, the separation process of the hydrogenated products at present basically adopts an extraction and rectification process, and the separation process of the traditional process is as follows: the hydrogenated oil firstly enters a main fractionating tower, xylene and heavy components are extracted from the tower bottom, the xylene products are further refined by a xylene removing tower, benzene, toluene and light components are extracted from the tower top, non-aromatic hydrocarbon is removed by an extraction and rectification system, and then pure benzene and toluene are respectively obtained by a pure benzene tower and a toluene tower in sequence.
In the prior art, the purity of the obtained toluene and xylene is lower in the refining process of the crude benzene; and the reaction is more severe in the process of introducing hydrogen, and the temperature variation in the fractionating tower is more severe, so that the refining effect is influenced.
Disclosure of Invention
In view of the above-mentioned drawbacks, the present invention provides a crude benzene hydrofining apparatus and method, which aims to solve the problems in the background, and includes the following steps:
step one: heating crude benzene by a heater, feeding the heated crude benzene into a fractionating tower through a crude benzene inlet pipe, and simultaneously introducing steam and hydrogen into the fractionating tower to fractionate the crude benzene;
step two: introducing the benzene fraction obtained after fractionation into an extraction rectifying tower for extraction rectification, and introducing an extractant into an extractant recovery tower from the extraction rectifying tower;
Step three: the mixture extracted from the bottom of the extraction rectifying tower enters an extractant recovery tower, pure benzene is obtained from the top of the recovery tower, and the pure benzene sequentially passes through a first condenser and a first gas-liquid separator and enters a first collecting tank;
Step four: the method comprises the steps that a mixture of toluene and xylene is obtained at the bottom of a fractionating tower, the mixture is introduced into a stripping tower, toluene is obtained at the top of the stripping tower, the toluene sequentially passes through a second condenser and a second gas-liquid separator to reach a toluene collecting tank, xylene is obtained at the middle of the stripping tower, and the xylene sequentially passes through a third condenser and a third gas-liquid separator to reach the xylene collecting tank;
step five: the catalyst at the bottom of the stripping tower sequentially passes through a water absorption tower, a filter and a filter centrifuge and returns to the fractionating tower.
Further, the heater temperature is 30-50 ℃.
Further, the catalyst comprises molybdenum trioxide, benzoic acid and zirconia.
The utility model provides a used device of crude benzene hydrofining method, includes the heater, the export intercommunication of heater has the entry of fractionating tower, the fractionating tower top is provided with the intake pipe, the top of the tower gaseous phase exit tube of fractionating tower is connected with the entry of extraction rectifying tower, the top of the extraction rectifying tower is equipped with the extractant entry, the top of the tower exit linkage of extraction rectifying tower has the entry of stripper, the export intercommunication of stripper has the second collecting vessel, the rectification export intercommunication of extraction rectifying tower has the entry of extractant recovery tower, extractant recovery tower top export has connected gradually first condenser, first gas-liquid separator, first collecting vessel, extractant recovery tower bottom is connected with the extractant entry of extraction rectifying tower, the discharge pipe intercommunication of fractionating tower has the entry of extraction rectifying tower, the upper portion export of extraction rectifying tower has connected gradually second condenser, second gas-liquid separator, toluene collecting vessel, the middle part export of extraction rectifying tower has connected gradually third condenser, third gas-liquid separator, xylene collecting vessel, the filter inlet connection has the entry of filter, the filter inlet connection of filter tower bottom has the entry.
Further, an air inlet pipe is arranged at the top of the fractionating tower, a crude benzene inlet pipe is arranged on the side wall of the fractionating tower, a steam inlet pipe is arranged at the lower part of the fractionating tower, a discharge pipe is arranged at the bottom of the fractionating tower, an air distribution pipe is communicated with the air inlet pipe, and a plurality of baffles are arranged below the air distribution pipe.
Further, the cooling tube is installed to the fractionating tower outer wall, the cooling tube has radiator, circulating pump in proper order intercommunication.
Further, the gas-distributing pipe comprises an outer shell, an inner shell is arranged on the inner wall of the outer shell, a hollow structure is arranged between the outer shell and the inner shell and is communicated with the gas inlet pipe, and a plurality of gas-distributing holes are formed in the inner shell.
