CN108456139B - Device and method for preparing dibutyl phthalate by batch catalytic reaction rectification - Google Patents
Device and method for preparing dibutyl phthalate by batch catalytic reaction rectification Download PDFInfo
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- CN108456139B CN108456139B CN201810310004.8A CN201810310004A CN108456139B CN 108456139 B CN108456139 B CN 108456139B CN 201810310004 A CN201810310004 A CN 201810310004A CN 108456139 B CN108456139 B CN 108456139B
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 73
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000007791 liquid phase Substances 0.000 claims abstract description 53
- 239000012071 phase Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 14
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005886 esterification reaction Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 9
- 238000007086 side reaction Methods 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract description 2
- 239000007792 gaseous phase Substances 0.000 abstract 2
- 238000004821 distillation Methods 0.000 abstract 1
- 238000000066 reactive distillation Methods 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000012856 packing Methods 0.000 description 4
- 239000004014 plasticizer Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005191 phase separation Methods 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- REOJLIXKJWXUGB-UHFFFAOYSA-N mofebutazone Chemical group O=C1C(CCCC)C(=O)NN1C1=CC=CC=C1 REOJLIXKJWXUGB-UHFFFAOYSA-N 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention relates to a device and a method for preparing dibutyl phthalate by batch catalytic reaction rectification. The device comprises a reaction rectifying tower, a tower kettle, a circulating pump, a tower top condenser and a tower top split-phase tank; the method is characterized in that gaseous phase obtained by gasifying phthalic anhydride and butanol in a tower kettle enters the reaction rectifying tower through a gaseous phase inlet at the lower part of the reaction rectifying tower, liquid phase in the tower kettle enters a liquid phase inlet at the upper part of the reaction rectifying tower through a circulating pump, and phthalic anhydride and butanol mixture undergoes esterification reaction in a catalyst bed layer of a distributor; the generated water and butanol form an azeotrope, the azeotrope is cooled by a condenser at the top of the tower and then enters a phase-splitting tank for phase splitting, the butanol after phase splitting flows back into a reaction rectifying tower for continuous reaction, and water phase is extracted from the bottom of the phase-splitting tank; the bottom product of the reactive distillation column enters another column kettle, and catalyst beds are respectively arranged in the column kettle and the distillation column, so that the time of the esterification reaction is increased. The method solves the problems of serious corrosion, more side reactions and more wastewater in the prior art, and has the advantages of simple and controllable process, lower organic matter content in wastewater and the like.
Description
Technical Field
The invention belongs to the technical field of catalytic reaction rectification, and particularly relates to a device and a method for preparing dibutyl phthalate by intermittent catalytic reaction rectification.
Background
Dibutyl phthalate (DBP) is a good plasticizer, is the most widely used plasticizer at present, accounts for about 75% of the total plasticizer yield, has strong dissolving capacity for various resins, is mainly used for processing polyvinyl chloride, and ensures that the product has good softness; the cellulose nitrate coating has good softening effect and excellent stability, flexing resistance, adhesiveness and waterproofness; can also be used as plasticizers for vinyl acetate, alkyd resins, ethylcellulose, and neoprene.
At present, the domestic common synthesis method is formed by esterifying phthalic anhydride and n-butanol under the action of sulfuric acid, and has the defects of low price of sulfuric acid, mature process, higher product yield, easiness in side reaction, serious corrosion, three-waste pollution, difficulty in controlling product quality and the like. The main working procedures of DBP production include esterification, neutralization and water washing, dealcoholization, filtration, wastewater treatment, recovery of alcohol treatment and the like. The wastewater generated in the generation process comes from chemical reaction to generate water, the raw materials are brought into water, and the water is neutralized and washed. The waste water has complex components, and contains DBP, phthalic acid, sodium sulfate and free H 2 SO 4 O-benzeneShan Xincu, monobutyl vinegar, etc., and the impurities in the wastewater are mainly organic matters.
Along with the improvement of the environmental protection requirement in China, the clean generation requirement on dibutyl phthalate is more and more urgent, and aiming at the problems existing in the traditional intermittent production process, a high-efficiency environmental-protection DBP production technology is developed, so that the product yield and conversion rate are improved, the wastewater yield is reduced, and the method has extremely important significance for society and enterprises.
Disclosure of Invention
Aiming at the problems of more side reactions and more sewage output, the invention develops an environment-friendly device and a method for preparing dibutyl phthalate by batch catalytic reaction rectification with high product yield and conversion rate, and improves the traditional esterification reaction process.
