CN105289027A - Reaction and rectification device and method for producing isopropanolamine - Google Patents
Reaction and rectification device and method for producing isopropanolamine Download PDFInfo
- Publication number
- CN105289027A CN105289027A CN201510630414.7A CN201510630414A CN105289027A CN 105289027 A CN105289027 A CN 105289027A CN 201510630414 A CN201510630414 A CN 201510630414A CN 105289027 A CN105289027 A CN 105289027A
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- Prior art keywords
- isopropanolamine
- tower
- reaction
- reactive distillation
- distillation column
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Links
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 67
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229940102253 isopropanolamine Drugs 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 68
- 238000000066 reactive distillation Methods 0.000 claims description 54
- 239000001294 propane Substances 0.000 claims description 34
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 24
- 238000012546 transfer Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 4
- 230000000306 recurrent effect Effects 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 23
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 239000006227 byproduct Substances 0.000 abstract description 5
- 230000009615 deamination Effects 0.000 abstract description 2
- 238000006481 deamination reaction Methods 0.000 abstract description 2
- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- 238000007086 side reaction Methods 0.000 abstract 1
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 description 4
- 229940043276 diisopropanolamine Drugs 0.000 description 4
- 238000010923 batch production Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 150000001412 amines Chemical group 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 description 1
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a reaction and rectification device and a reaction and rectification method for producing isopropanolamine. In the condition that water is used as a catalyst, ammonia and epoxypropane are used as raw materials to be put into a reaction and rectification tower for reaction, heavy components after the reaction are purified by a stripping section, light components after the reaction are purified by a rectifying section and then enter a condenser to be condensed, a part of distillate in the condenser flows back to the reaction and rectification tower again through a distillate return pipe, and the other part of distillate is discharged out of the tower through a top product discharge pipe and is collected as products; materials at the bottom of the tower enter a reboiler for being heated through a communicating pipe, a part of the materials at the bottom of the tower is discharged out of the tower through a bottom product discharge pipe and is collected as an isopropanolamine mixture, and the other part of the materials at the bottom of the tower flow back to the top of the reaction and rectification tower through a reboiled material circulating return pipe. By using the reaction and rectification device and the reaction and rectification method, the total energy consumption of deamination and dehydration can be reduced, side reactions and by-products are effectively avoided, and the product purity is increased.
Description
Technical field
The present invention relates to isopropanolamine production technical field, especially relate to a kind of reaction and rectification device and method of producing isopropanolamine.
Background technology
Isopropanolamine is a kind of chemicals having surcharge, has important purposes, as final products or intermediate in numerous industry such as medicine, chemical industry, petrochemical industry.Isopropanolamine is mainly generated by expoxy propane and ammonia react, and reactant is all the mixture of three kinds of derivatives of isopropanolamine usually.
Manufacturer's great majority domestic at present adopt batch process to produce, and use ammoniacal liquor production technology, are passed into by expoxy propane in batch reactor, react with the low concentration ammoniacal liquor of about 25%, after batch reactor reaction, then are purified by rectifying column.Batch process is adopted to produce isopropanolamine, processing step is loaded down with trivial details, efficiency is low, and energy consumption is high, due to ammonia concn and reaction temperature all lower (being no more than 60 DEG C), therefore reaction speed is slow, the reactor volume of identical productivity is large, and the energy consumption of deamination, dehydration after reaction is large, and production cost is high, production technology falls behind, and need carry out technological transformation.
Summary of the invention
The present invention is the problem that batch process in order to solve prior art produces that isopropanolamine processing step is loaded down with trivial details, efficiency is low, energy consumption is high, provides the reaction and rectification device of production isopropanolamine that a kind of continuous production is good, can reduce energy consumption, reduce gross investment and running cost, enhance productivity.
Present invention also offers a kind of processing step simple, process stabilization is controlled, and production efficiency is high, the method for the production isopropanolamine that energy consumption is low.
To achieve these goals, the present invention is by the following technical solutions:
A kind of reaction and rectification device producing isopropanolamine, comprise reactive distillation column, condenser and reboiler, described reactive distillation column is divided into rectifying section from top to bottom, conversion zone and stripping section, reactive distillation top of tower is provided with water inlet pipe and condenser feed pipe, described condenser feed pipe is connected with condenser inlet, condensator outlet is connected with the distillate return duct and overhead product discharge nozzle that are connected with rectifying section, the top of described conversion zone is provided with ammoniacal liquor feed pipe, the middle part of conversion zone is provided with propylene oxide feed pipe, be connected with reboiler import by communicating pipe at the bottom of reactive distillation column tower, described reboiler top is connected to the discharging recurrent canal that boils again be connected with reactive distillation column bottom, the Matter Transfer return duct that boils again being connected with bottom product discharge nozzle bottom described reboiler and being connected with reactive distillation column overhead.The reaction and rectification device of production isopropanolamine of the present invention, utilize the reaction between ammonia and expoxy propane very fast, and the feature that the boiling point difference of reactant and product isopropanolamine is very large, make expoxy propane and ammonia carry out reacting and purifying in a reactive distillation column simultaneously, structure is simple, energy continuous seepage isopropanolamine, greatly reduces energy consumption, reduces gross investment and running cost.