Further, the gas-distributing pipe is of a conical structure.
Further, the baffle is cylindrical structure, the baffle both ends are feed end and discharge end respectively, the feed end diameter is greater than the discharge end diameter.
Further, the side wall of the baffle is provided with a plurality of through holes which are uniformly distributed.
Advantageous effects
According to the method, the removal of impurities in crude benzene is promoted by the molybdenum trioxide catalyst, so that the purity and quality of a product are improved; benzoic acid reduces the activation energy of hydrogenation reaction, thereby improving the reaction rate and the product purity; the surface of the zirconia has moderate acid and alkali, which is favorable for adsorbing and activating reactant molecules and promoting the hydrogenation reaction; the gas distribution pipe of the fractionating tower distributes hydrogen to prevent hydrogen from over-reacting; the baffle is matched with the gas distribution pipe to enhance the uniformity of the reaction; the stripping tower separates the toluene and the xylene, and the obtained catalyst returns to the fractionating tower after being treated, so that the use is convenient; the circulating pump is matched with the radiator to control the temperature of the fractionating tower and improve the refining effect.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is an isometric view of a fractionation column of the present invention;
FIG. 3 is a schematic diagram of the interior of the fractionation column of the present invention;
FIG. 4 is an isometric view of a baffle of the fractionation column of the present invention;
FIG. 5 is a vapor distribution tube isometric view of the fractionation column of the present invention;
fig. 6 is an isometric view of a radiator of the fractionation column of the present invention.
In the figure, 1-heater, 2-fractionating tower, 201-sealing cover, 202-supporting leg, 203-radiating pipe, 204-baffle, 205-through hole, 206-feeding end, 207-discharging end, 208-gas distributing pipe, 209-outer shell, 210-inner shell, 211-gas distributing hole, 212-gas inlet end, 213-gas outlet end, 214-radiator, 215-shell, 216-fixed frame, 217-fan blade, 218-motor, 219-copper pipe, 220-circulating pump, 3-crude benzene inlet pipe, 4-steam inlet pipe, 5-catalyst inlet pipe, 6-gas inlet pipe, 7-gas phase outlet pipe, 8-discharging pipe, 9-second collecting tank, 10-stripping tower, 11-extraction rectifying tower, 12-rectifying inlet, 13-overhead outlet, 14-extractant inlet, 15-rectifying outlet, 16-extractant recovering tower, 17-heat exchanger, 18-first condenser, 19-first gas-liquid separator, 20-first collecting tank, 21-stripping tower, 22-second condenser, 23-second condenser, 24-liquid separator, 24-toluene separator, 26-third collecting tank, 25-toluene separator, and third collecting tank, and water separator, and third filter.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Referring to fig. 1 to 6, the invention aims to provide a crude benzene hydrofining device, which comprises a heater 1, wherein the heater 1 is a tube furnace, and is provided with an inlet for feeding crude benzene raw materials; the outlet of the heater 1 is communicated with a crude benzene inlet pipe 3 of the fractionating tower 2; the side wall of the fractionating tower 2 is provided with a steam inlet pipe 4 for introducing external steam; an air inlet pipe 6 is arranged at the top of the fractionating tower 2, and hydrogen is introduced into the air inlet pipe 6; the top gas phase outlet pipe 7 of the fractionating tower 2 is communicated with a rectifying inlet 12 of the extraction rectifying tower 11; the top of the extraction rectifying tower 11 is provided with an extractant inlet 14, the top outlet 13 of the extraction rectifying tower 11 is connected with the inlet of the stripping tower 10, and the outlet of the stripping tower 10 is communicated with the second collecting tank 9; the bottom of the extractive distillation column 11 is communicated with an inlet of an extractant recovery column 16 through a distillation outlet 15, the top outlet of the extractant recovery column 16 is sequentially connected with a first condenser 18, a first gas-liquid separator 19 and a first collecting tank 20, and the bottom outlet of the extractant recovery column 16 is connected with an extractant inlet 14 at the top of the extractive distillation column 11 through a heat exchanger 17.