The technical scheme adopted for solving the technical problems is as follows:
a device for preparing dibutyl phthalate by batch catalytic reaction rectification comprises a reaction rectifying tower (C1), a first tower kettle (T1), a second tower kettle (T2), a circulating pump (P1), a condenser (E1) and a phase separation tank (D); the middle upper part, the middle part and the lower part of the reaction rectifying tower (C1) are respectively provided with a gas-liquid distributor, catalyst sulfonic acid resin is filled in the gas-liquid distributor, and the middle parts and the lower parts of the first tower kettle (T1) and the second tower kettle (T2) are respectively provided with a bed layer filled with the catalyst resin;
in the reaction rectifying tower (C1), a gas phase outlet is arranged at the top of the tower, and a butanol reflux port, a tower kettle liquid phase inlet, two tower lower gas phase inlets and a tower bottom extraction outlet are respectively arranged on the tower body of the reaction rectifying tower (C1) from top to bottom;
the top of the phase separation tank (D) is provided with a liquid phase inlet, the upper part is provided with a butanol reflux outlet, and the bottom is provided with a water phase extraction outlet;
the tops of the first tower kettle (T1) and the second tower kettle (T2) are provided with gas phase outlets, the upper part is provided with a liquid phase inlet, and the bottom is provided with a liquid phase outlet;
the gas phase outlet at the top of the reaction rectifying tower (C1) is connected with the condenser (E1), the outlet of the condenser (E1) is connected with the liquid phase inlet of the phase splitting tank (D), the outlet at the upper part of the phase splitting tank (D) is connected with the butanol reflux port at the upper part of the reaction rectifying tower (C1), the gas phase inlet at the lower part of the reaction rectifying tower (C1) is respectively connected with the gas phase outlets of the first tower kettle (T1) and the second tower kettle (T2), the liquid phase outlet at the bottom of the reaction rectifying tower (C1) is respectively connected with the liquid phase inlets at the upper parts of the first tower kettle (T1) and the second tower kettle (T2), the liquid phase outlet at the bottom of the first tower kettle (T1) and the liquid phase outlet at the bottom of the second tower kettle (T2) are connected with the inlet of the reflux pump (P1), and the outlet of the reflux pump (P1) is connected with the liquid phase inlet at the upper tower kettle of the reaction rectifying tower (C1).
A method for preparing dibutyl phthalate by batch catalytic reaction rectification comprises the following steps:
the liquid phase outlet at the bottom of the reaction rectifying tower (C1) is disconnected from the liquid phase inlet at the upper part of the first tower kettle (T1), the liquid phase outlet at the bottom of the second tower kettle (T2) is disconnected from the inlet of the reflux pump (P1), and the liquid phase outlet at the bottom of the reaction rectifying tower (C1) and the liquid phase inlet at the upper part of the second tower kettle (T2) are communicated, and the liquid phase outlet at the bottom of the first tower kettle (T1) and the inlet of the reflux pump (P1) are communicated;
phthalic anhydride and butanol in the first tower kettle (T1) are heated to 140 ℃, phthalic anhydride: the mass ratio of butanol is 1:1.4, and esterification reaction is carried out in a catalyst bed layer; the gasified gas phase of the first tower kettle (T1) enters the normal pressure reaction rectifying tower (C1) through a gas phase inlet at the lower part of the reaction rectifying tower, the liquid phase in the first tower kettle (T1) enters a liquid phase inlet at the upper part of the reaction rectifying tower (C1) through a circulating pump (P1), and phthalic anhydride and butanol mixture is subjected to esterification reaction in a catalyst bed layer of a distributor; the generated water and butanol form an azeotrope, the azeotrope is cooled by a tower top condenser (E1) and then enters a phase-splitting tank (D) for phase splitting, the butanol after phase splitting flows back into a reaction rectifying tower (C1) for continuous reaction, and a water phase is extracted from the bottom of the phase-splitting tank (D);
the bottom product of the reaction rectifying tower (C1) enters a liquid phase inlet of a second tower kettle (T2), the temperature of the second tower kettle (T2) is controlled at 140 ℃, so that the mixture continuously reacts in a catalyst bed layer of the second tower kettle (T2), the whole process is carried out until all feed liquid in the first tower kettle (T1) enters the reaction rectifying tower, a liquid phase outlet at the bottom of the reaction rectifying tower (C1) is communicated with a liquid phase inlet at the upper part of the first tower kettle (T1), a liquid phase outlet at the bottom of the second tower kettle (T2) is communicated with a reflux pump (P1) inlet, a liquid phase outlet at the bottom of the reaction rectifying tower (C1) is disconnected from a liquid phase inlet at the upper part of the second tower kettle (T2), the liquid phase outlet at the bottom of the first tower kettle (T1) is disconnected from the reflux pump (P1) inlet, the feed liquid in the second tower kettle (T2) is used as a reaction raw material, and the reaction process is carried out until the reaction is completed.
