CN204342701U - Butyraldehyde hydrogenation produces the reaction and rectification device of butanols - Google Patents

Butyraldehyde hydrogenation produces the reaction and rectification device of butanols Download PDF

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CN204342701U
CN204342701U CN201420738995.7U CN201420738995U CN204342701U CN 204342701 U CN204342701 U CN 204342701U CN 201420738995 U CN201420738995 U CN 201420738995U CN 204342701 U CN204342701 U CN 204342701U
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butanols
reactive distillation
tower
positive
distillation column
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李洪
高鑫
丛山
贾雪婷
李鑫钢
徐明仲
武金峰
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Tianjin University
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Tianjin University
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

The utility model relates to the reaction and rectification device that butyraldehyde produces butanols.Comprise vaporizer, reactive distillation column, butanols rectifying tower, positive isobutanol separation column, condenser, reboiler, compressor, pump and relevant feedstocks pipeline and the pipeline being connected above equipment; The feature of method of the present utility model and device is the employing of reaction rectification technique and equipment, light constituent can be isolated by tower top while reactive distillation column carries out butyraldehyde hydrogenation reaction, just can obtained by later separation, isopropylcarbinol, butyraldehyde is produced butanols and purification rectifying separation two unit operations, be coupled in an equipment and carry out simultaneously, react and reaction product has been purified simultaneously, both saved facility investment, additionally reduced follow-up process cost.The propyl carbinol quality purity obtained after being separated with positive isobutanol separation column by follow-up butanols rectifying tower can reach 99.5%, and the quality purity of isopropylcarbinol can reach 99%.