The outlet pipe 8 of the fractionating tower 2 is communicated with the inlet of the stripping tower 21; the upper outlet of the stripping tower 21 is sequentially communicated with a second condenser 22, a second gas-liquid separator 23 and a toluene collecting tank 24; the middle outlet of the stripping tower 21 is sequentially communicated with a third condenser 25, a third gas-liquid separator 26 and a xylene collecting tank 27; the bottom outlet of the stripping tower 21 is communicated with the inlet of a water absorption tower 28, the outlet of the water absorption tower 28 is connected with the inlet of a filter 29, the outlet of the filter 29 is communicated with the inlet of a filter centrifuge 30, and the outlet of the filter centrifuge 30 is connected with a catalyst inlet pipe 5 of the fractionating tower 2.
The fractionating tower 2 is of a hollow structure, and four supporting legs 202 are connected to the side wall of the fractionating tower 2 through bolts; the top of the fractionating tower 2 is connected with a sealing cover 201 through bolts, and an air inlet pipe 6 penetrates through the middle part of the sealing cover 201; the side wall of the fractionating tower 2 is communicated with a crude benzene inlet pipe 3, a steam inlet pipe 4 is arranged below the crude benzene inlet pipe 3, and the steam inlet pipe 4 is communicated with the inner wall of the fractionating tower 2; the air inlet pipe 6 extends into the fractionating tower 2 and is communicated with an air distribution pipe 208, the air distribution pipe 208 is of a conical structure, the air distribution pipe 208 comprises an air inlet end 212 and an air outlet end 213, the diameter of the air outlet end 213 is larger than that of the air inlet end 212, and the air outlet end 213 is vertically arranged downwards; the gas distributing pipe 208 comprises an outer shell 209, an inner shell 210 is welded in the outer shell 209, and a space between the outer shell 209 and the inner shell 210 is hollow and communicated with the gas inlet pipe 6; the inner shell 210 is provided with a plurality of uniformly distributed air distribution holes 211, and the air distribution holes 211 are communicated with the air distribution pipe 208; two baffles 204 which are linearly arranged along the axial direction of the fractionating tower 2 are arranged below the gas distribution pipe 208, the baffles 204 are of cylindrical structures, two ends of each baffle 204 are respectively provided with a feeding end 206 and a discharging end 207, the diameter of each feeding end 206 is larger than that of each discharging end 207, and each feeding end 206 is vertically upwards arranged; the sidewall of the baffle 204 is provided with uniformly distributed through holes 205 and corresponds to the gas-distributing holes 211.
A radiating pipe 203 is wound below the fractionating tower 2, and one end of the radiating pipe 203 is communicated with a radiator 214 through a pipeline; specifically, the heat sink 214 is bolted to the support leg 202; the radiator 214 comprises a shell 215, a copper pipe 219 is arranged in the shell 215 through a clamp, the radiating pipe 203 is communicated with one end of the copper pipe 219, and the copper pipe 219 is wound in the shell 215; the side wall of the shell 215 is connected with two fixed frames 216 through bolts, a motor 218 is connected in each fixed frame 216 through bolts, and the output end of the motor 218 is connected with a fan blade 217 through a bolt; the other end of the copper pipe 219 is connected to an inlet end of the circulation pump 220, and an outlet end of the circulation pump 220 is connected to the other end of the radiating pipe 203.