The invention has the following advantages and positive effects:
the invention uses sulfonic acid resin to replace sulfuric acid as catalyst, the reaction rectifying tower to replace stirring reaction kettle, reduces side reaction in the reaction process, integrates the reaction and dehydration process, avoids the neutralization and water washing process, and reduces the wastewater amount.
The method solves the problems of serious corrosion, more side reactions and more wastewater in the prior art, and has the advantages of simple and controllable process, lower organic matter content in wastewater and the like.
Drawings
FIG. 1 is a process flow for preparing dibutyl phthalate by batch catalytic reaction rectification according to the invention.
The device comprises a C1-reaction rectifying tower, an E1-condenser, a T1-tower kettle, a T2-tower kettle, a D-phase separation tank, a P1-circulating pump, a Z1-valve, a Z2-valve, a Z3-valve and a Z4-valve;
description of liquid in the pipe: 1-condensate, 2-refluxing butanol, 3-extracted water phase, 4-tower kettle liquid phase, 5-tower kettle gas phase, 6-tower kettle gas phase, 7-reaction rectifying tower bottom liquid phase, 8-reaction rectifying tower bottom liquid phase, 9-tower kettle liquid phase and 10-tower kettle liquid phase.
Detailed Description
The following detailed description of the present invention is provided merely to illustrate the present invention, but the scope of the present invention is not limited to the embodiments.
Example 1
The valves Z1 and Z4 are closed, the valves Z2 and Z3 are opened, the mass ratio of phthalic anhydride to butanol in the first tower kettle T1 is 1:1.4, the phthalic anhydride and butanol are heated to 140 ℃ in the tower kettle, and esterification reaction is carried out in the catalyst bed; the gas phase gasified by the first tower kettle T1 enters the reaction rectifying tower C1 through a gas phase inlet at the lower part of the reaction rectifying tower, the liquid phase in the first tower kettle T1 enters a liquid phase inlet at the upper part of the reaction rectifying tower C1 through a circulating pump P1, the rectifying tower packing of the reaction rectifying tower is silk screen corrugated structured packing, the operation is carried out at normal pressure, the theoretical plate number is 12, and the mixture of phthalic anhydride and butanol is subjected to esterification reaction in a catalyst bed layer of a distributor; the generated water and butanol form an azeotrope (characterized by the water content of 16 percent and the butanol content of 83 percent), the azeotrope is cooled by a tower top condenser E1 and then enters a phase-splitting tank D for phase splitting, the butanol after phase splitting flows back into a reactive rectifying tower C1 for continuous reaction, and a water phase is extracted from the bottom of the phase-splitting tank D; the bottom product of the reaction rectifying tower C1 enters a liquid phase inlet of a second tower kettle T2, the temperature of the second tower kettle T2 is controlled at 140 ℃, so that the mixture continues to react in a catalyst bed layer of the second tower kettle T2, and the whole process is carried out until the feed liquid in the first tower kettle T1 completely enters the reaction rectifying tower. And then closing valves Z2 and Z3, opening valves Z1 and Z4, taking the feed liquid in the second tower kettle T2 as a reaction raw material, and performing the above reaction process, and performing cyclic operation, wherein the equipment continuously operates for 2 hours until the reaction is complete, wherein the purity of the finally obtained product is 99.7%.