Description

Butyraldehyde hydrogenation produces the reaction and rectification device of butanols
Technical field
The utility model relates to production of butanol technical field, particularly relates to the reaction and rectification device that a kind of butyraldehyde hydrogenation produces butanols.
Background technology
Butanols is important basic organic chemical industry raw material, main application is the raw material as resin, paint, sizing agent and softening agent, also can be used as the extraction agent of grease, spices and medicine and the additive of phthalic resin coating, can be used as the raw material of ore dressing defoamer, washing composition, dewatering agent and synthetic perfume in addition.
The mode of production of butanols can be divided into fermentation method, Acetaldehyde and oxo synthesis.Due to fermentation method and Acetaldehyde technical process long, equipment corrosion is serious, and extremely uneconomical, existing apparatus is substantially superseded.The main method of current production of butanol take propylene as feedstock carbonyl synthesis method synthesis butyraldehyde, then produce butanols by butyraldehyde hydrogenation.CN1221723A discloses a kind of method that aldehyde gas phase hydrogenation prepares alcohol, treats in the aldehyde of hydrogenation by being joined by nitrogenous alkali, thus suppresses the generation of by product, obtains the alcohol of highly selective and high yield.CN1278237A discloses a kind of method of producing propyl carbinol, under the moisture being less than or equal to about 6 % by weight exists, butyraldehyde-n obtains propyl carbinol reaction product by hydrogenation, and under there is about 0.01-6 % by weight water condition in separation column, purify to product, object is that by product di-n-butyl ether is separated with propyl carbinol with the form of the low azeotropic of ternary.CN102408304A discloses a kind of method that aldehyde selec-tive hydrogenation prepares alcohol, the hydrogenation catalyst containing carrier, metal active constituent and silane group is used in patent, on this catalyzer, the amount of by product can significantly reduce, and has catalyzer long service life, the advantage that carbon distribution is few.
Butyraldehyde hydrogenation reaction is except generating propyl carbinol and isopropylcarbinol, and also a small amount of by product can occur, by product has amylalcohol, octanol, ester and ether etc.At present, to the separation of hydrogenation reaction product, the main lightness-removing column and weight-removing column and positive isobutanol separation column of adopting obtains propyl carbinol product and isobutanol product.Reaction rectification technique applies day by day a kind of process intensification technology simultaneously carried out in same equipment by simultaneous reaction and separation widely in chemical industry, and in facility investment, this technology is also than reacting and being separated the flow process of separate operation more economically.Also reaction rectification technique is not applied in Patents and the report of butyraldehyde Hydrogenation butanols process at present.
Summary of the invention
The purpose of this utility model is to provide a kind of butyraldehyde hydrogenation and produces the reaction and rectification device of butanols, the catalytic reaction rectification method using the utility model to provide, the advantage such as have that technical process is simple, facility investment is lower, easy to operate and energy consumption is lower.
Butyraldehyde hydrogenation of the present utility model produces reactive distillation method and the device of butanols, and primarily of vaporizer, reactive distillation column, butanols rectifying tower and positive isobutanol separation column composition, main products is propyl carbinol and isopropylcarbinol.The feature of method of the present utility model and device is the employing of reaction rectification technique and equipment, light constituent can be isolated by tower top while reactive distillation column carries out butyraldehyde hydrogenation reaction, just can obtained by later separation, isopropylcarbinol, reduce technical process, save facility investment.
The technical solution of the utility model is as follows:
Butyraldehyde of the present utility model produces the reaction and rectification device of butanols, comprises vaporizer, reactive distillation column, butanols rectifying tower, positive isobutanol separation column, condenser, reboiler, compressor, pump and relevant feedstocks pipeline and the pipeline being connected above equipment; Reactive distillation column, butanols rectifying tower, positive isobutanol separation column tower top all arrange condenser, all arrange reboiler at the bottom of reactive distillation column, butanols rectifying tower, positive isobutanol separation column tower; Evaporator overhead gaseous phase outlet is connected to reactive distillation column; Reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, and compressor outlet is connected to reactive distillation column hydrogen feed mouth, and condensator outlet liquid phase, as light component product extraction, is that cymogene alcohol product is connected to butanols rectifying tower opening for feed at the bottom of tower; Butanols rectifying tower ejects material and enters positive isobutanol separation column for mixed butyl alcohol, is heavy constituent by product at the bottom of tower; The discharging of positive isobutanol separation column tower top is isobutanol product, and discharging at the bottom of tower is propyl carbinol product.
The reactive distillation method that butyraldehyde hydrogenation of the present utility model produces butanols is: the butyraldehyde gas (S02) of raw material butyraldehyde (S01) after evaporator (V1) vaporization enters the bottom of reactive distillation column (T1) conversion zone together with raw hydrogen (S03), reactive distillation column (T1) top gaseous phase (S04) enters reactive distillation column overhead condenser (E1), after condensation, gas phase is that the hydrogen (S06) of unreacted hydrogen (S05) after compressor (C1) pressurization returns reactive distillation column (T1) charging, after condensation, liquid phase (S07) obtains liquid phase through reactive distillation column reflux-withdrawal pump (P1), control by operating reflux ratio, a part is as phegma (S08), another part is as tower top light constituent (S09) extraction, at the bottom of tower, extraction cymogene alcohol (S10) is as the charging of butanols rectifying tower (T2), butanols rectifying tower (T2) top gaseous phase (S11) obtains liquid phase through condenser (E3) condensed liquid phase (S12) through butanols rectifier column reflux extraction pump (P2), control by operating reflux ratio, a part is as phegma (S13), another part be mixed butyl alcohol (S14) as positive isobutanol separation column (T3) charging, extraction heavy constituent by product (S15) at the bottom of tower, positive isobutanol separation column (T3) top gaseous phase (S16) obtains liquid phase through condenser (E5) condensed liquid phase (S17) through positive isobutanol separation column reflux-withdrawal pump (P3), control by operating reflux ratio, a part is as phegma (S18), another part as isobutanol product (S19) extraction, extraction propyl carbinol (S20) product at the bottom of tower.
Butyraldehyde hydrogenation is produced in the reactive distillation method of butanols: evaporator pressure is 0.01-3MPa; Reactive distillation column adopts nickel and/or copper-based catalysts, and conversion zone temperature is 100-250 DEG C, preferred 110-130 DEG C, and pressure is 0.01-2MPa, and reflux ratio is 10-100, and hydrogen aldehyde mol ratio is 10:1-30:1; Butanols rectifying tower pressure is 0.5-1MPa, and reflux ratio is 1-100; Positive isobutanol separation column pressure is 0.1-1MPa, and reflux ratio is 20-100; Pressure all represents by absolute pressure herein.