A crude benzene hydrofining method comprises the following steps:
Step one: the heater 1 heats crude benzene through a heating resistor at 30-45 ℃, the heated crude benzene enters the fractionating tower 2 through the crude benzene inlet pipe 3, meanwhile, steam is introduced into the steam inlet pipe 4, hydrogen is introduced into the air inlet pipe 6 to fractionate the crude benzene, and the gas distribution pipe 208 spreads the hydrogen, so that the reaction uniformity is improved, and uneven reaction caused by excessive concentration of the hydrogen is prevented; the hydrogen introduced into the air inlet pipe 6 penetrates through the through hole 205 at the top of the baffle 204, so that the gasified mixture of toluene and xylene is conveniently condensed and drops downwards, turbulence when the hydrogen is mixed with steam is avoided, and the fractionation effect is improved; the hydrogen gas gathers downward from the inner case 210, ensuring the concentration of the hydrogen gas; meanwhile, the circulating pump 220 cools the fractionating tower 2 through the radiator 214 and the radiating pipe 203, controls the temperature in the fractionating tower 2, and ensures the fractionating effect;
Step two: the benzene fraction obtained after fractionation is fed into an extraction rectifying tower 11 for extraction rectification, meanwhile, the upper part of the extraction rectifying tower 11 is fed with an extractant from an extractant recovery tower 16, the extractant comprises 30% of ethyl acetate by mass and 70% of dibutyl phosphate by mass, and the ethyl acetate can selectively dissolve components in crude benzene hydrogenation products, so that the components are separated from the mixture. This contributes to an improvement in the purity and yield of the target product; dibutyl phosphate is capable of selectively interacting with components in crude benzene hydrogenation products to effect efficient separation of these components from the mixture. This selective extraction capability helps to improve the purity and recovery of the target product.
Step three: and the non-aromatic hydrocarbon solvent oil is distilled out from the top of the extraction rectifying tower 11, the non-aromatic hydrocarbon solvent oil is communicated with a stripping tower 10, and the stripping tower 10 separates the non-aromatic hydrocarbon solvent oil to obtain non-aromatic hydrocarbon and is collected in a second collecting tank 9. The mixture of the extracting agent and the benzene is extracted from the bottom of the extractive distillation tower 11, the mixture enters an extracting agent recovery tower 16, pure benzene is obtained from the top of the extracting agent recovery tower 16, the pure benzene is condensed through a first condenser 18 in sequence, then gas and liquid are separated through a first gas-liquid separator 19, bubbles and uncondensed gas in the pure benzene are removed, and the pure benzene enters a first collecting tank 20. The extractant is obtained from the tower bottom of the extractant recovery tower 16, and the extractant is subjected to heat recovery through the heat exchanger 17 and then is introduced into the extractive distillation tower 11.
Step four: the mixture of toluene and xylene is obtained at the tower bottom of the fractionating tower 2, the mixture of toluene and xylene is introduced into a stripping tower 21, the stripping tower 21 separates the toluene from the xylene, the toluene is condensed by a second condenser 22, then gas and liquid are separated by a second gas-liquid separator 23, bubbles and uncondensed gas in the toluene are removed, and the toluene enters a first collecting tank 20; the xylene is condensed by a third condenser 25, then the gas and the liquid are separated by a third gas-liquid separator 26, the bubbles and the uncondensed gas in the xylene are removed, and the xylene enters a xylene collecting tank 27;
Step five: the catalyst is obtained at the bottom of the stripping tower 21, is introduced into a water absorption tower 28 for cooling, meanwhile, the damage of the catalyst is reduced, the service life of the catalyst is prolonged, the catalyst is introduced into a filter 29 for filtering, the solvent is removed, then the catalyst is introduced into a filter centrifuge 30 for realizing the separation of the catalyst, the separated catalyst is introduced into a fractionating tower 2, the catalyst participates in chemical reaction in the introduction process, and the catalyst comprises molybdenum trioxide, benzoic acid and zirconia. The molybdenum trioxide catalyst can effectively promote the removal of impurities in crude benzene, thereby improving the purity and quality of the product; benzoic acid is used as an organic catalyst, so that the activation energy of hydrogenation reaction is reduced, the reaction rate and the production efficiency are improved, and the product purity is improved; zirconia has excellent thermal and chemical stability, which enables it to maintain good catalytic activity under hydrogenation conditions of high temperature and high pressure. In addition, the surface of the zirconia has moderate acid and alkali, which is favorable for adsorbing and activating reactant molecules and promoting the hydrogenation reaction.