A kind of method of producing isopropanolamine, in reactive distillation column, with ammonia and expoxy propane for raw material, under the condition of water as catalyst, reaction generates isopropanolamine product, concrete steps are: ammoniacal liquor, expoxy propane are reacted under dropping into the effect of conversion zone at catalyst through ammoniacal liquor feed pipe, propylene oxide feed pipe respectively, catalyst water, through the water inlet pipe charging of tower top, enters conversion zone through rectifying section and carries out catalysis; Reacted heavy constituent enters stripping section downwards and purifies, reacted light component is upwards after rectifying section is purified, condenser condenses is entered through condenser feed pipe, a part of distillate in condenser is back to reactive distillation column again through distillate return duct, and another part distillate discharges tower and collect as product outward through overhead product discharge nozzle; Materials at bottom of tower heats through entering reboiler communicating pipe again, and a part of materials at bottom of tower discharges tower and collect as isopropanolamine mixture outward through bottom product discharge nozzle, and another part materials at bottom of tower is back to reactive distillation column overhead through the Matter Transfer return duct that boils again.The method of production isopropanolamine of the present invention is implemented in reactive distillation column, design is optimized to reactive distillation column, by distillate reflux entry evaporation endothermic to control balanced reaction heat release, the reaction temperature caused because of reaction very exothermic is avoided to rise, thus it is controlled to make whole course of reaction stablize, adjustable suitable reflux ratio is with the amine chain rate making reactive distillation column maintenance higher simultaneously, thus reduce or avoid the formation of byproduct, obtain the high-purity isopropanolamine product that byproduct is less; A part of materials at bottom of tower is back to reactive distillation column through the Matter Transfer return duct that boils again again purify, after the water mixing of wherein unreacted monoisopropanolamine and tower top charging, can be used as catalyst, to save the consumption of catalyst water; Ammoniacal liquor and expoxy propane can arrange one or more charging aperture, but the feed entrance point of ammoniacal liquor must be positioned on the feed entrance point of expoxy propane, and distance sets according to actual production between the two; Reactive distillation column tower bottom product is the isopropanolamine mixture of monoisopropanolamine, diisopropanolamine (DIPA), triisopropanolamine and water, in Propanolamine mixture, the content of diisopropanolamine (DIPA) is 90 ~ 99.5%(wt), reactive distillation column tower bottom product can be delivered to rectifying column and purifies further or directly deliver to user.
As preferably, the proportioning that described ammoniacal liquor, expoxy propane are 0.1 ~ 1.1 by ammonia and expoxy propane molar ratio feeds intake.
As preferably, the feeding temperature of described ammoniacal liquor, expoxy propane is 30 ~ 300 DEG C.
As preferably, by controlling distillate reflux ratio to make the molar ratio of ammonia and expoxy propane in conversion zone for 1.1 ~ 300.
As preferably, described reactive distillation column overhead temperatures is 30 ~ 101 DEG C.
As preferably, described conversion zone temperature is 101 ~ 350 DEG C.
As preferably, described reactive distillation column column bottom temperature is 180 ~ 240 DEG C.
As preferably, the full tower operating pressure of described reactive distillation column is 1 ~ 100bar.
As preferably, described reboiler temperature is 290 ~ 400 DEG C.
Therefore, the present invention has following beneficial effect:
(1) a kind of reaction and rectification device producing isopropanolamine is devised, utilize the reaction between ammonia and expoxy propane very fast, and the feature that the boiling point difference of reactant and product isopropanolamine is very large, make expoxy propane and ammonia carry out reacting and purifying in a reactive distillation column simultaneously, structure is simple, energy continuous seepage isopropanolamine, greatly reduces energy consumption, reduces gross investment and running cost.
(2) method of production isopropanolamine of the present invention is implemented in reactive distillation column, design is optimized to reactive distillation column, by distillate reflux entry evaporation endothermic to control balanced reaction heat release, the reaction temperature caused because of reaction very exothermic is avoided to rise, thus it is controlled to make whole course of reaction stablize, control reflux ratio simultaneously and keep high amine chain rate to make reactive distillation column, thus reduce or avoid the formation of byproduct, obtain the high-quality isopropanolamine that byproduct is less.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation that the present invention produces the reaction and rectification device of isopropanolamine.