Butyraldehyde hydrogenation of the present utility model produces reactive distillation method and the device of butanols, its advantage is butyraldehyde hydrogenation reaction and butanols purification rectifying separation two unit operations, organically be coupled in an equipment and carry out simultaneously, react and reaction product has been purified simultaneously, both save facility investment, additionally reduce follow-up process cost.The propyl carbinol quality purity obtained after being separated with positive isobutanol separation column by follow-up butanols rectifying tower can reach 99.5%, and the quality purity of isopropylcarbinol can reach 99%.
Accompanying drawing explanation
Fig. 1 is the reaction and rectification device schematic diagram that butyraldehyde hydrogenation produces butanols.
Equipment: V1. vaporizer, T1. reactive distillation column, T2. butanols rectifying tower, T3. positive isobutanol separation column, P1. reactive distillation column reflux-withdrawal pump, P2. butanols rectifier column reflux extraction pump, P3. positive isobutanol separation column reflux-withdrawal pump, E1. reactive distillation column condenser, E2. reactive distillation column reboiler, E3. butanols rectifying tower condenser, E4. butanols rectifying tower reboiler, the positive isobutanol separation column condenser of E5., the positive isobutanol separation column reboiler of E6., C1. compressor
Logistics: S01. raw material butyraldehyde, S02. butyraldehyde gas, S03. raw hydrogen, S04. reactive distillation column top gaseous phase, S05. unreacted hydrogen, S06. the hydrogen after compressor, S07. liquid phase after condensation, S08. reactive distillation column phegma, S09. reactive distillation column overhead extraction light component product, S10. cymogene alcohol product, S11. butanols rectifying tower top gaseous phase, S12. condensator outlet liquid phase, S13. butanols rectifier column reflux liquid, S14. mixed butyl alcohol, S15. heavy constituent by product, S16. positive isobutanol separation column top gaseous phase, S17. liquid phase after condensation, S18. positive isobutanol separation column phegma, S19. isobutanol product, S20. propyl carbinol product
Embodiment
Below in conjunction with accompanying drawing, method provided by the utility model and device are further detailed.
The utility model is achieved by the following technical solution:
Butyraldehyde hydrogenation produces the reaction and rectification device of butanols, as shown in Figure 1, comprises vaporizer, reactive distillation column, butanols rectifying tower, positive isobutanol separation column, condenser, reboiler, compressor, pump and relevant feedstocks pipeline and the pipeline being connected above equipment; Reactive distillation column, butanols rectifying tower, positive isobutanol separation column tower top all arrange condenser, all arrange reboiler at the bottom of reactive distillation column, butanols rectifying tower, positive isobutanol separation column tower; Evaporator overhead gaseous phase outlet is connected to reactive distillation column; Reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, and compressor outlet is connected to reactive distillation column hydrogen feed mouth, and condensator outlet liquid phase, as light component product extraction, is that cymogene alcohol product is connected to butanols rectifying tower opening for feed at the bottom of tower; Butanols rectifying tower ejects material and enters positive isobutanol separation column for mixed butyl alcohol, is heavy constituent by product at the bottom of tower; The discharging of positive isobutanol separation column tower top is isobutanol product, and discharging at the bottom of tower is propyl carbinol product.
The reactive distillation method that butyraldehyde hydrogenation of the present utility model produces butanols is: the butyraldehyde gas (S02) of raw material butyraldehyde (S01) after evaporator (V1) vaporization enters the bottom of reactive distillation column (T1) conversion zone together with raw hydrogen (S03), reactive distillation column (T1) top gaseous phase (S04) enters reactive distillation column overhead condenser (E1), after condensation, gas phase is that the hydrogen (S06) of unreacted hydrogen (S05) after compressor (C1) pressurization returns reactive distillation column (T1) charging, after condensation, liquid phase (S07) obtains liquid phase through reactive distillation column reflux-withdrawal pump (P1), control by operating reflux ratio, a part is as phegma (S08), another part is as tower top light constituent (S09) extraction, at the bottom of tower, extraction cymogene alcohol (S10) is as the charging of butanols rectifying tower (T2), butanols rectifying tower (T2) top gaseous phase (S11) obtains liquid phase through condenser (E3) condensed liquid phase (S12) through butanols rectifier column reflux extraction pump (P2), control by operating reflux ratio, a part is as phegma (S13), another part be mixed butyl alcohol (S14) as positive isobutanol separation column (T3) charging, extraction heavy constituent by product (S15) at the bottom of tower, positive isobutanol separation column (T3) top gaseous phase (S16) obtains liquid phase through condenser (E5) condensed liquid phase (S17) through positive isobutanol separation column reflux-withdrawal pump (P3), control by operating reflux ratio, a part is as phegma (S18), another part as isobutanol product (S19) extraction, extraction propyl carbinol (S20) product at the bottom of tower.
Butyraldehyde hydrogenation is produced in the reactive distillation method of butanols: evaporator pressure is 0.01-3MPa; Reactive distillation column adopts nickel and/or copper-based catalysts, and conversion zone temperature is 100-250 DEG C, preferred 110-130 DEG C, and pressure is 0.01-2MPa, and reflux ratio is 10-100, and hydrogen aldehyde mol ratio is 10:1-30:1; Butanols rectifying tower pressure is 0.5-1MPa, and reflux ratio is 1-100; Positive isobutanol separation column pressure is 0.1-1MPa, and reflux ratio is 20-100.
Embodiment 1
In this example, evaporator pressure is 0.01MPa; Reactive distillation column adopts copper-based catalysts, and conversion zone temperature is 250 DEG C, and pressure is 0.01MPa, and reflux ratio is 100, and hydrogen aldehyde mol ratio is 30:1; Butanols rectifying tower pressure is 0.5MPa, and reflux ratio is 100; Positive isobutanol separation column pressure is 0.1MPa, and reflux ratio is 100.Finally obtaining isopropylcarbinol quality purity is 99.9%, and propyl carbinol quality purity is 99.9%.
Embodiment 2
In this example, evaporator pressure is 3MPa; Reactive distillation column adopts nickel-base catalyst, and conversion zone temperature is 100 DEG C, and pressure is 2MPa, and reflux ratio is 10, and hydrogen aldehyde mol ratio is 10:1; Butanols rectifying tower pressure is 0.7MPa (a), and reflux ratio is 1; Positive isobutanol separation column pressure is 1MPa, and reflux ratio is 20.Finally obtaining isopropylcarbinol quality purity is 99%, and propyl carbinol quality purity is 99.5%.
Embodiment 3
In this example, evaporator pressure is 1MPa (a); Reactive distillation column adopts copper-based catalysts, and conversion zone temperature is 120 DEG C, and pressure is 0.6MPa, and reflux ratio is 30, and hydrogen aldehyde mol ratio is 20:1; Butanols rectifying tower pressure is 1MPa, and reflux ratio is 30; Positive isobutanol separation column pressure is 0.5MPa, and reflux ratio is 50.Finally obtaining isopropylcarbinol quality purity is 99.8%, and propyl carbinol quality purity is 99.9%.