Example 1:
Crude benzene is introduced into a heater 1, the temperature of the heater 1 is 30 ℃, the heated crude benzene is communicated with an inlet of a fractionating tower 2, a gas phase outlet pipe 7 at the top of the fractionating tower 2 is communicated with an inlet of an extraction rectifying tower 11, an extractant inlet 14 is arranged at the top of the extraction rectifying tower 11, an outlet 13 at the top of the extraction rectifying tower is connected with an inlet of a stripping tower 10, an outlet of the stripping tower 10 is communicated with a second collecting tank 9, a rectifying outlet 15 of the extraction rectifying tower 11 is communicated with an inlet of an extractant recovery tower 16, and the extractant comprises 30% of ethyl acetate by mass and 70% of dibutyl phosphate by mass. The top of the extractant recovery tower 16 is connected with a first condenser 18, a first gas-liquid separator 19 and a first collection tank 20 in sequence. The bottom outlet of the extractant recovery tower 16 is communicated with the top extractant inlet 14 of the extractive distillation tower 11.
The outlet pipe 8 of the fractionating tower 2 is communicated with the inlet of the stripping tower 21; the upper outlet of the stripping tower 21 is sequentially connected with a second condenser 22, a second gas-liquid separator 23 and a toluene collecting tank 24; the middle outlet of the stripping tower 21 is sequentially connected with a third condenser 25, a third gas-liquid separator 26 and a xylene collecting tank 27; the outlet of the bottom of the stripping tower 21 is communicated with the inlet of a water absorption tower 28, the outlet of the water absorption tower 28 is connected with the inlet of a filter 29, the outlet of the filter 29 is communicated with the inlet of a filter centrifuge 30, and the outlet of the filter centrifuge 30 is connected with a catalyst inlet pipe 5 of the fractionating tower 2. The catalyst comprises 20% of molybdenum trioxide, 40% of benzoic acid and 40% of zirconia by mass fraction. The reaction conditions of each tower kettle are shown in table 1.
TABLE 1 reaction conditions for each column bottom
The refining effect is shown in Table 2.
TABLE 2 purity of the products
Example 2:
Crude benzene is introduced into a heater 1, the temperature of the heater 1 is 30 ℃, the heated crude benzene is communicated with an inlet of a fractionating tower 2, a gas phase outlet pipe 7 at the top of the fractionating tower 2 is communicated with an inlet of an extraction rectifying tower 11, an extractant inlet 14 is arranged at the top of the extraction rectifying tower 11, an outlet 13 at the top of the tower is connected with an inlet of a stripping tower 10, an outlet of the stripping tower 10 is communicated with a second collecting tank 9, a rectifying outlet 15 of the extraction rectifying tower 11 is communicated with an inlet of an extractant recovery tower 16, and the extractant comprises 40% of ethyl acetate by mass and 60% of dibutyl phosphate by mass. The top of the extractant recovery tower 16 is connected with a first condenser 18, a first gas-liquid separator 19 and a first collection tank 20 in sequence. The bottom outlet of the extractant recovery tower 16 is communicated with the top extractant inlet 14 of the extractive distillation tower 11.
The outlet pipe 8 of the fractionating tower 2is communicated with the inlet of the stripping tower 21; the upper outlet of the stripping tower 21 is sequentially connected with a second condenser 22, a second gas-liquid separator 23 and a toluene collecting tank 24; the middle outlet of the stripping tower 21 is sequentially connected with a third condenser 25, a third gas-liquid separator 26 and a xylene collecting tank 27; the outlet of the bottom of the stripping tower 21 is communicated with the inlet of a water absorption tower 28, the outlet of the water absorption tower 28 is connected with the inlet of a filter 29, the outlet of the filter 29 is communicated with the inlet of a filter centrifuge 30, and the outlet of the filter centrifuge 30 is connected with a catalyst inlet pipe 5 of the fractionating tower 2. The catalyst comprises 30% of molybdenum trioxide, 40% of benzoic acid and 30% of zirconia by mass fraction. The reaction conditions of each tower kettle are shown in Table 3.
TABLE 3 reaction conditions for each column
The refining effect is shown in Table 4.