In figure: reactive distillation column 1, condenser 2, reboiler 3, rectifying section 4, conversion zone 5, stripping section 6, water inlet pipe 7, condenser feed pipe 8, ammoniacal liquor feed pipe 9, propylene oxide feed pipe 10, distillate return duct 11, overhead product discharge nozzle 12, communicating pipe 13, boil discharging recurrent canal 14 again, bottom product discharge nozzle 15, then the Matter Transfer return duct 16 that boils.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
A kind of reaction and rectification device producing isopropanolamine as shown in Figure 1, reaction and rectification device comprises reactive distillation column 1, condenser 2 and reboiler 3, reactive distillation column is divided into rectifying section 4 from top to bottom, conversion zone 5 and stripping section 6, reactive distillation top of tower is provided with water inlet pipe 7 and condenser feed pipe 8, condenser feed pipe is connected with condenser inlet, condensator outlet is connected with the distillate return duct 11 and overhead product discharge nozzle 12 that are connected with rectifying section, the top of conversion zone is provided with ammoniacal liquor feed pipe 9, the middle part of conversion zone is provided with propylene oxide feed pipe 10, by being connected with reboiler import communicating pipe 13 at the bottom of reactive distillation column tower, reboiler top is connected with the discharging recurrent canal 14 that boils again be connected with reactive distillation column bottom, the Matter Transfer return duct 16 that boils again being connected with bottom product discharge nozzle 15 bottom reboiler and being connected with reactive distillation column overhead.
A kind of method of producing isopropanolamine, in reactive distillation column, with ammonia and expoxy propane for raw material, under the condition of water as catalyst, reaction generates isopropanolamine product, concrete steps are: by ammoniacal liquor, expoxy propane is respectively through ammoniacal liquor feed pipe, propylene oxide feed pipe drops into conversion zone and reacts under the effect of catalyst water, ammoniacal liquor, the proportioning that expoxy propane is 0.1 by ammonia and expoxy propane molar ratio feeds intake, control ammoniacal liquor, the feeding temperature of expoxy propane is 30 DEG C, catalyst water is through the water inlet pipe charging of tower top, enter conversion zone through rectifying section and carry out catalysis, controlling reactive distillation column overhead temperatures is 30 DEG C, conversion zone temperature is 101 DEG C, reactive distillation column column bottom temperature is 180 DEG C, the full tower operating pressure of reactive distillation column is 1bar, reacted heavy constituent enters stripping section downwards and purifies, reacted light component is upwards after rectifying section is purified, condenser condenses is entered through condenser feed pipe, a part of distillate in condenser is back to reactive distillation column again through distillate return duct, control distillate reflux ratio to make the molar ratio of ammonia and expoxy propane in conversion zone for 1.1, another part distillate through overhead product discharge nozzle discharge tower outward and collect, materials at bottom of tower heats through entering reboiler communicating pipe again, reboiler temperature is 290 DEG C, part materials at bottom of tower discharges tower and collect as isopropanolamine mixture outward through bottom product discharge nozzle, and another part materials at bottom of tower is back to reactive distillation column rectification and purification again through the Matter Transfer return duct that boils again.
Embodiment 2
The reaction and rectification device of the production isopropanolamine in the present embodiment is identical with Fig. 1 of embodiment 1, difference is technological parameter in the method for production isopropanolamine, be specially: the proportioning that ammoniacal liquor, expoxy propane are 1 by ammonia and expoxy propane molar ratio feeds intake, the feeding temperature of control ammoniacal liquor, expoxy propane is 250 DEG C; Controlling reactive distillation column overhead temperatures is 50 DEG C, and conversion zone temperature is 300 DEG C, and reactive distillation column column bottom temperature is 200 DEG C, and the full tower operating pressure of reactive distillation column is 50bar; In conversion zone, the molar ratio of ammonia and expoxy propane is 30.
Embodiment 3
The reaction and rectification device of the production isopropanolamine in the present embodiment is identical with Fig. 1 of embodiment 1, difference is technological parameter in the method for production isopropanolamine, be specially: the proportioning that ammoniacal liquor, expoxy propane are 1.1 by ammonia and expoxy propane molar ratio feeds intake, the feeding temperature of control ammoniacal liquor, expoxy propane is 300 DEG C; Controlling reactive distillation column overhead temperatures is 101 DEG C, and conversion zone temperature is 350 DEG C, and reactive distillation column column bottom temperature is 240 DEG C, and the full tower operating pressure of reactive distillation column is 100bar; In conversion zone, the molar ratio of ammonia and expoxy propane is 300.