Claims (1)

1. butyraldehyde produces a reaction and rectification device for butanols, comprises vaporizer, reactive distillation column, butanols rectifying tower, positive isobutanol separation column, condenser, reboiler, compressor, pump and relevant feedstocks pipeline and the pipeline being connected above equipment; It is characterized in that reactive distillation column, butanols rectifying tower and positive isobutanol separation column tower top all arrange condenser, the end all arranges reboiler; Evaporator overhead gaseous phase outlet is connected to reactive distillation column; Reactive distillation column overhead condenser gaseous phase outlet is connected to compressor, and compressor outlet is connected to reactive distillation column hydrogen feed mouth, and condensator outlet liquid phase, as light component product extraction, is that cymogene alcohol product is connected to butanols rectifying tower opening for feed at the bottom of tower; Butanols rectifying tower ejects material and enters positive isobutanol separation column for mixed butyl alcohol, is heavy constituent by product at the bottom of tower; The discharging of positive isobutanol separation column tower top is isobutanol product, and discharging at the bottom of tower is propyl carbinol product.
CN201420738995.7U 2014-11-28 2014-11-28 Butyraldehyde hydrogenation produces the reaction and rectification device of butanols Expired - Fee Related CN204342701U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115006862A (en) * 2022-06-15 2022-09-06 浙江卫星能源有限公司 Energy-saving high-purity n-butanol extraction system and method
CN116212771A (en) * 2023-03-09 2023-06-06 宁波巨化化工科技有限公司 Liquid phase single reaction kettle capable of circularly reacting to improve overall yield

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115006862A (en) * 2022-06-15 2022-09-06 浙江卫星能源有限公司 Energy-saving high-purity n-butanol extraction system and method
CN115006862B (en) * 2022-06-15 2023-10-17 浙江卫星能源有限公司 Energy-saving high-purity n-butanol extraction system and method
CN116212771A (en) * 2023-03-09 2023-06-06 宁波巨化化工科技有限公司 Liquid phase single reaction kettle capable of circularly reacting to improve overall yield

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