Example 2
Valves Z1 and Z4 are closed, valves Z2 and Z3 are opened, phthalic anhydride and butanol in the first tower kettle T1 are heated to 150 ℃ in the tower kettle according to the mass ratio of 1:1.4, and esterification reaction is carried out in a catalyst bed; the gas phase gasified by the first tower kettle T1 enters the reaction rectifying tower C1 through a gas phase inlet at the lower part of the reaction rectifying tower, the liquid phase in the first tower kettle T1 enters a liquid phase inlet at the upper part of the reaction rectifying tower C1 through a circulating pump P1, the rectifying tower packing of the reaction rectifying tower is silk screen corrugated structured packing, the operation is carried out at normal pressure, the theoretical plate number is 12, and the mixture of phthalic anhydride and butanol is subjected to esterification reaction in a catalyst bed layer of a distributor; the generated water and butanol form an azeotrope (characterized by the water content of 16 percent and the butanol content of 83 percent), the azeotrope is cooled by a tower top condenser E1 and then enters a phase-splitting tank D for phase splitting, the butanol after phase splitting flows back into a reactive rectifying tower C1 for continuous reaction, and a water phase is extracted from the bottom of the phase-splitting tank D; the bottom product of the reaction rectifying tower C1 enters a liquid phase inlet of a second tower kettle T2, the temperature of the second tower kettle T2 is controlled at 150 ℃, so that the mixture continues to react in a catalyst bed layer of the second tower kettle T2, and the whole process is carried out until the feed liquid in the first tower kettle T1 completely enters the reaction rectifying tower. And then closing valves Z2 and Z3, opening valves Z1 and Z4, taking the feed liquid in the second tower kettle T2 as a reaction raw material, and performing the above reaction process, and performing cyclic operation, wherein the equipment continuously operates for 2 hours until the reaction is complete, wherein the purity of the finally obtained product is 99.8%.
Claims (1)
1. A method for preparing dibutyl phthalate by batch catalytic reaction rectification is characterized by comprising the following steps: the method comprises the following steps: the liquid phase outlet at the bottom of the reaction rectifying tower (C1) is disconnected from the liquid phase inlet at the upper part of the first tower kettle (T1), the liquid phase outlet at the bottom of the second tower kettle (T2) is disconnected from the inlet of the reflux pump (P1), and the liquid phase outlet at the bottom of the reaction rectifying tower (C1) and the liquid phase inlet at the upper part of the second tower kettle (T2) are communicated, and the liquid phase outlet at the bottom of the first tower kettle (T1) and the inlet of the reflux pump (P1) are communicated; heating phthalic anhydride and butanol in the first tower kettle (T1) to 140 ℃, and carrying out esterification reaction in a catalyst bed layer, wherein the mass ratio of phthalic anhydride to butanol is 1:1.4; the gasified gas phase of the first tower kettle (T1) enters the normal pressure reaction rectifying tower (C1) through a gas phase inlet at the lower part of the reaction rectifying tower, the liquid phase in the first tower kettle (T1) enters a liquid phase inlet at the upper part of the reaction rectifying tower (C1) through a reflux pump (P1), and phthalic anhydride and butanol mixture is subjected to esterification reaction in a catalyst bed layer of a distributor; the generated water and butanol form an azeotrope, the azeotrope is cooled by a tower top condenser (E1) and then enters a phase-splitting tank (D) for phase splitting, the butanol after phase splitting flows back into a reaction rectifying tower (C1) for continuous reaction, and a water phase is extracted from the bottom of the phase-splitting tank (D); the bottom product of the reaction rectifying tower (C1) enters a liquid phase inlet of a second tower kettle (T2), the temperature of the second tower kettle (T2) is controlled at 140 ℃, so that the mixture continuously reacts in a catalyst bed layer of the second tower kettle (T2), the whole process is carried out until all feed liquid in the first tower kettle (T1) enters the reaction rectifying tower, a liquid phase outlet at the bottom of the reaction rectifying tower (C1) is communicated with a liquid phase inlet at the upper part of the first tower kettle (T1), a liquid phase outlet at the bottom of the second tower kettle (T2) is communicated with a reflux pump (P1) inlet, a liquid phase outlet at the bottom of the reaction rectifying tower (C1) is disconnected from a liquid phase inlet at the upper part of the second tower kettle (T2), the liquid phase outlet at the bottom of the first tower kettle (T1) is disconnected from the reflux pump (P1) inlet, the feed liquid in the second tower kettle (T2) is used as a reaction raw material, and the reaction process is carried out until the reaction is completed.
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| CN106810450A (en) * | 2017-02-23 | 2017-06-09 | 天津大学 | The apparatus and method that a kind of catalytic reaction rectification prepares dibutyl phthalate |
| CN208166890U (en) * | 2018-04-09 | 2018-11-30 | 石家庄白龙化工股份有限公司 | Interval catalytic reaction rectification prepares the device of dibutyl phthalate |
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| CN106810450A (en) * | 2017-02-23 | 2017-06-09 | 天津大学 | The apparatus and method that a kind of catalytic reaction rectification prepares dibutyl phthalate |
| CN208166890U (en) * | 2018-04-09 | 2018-11-30 | 石家庄白龙化工股份有限公司 | Interval catalytic reaction rectification prepares the device of dibutyl phthalate |
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