TABLE 4 purity of the products
Example 3:
Crude benzene is introduced into a heater 1, the temperature of the heater 1 is 30 ℃, the heated crude benzene is communicated with an inlet of a fractionating tower 2, a gas phase outlet pipe 7 at the top of the fractionating tower 2 is communicated with an inlet of an extraction rectifying tower 11, an extractant inlet 14 is arranged at the top of the extraction rectifying tower 11, an outlet 13 at the top of the extraction rectifying tower is connected with an inlet of a stripping tower 10, an outlet of the stripping tower 10 is communicated with a second collecting tank 9, a rectifying outlet 15 of the extraction rectifying tower 11 is communicated with an inlet of an extractant recovery tower 16, and the extractant comprises 70% of ethyl acetate by mass and 30% of dibutyl phosphate by mass. The top of the extractant recovery tower 16 is connected with a first condenser 18, a first gas-liquid separator 19 and a first collection tank 20 in sequence. The bottom outlet of the extractant recovery tower 16 is communicated with the top extractant inlet 14 of the extractive distillation tower 11.
The outlet pipe 8 of the fractionating tower 2 is communicated with the inlet of the stripping tower 21; the upper outlet of the stripping tower 21 is sequentially connected with a second condenser 22, a second gas-liquid separator 23 and a toluene collecting tank 24; the middle outlet of the stripping tower 21 is sequentially connected with a third condenser 25, a third gas-liquid separator 26 and a xylene collecting tank 27; the outlet of the bottom of the stripping tower 21 is communicated with the inlet of a water absorption tower 28, the outlet of the water absorption tower 28 is connected with the inlet of a filter 29, the outlet of the filter 29 is communicated with the inlet of a filter centrifuge 30, and the outlet of the filter centrifuge 30 is connected with a catalyst inlet pipe 5 of the fractionating tower 2. The catalyst comprises 50% molybdenum trioxide, 30% benzoic acid and 20% zirconia. The reaction conditions of each tower kettle are shown in Table 5.
TABLE 5 reaction conditions for each column
The refining effect is shown in Table 6.
TABLE 6 purity of the products
In conclusion, the molybdenum trioxide catalyst effectively promotes the removal of impurities in crude benzene, so that the purity and quality of the product are improved; benzoic acid reduces the activation energy of hydrogenation reaction, thereby improving the reaction rate and the product purity; the surface of the zirconia has moderate acid and alkali, which is favorable for adsorbing and activating reactant molecules and promoting the hydrogenation reaction; the gas-distributing pipe 208 of the fractionating tower 2 distributes the hydrogen gas to prevent the hydrogen gas from over-reacting; baffle 204 cooperates with gas distribution tube 208 to enhance reaction uniformity; the fractionating tower 21 separates the toluene and the xylene, and the obtained catalyst is returned to the fractionating tower 2 after being treated, so that the use is convenient.
Of course, the present invention is capable of other various embodiments and its several details are capable of modification and variation in light of the present invention by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (2)
1. A hydrofining method of crude benzene is characterized in that: the method comprises the following steps:
Step one: heating crude benzene by a heater (1) at 30-50 ℃, feeding the heated crude benzene into a fractionating tower (2) through a crude benzene feeding pipe (3), and simultaneously introducing steam and hydrogen into the fractionating tower (2) to fractionate the crude benzene;
Step two: introducing the benzene fraction obtained after fractionation into an extraction rectifying tower (11) for extraction rectification, and introducing an extractant into an extractant recovery tower (16) from the extraction rectifying tower (11);
step three: the mixture extracted from the bottom of the extraction rectifying tower (11) enters an extractant recovery tower (16), pure benzene is obtained from the top of the extractant recovery tower (16), and the pure benzene sequentially enters a first collecting tank (20) through a first condenser (18) and a first gas-liquid separator (19);
Step four: the method comprises the steps that a mixture of toluene and xylene is obtained from a tower kettle of a fractionating tower (2), the mixture is introduced into a stripping tower (21), toluene is obtained from the top of the stripping tower (21), the toluene sequentially passes through a second condenser (22) and a second gas-liquid separator (23) to reach a toluene collecting tank (24), xylene is obtained from the middle of the stripping tower (21), and the xylene sequentially passes through a third condenser (25) and a third gas-liquid separator (26) to reach a xylene collecting tank (27);