Above-described embodiment only for technical conceive of the present invention and feature are described, its object is to allow person skilled in the art scholar can understand content of the present invention practical according to this, can not limit the scope of the invention with this.All equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (10)
1. produce the reaction and rectification device of isopropanolamine for one kind, it is characterized in that, described reaction and rectification device comprises reactive distillation column (1), condenser (2) and reboiler (3), described reactive distillation column is divided into rectifying section (4) from top to bottom, conversion zone (5) and stripping section (6), reactive distillation top of tower is provided with water inlet pipe (7) and condenser feed pipe (8), described condenser feed pipe is connected with condenser inlet, condensator outlet is connected with the distillate return duct (11) and overhead product discharge nozzle (12) that are connected with rectifying section, the top of described conversion zone is provided with ammoniacal liquor feed pipe (9), the middle part of conversion zone is provided with propylene oxide feed pipe (10), by being connected with reboiler import communicating pipe (13) at the bottom of reactive distillation column tower, described reboiler top is connected with the discharging recurrent canal (14) that boils again be connected with reactive distillation column bottom, the Matter Transfer return duct (16) that boils again being connected with bottom product discharge nozzle (15) bottom described reboiler and being connected with reactive distillation column overhead.
2. the method utilizing reaction and rectification device as claimed in claim 1 to produce isopropanolamine, it is characterized in that, in reactive distillation column, with ammonia and expoxy propane for raw material, under the condition of water as catalyst, reaction generates isopropanolamine product, concrete steps are: ammoniacal liquor, expoxy propane are reacted under dropping into the effect of conversion zone at catalyst through ammoniacal liquor feed pipe, propylene oxide feed pipe respectively, catalyst water, through the water inlet pipe charging of tower top, enters conversion zone through rectifying section and carries out catalysis; Reacted heavy constituent enters stripping section downwards and purifies, reacted light component is upwards after rectifying section is purified, condenser condenses is entered through condenser feed pipe, a part of distillate in condenser is back to reactive distillation column again through distillate return duct, and another part distillate discharges tower and collect as product outward through overhead product discharge nozzle; Materials at bottom of tower heats through entering reboiler communicating pipe again, part materials at bottom of tower discharges tower and collect as isopropanolamine mixture outward through bottom product discharge nozzle, and another part materials at bottom of tower is back to reactive distillation column rectification and purification again through the Matter Transfer return duct that boils again.
3. the method for production isopropanolamine according to claim 2, is characterized in that, the proportioning that described ammoniacal liquor, expoxy propane are 0.1 ~ 1.1 by ammonia and expoxy propane molar ratio feeds intake.
4. the method for the production isopropanolamine according to Claims 2 or 3, is characterized in that, the feeding temperature of described ammoniacal liquor, expoxy propane is 30 ~ 300 DEG C.
5. the method for production isopropanolamine according to claim 2, is characterized in that, by controlling distillate reflux ratio to make the molar ratio of ammonia and expoxy propane in conversion zone for 1.1 ~ 300.
6. the method for production isopropanolamine according to claim 2, is characterized in that, described reactive distillation column overhead temperatures is 30 ~ 101 DEG C.
7. the method for production isopropanolamine according to claim 2, is characterized in that, described conversion zone temperature is 101 ~ 350 DEG C.
8. the method for production isopropanolamine according to claim 2, is characterized in that, described reactive distillation column column bottom temperature is 180 ~ 240 DEG C.
9. the method for production isopropanolamine according to claim 2, is characterized in that, the full tower operating pressure of described reactive distillation column is 1 ~ 100bar.
10. the method for production isopropanolamine according to claim 2, is characterized in that, described reboiler temperature is 290 ~ 400 DEG C.
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CN201510630414.7A CN105289027B (en) | 2015-09-29 | 2015-09-29 | Reaction and rectification device and method for producing isopropanolamine |
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CN201510630414.7A CN105289027B (en) | 2015-09-29 | 2015-09-29 | Reaction and rectification device and method for producing isopropanolamine |
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CN105289027B CN105289027B (en) | 2017-05-10 |
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Cited By (2)
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CN110559678A (en) * | 2019-10-21 | 2019-12-13 | 无锡赫利邦化工科技有限公司 | rectifying tower for synthesizing and separating polymethoxy dimethyl ether and use method thereof |
CN110878027A (en) * | 2019-10-23 | 2020-03-13 | 合肥亿帆生物制药有限公司 | Synthesis method and device of N-N-butyl ethanolamine |
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Cited By (3)
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CN110559678B (en) * | 2019-10-21 | 2024-02-27 | 无锡赫利邦化工科技有限公司 | Rectifying tower for synthesizing and separating polymethoxy dimethyl ether and application method thereof |
CN110878027A (en) * | 2019-10-23 | 2020-03-13 | 合肥亿帆生物制药有限公司 | Synthesis method and device of N-N-butyl ethanolamine |
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