Step five: the catalyst at the bottom of the stripping tower (21) sequentially passes through a water absorption tower (28), a filter (29) and a filter centrifuge (30) and returns to the fractionating tower (2), wherein the catalyst comprises molybdenum trioxide, benzoic acid and zirconia;
The utility model discloses a fractionating tower, including fractionating tower (2), heater (1), fractionating tower (2), steam inlet pipe (4) are installed to the export of heater (1) and the entry intercommunication of fractionating tower (2), crude benzol inlet pipe (3) are installed to fractionating tower (2) top, steam inlet pipe (4) are installed to fractionating tower (2) lower part, discharge pipe (8) are installed to fractionating tower (2) bottom, air inlet pipe (6) intercommunication has branch trachea (208), branch trachea (208) are the toper structure, branch trachea (208) include shell (209), shell (209) inner wall installs shell (210), be hollow structure and with intake pipe (6) intercommunication between shell (209) and shell (210), shell (210) are provided with a plurality of minute holes (211), a plurality of baffles (204) are installed to dividing trachea (208) below, baffle (204) are tubular structure, baffle (204) lateral wall are provided with a plurality of evenly distributed's through-holes (205), baffle (204) both ends are feed end (206) and discharge end (207) respectively, diameter of rectifying tower (206) are connected with the diameter of rectifying tower (7) inlet (7), the top of the extraction rectifying tower (11) is provided with an extractant inlet (14), an outlet (13) of the top of the extraction rectifying tower (11) is connected with an inlet of a stripping tower (10), an outlet of the stripping tower (10) is communicated with a second collecting tank (9), a rectifying outlet (15) of the extraction rectifying tower (11) is communicated with an inlet of an extractant recovery tower (16), the outlet (13) of the top of the extractant recovery tower (16) is sequentially connected with a first condenser (18), a first gas-liquid separator (19) and a first collecting tank (20), the bottom of the extractant recovery tower (16) is connected with an extractant inlet (14) of the extraction rectifying tower (11), a discharge pipe (8) of the fractionating tower (2) is communicated with an inlet of the stripping tower (21), an upper outlet of the stripping tower (21) is sequentially connected with a second condenser (22), a second gas-liquid separator (23) and a toluene collecting tank (24), a middle outlet of the stripping tower (21) is sequentially connected with a third condenser (25), a third gas-liquid separator (25) and an inlet of the third gas-liquid separator (28) are sequentially connected with an inlet of the absorption tower (28) and water inlet of the third gas-liquid separator (28), the outlet of the filter (29) is communicated with the inlet of the filter centrifuge (30), and the outlet of the filter centrifuge (30) is connected with the catalyst inlet of the fractionating tower (2).
2. The crude benzene hydrorefining method according to claim 1, wherein a radiating pipe (203) is installed on the outer wall of the fractionating tower (2), and the radiating pipe (203) is sequentially communicated with a radiator (214) and a circulating pump (220).
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| DE10019196C1 (en) * | 2000-04-17 | 2001-09-27 | Krupp Uhde Gmbh | Recovery of pure benzene, toluene or toluene and xylene from aromatic fraction containing non-aromatics uses on column with main zone of 2 parallel chambers for extractive distillation and extractant recovery |
| CN100378046C (en) * | 2006-07-06 | 2008-04-02 | 湖南长岭石化科技开发有限公司 | Method for producing benzene aromatic hydrocarbon from crude benzole |
| CN104725178A (en) * | 2015-02-04 | 2015-06-24 | 沾化瑜凯新材料科技有限公司 | Rectification process for preparing benzene, methylbenzene and dimethylbenzene from crude benzene |
| CN106916044A (en) * | 2015-12-24 | 2017-07-04 | 上海宝钢化工有限公司 | A kind of method for refining carbonization crude benzole |
| CN116640603A (en) * | 2022-09-08 | 2023-08-25 | 临涣焦化股份有限公司 | A kind of method of crude benzene refining by-product high boiling point solvent oil |
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| 粗苯加氢三苯馏分工艺的优化研究;冯晴洁;《江西化工》;20230430;第39卷(第2期);第92-94页 * |
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