CN106349085A - Separation and purification method of crude isopropyl amine - Google Patents
Separation and purification method of crude isopropyl amine Download PDFInfo
- Publication number
- CN106349085A CN106349085A CN201610736843.7A CN201610736843A CN106349085A CN 106349085 A CN106349085 A CN 106349085A CN 201610736843 A CN201610736843 A CN 201610736843A CN 106349085 A CN106349085 A CN 106349085A
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- China
- Prior art keywords
- tower
- aminopropane
- isopropyl amine
- purification method
- deammoniation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a separation and purification method of crude isopropyl amine. The separation and purification method includes: sequentially subjecting the crude isopropyl amine obtained by the hydrogenation ammonization of acetone to continuous distillation of a deamination tower and an isopropyl amine under a pressurizing condition to separate the isopropyl amine so as to obtain the isopropyl amine product with the purity being above 99.8%. The separation and purification method is little in equipment, simple in flow, low in energy consumption and easy to operate.
Description
First, technical field
The present invention relates to a kind of process for purification, the isolation and purification method of specifically a kind of thick 2-aminopropane..
2nd, background technology
2-aminopropane., also known as Mono Isopropylamine, molecular formula is c3h9N, colourless have volatile liquid, has ammonia odor, can with water,
Ethanol and ether are miscible.2-aminopropane. is a kind of important fine-chemical intermediate, belongs to low-carbon (LC) fatty amine (c2～c8) class product,
Can be used for producing pesticide (as herbicide atrazine, prometryn, glyphosate isopropyl amine salt, bentazone), medicine (as diisopropylamine dichloroacetate, gains in depth of comprehension
Peace, carvisken, clorprenaline etc.), dyestuff intermediate, rubber accelerator, hard water inorganic agent and detergent, be also used for manufacturing surface and live
Property agent, textile auxiliary, solubilizing agent, detergent, depilatory etc..
With acetone for the production technology of Material synthesis 2-aminopropane., though acetone is largely converted into 2-aminopropane., unavoidably
The small part that has be converted into isopropanol and diisopropylamine.Therefore, isopropanol, two different can be contained in the isopropyl amine crude product of synthesis
Propylamine and other impurities.
The thick 2-aminopropane. purifying plant of tradition: generally comprise 2-aminopropane. knockout tower and dehydrating tower, 2-aminopropane. knockout tower and dehydration
Tower, all using forced refluence condenser, is equipped with return tank and reflux pump；Bottom of towe is provided with reboiler.The 2-aminopropane. that this technique obtains produces
Product purity is relatively low, and diisopropylamine returns synthesis system, and plant energy consumption is higher, is unfavorable for that synthesis system is reacted.
2-aminopropane. purifying plant after improvement: using four Deethanizer design, including 2-aminopropane. knockout tower, Mono Isopropylamine tower, dehydration
Tower, diisopropylamine tower, can respectively be isolated by Mono Isopropylamine, diisopropylamine product.This device increased equipment investment it is adaptable to
The high thick 2-aminopropane. purification of diisopropylamine content.As very low thick isopropyl amine product in purified diisopropylamine content, then increased not
Necessary investment and operating cost, economy is poor.
3rd, content of the invention
The present invention is intended to provide a kind of isolation and purification method of thick 2-aminopropane., technical problem to be solved is by 2-aminopropane.
Separating-purifying from by-product, obtains 2-aminopropane. sterling.The inventive method process route is short, number of devices is few, operation energy consumption is low,
The purity that 2-aminopropane. can be made reaches more than 99.8%.
The thick 2-aminopropane. that the present invention uses makes synthesis by oneself for acetone hydrogenation ammoniation process, and concrete preparation process is as follows:
1st, before reaction feeds intake, first use the air in nitrogen displacement reactor, then the hydrogen of preheating is continually fed into instead
Answer in device, make the catalyst temperature in reactor rise to 90～180 DEG C, the pressure in reactor rise to 0.2～1.8mpa；
2nd, acetone is preheated to 60～110 DEG C；
3rd, hydrogen and gas ammonia are mixed to get gaseous mixture, by described charge heating to 60～130 DEG C；
4th, the gaseous mixture after the acetone after preheating step 2 and step 3 preheat first sends into carburator, heats mixing with steam
Material is to 80～130 DEG C, then mixed material is sent into superheater, with steam heating mixt material to 85～180 DEG C, is then fed into
In the reactor of step 1, carry out in the presence of a catalyst being hydrogenated with aminating reaction (instead at 0.2～1.8mpa, 90～180 DEG C
Should be successive reaction), obtain crude product, after prepared crude product cooling through cooler cooling, gas-liquid separator separates gas and
Liquid, gas main component is hydrogen, can recycle；Liquid is thick 2-aminopropane., isopropyl amine content ＞ in thick 2-aminopropane.
50%.
Described mixed material is hydrogen, ammonia, the gaseous mixture material of acetone.
Acetone, hydrogen, the mol ratio of ammonia are 1:1～6:1～6.
Acetone air speed is 0.1～1.5h-1.
Described reactor is calandria type fixed bed reactor, using the design concept of water shifting heat, to keep course of reaction to be
Isothermal reaction.
Described catalyst is mo-co-ni/al2o3Catalyst, ball shape structure is it is easy to reaction produces the diffusion of heat.
The isolation and purification method of the thick 2-aminopropane. of the present invention, is in the bar pressurizeing by the prepared thick 2-aminopropane. of acetone hydrogenation ammonification
Pass sequentially through deammoniation tower and 2-aminopropane. tower continuous still under part, separate the isopropyl amine product obtaining purity more than 99.8%.
Technical process is as follows:
Thick 2-aminopropane. is sent in deammoniation tower, deammoniation tower bottom temperature is 120～200 DEG C, tower top temperature is 35～70 DEG C,
Tower pressure interior force controls in 0.8～0.3mpa (absolute pressure)；Gas ammonia, can be former as 2-aminopropane. synthesis from deammoniation tower removed overhead
Material；The material that deammoniation tower tower reactor bottom is discharged enters the purification of 2-aminopropane. tower in the presence of pressure reduction.2-aminopropane. tower bottom temperature is
105～140 DEG C, tower top temperature is 55～80 DEG C, and tower pressure interior force controls in 0.2～0.6mpa (absolute pressure)；2-aminopropane. tower tower
After the condensation of gaseous substance condensed device that top row goes out, a part produces as isopropyl amine product, and a part is as backflow backflow；Different
The waste water that propylamine tower tower reactor bottom is discharged discharges after being fed directly to sewage-treatment plant process up to standard.
The supplementary liquefied ammonia of deammoniation tower, as backflow, need not arrange return-flow system, energy consumption is relatively low.
The 2-aminopropane. purity of 2-aminopropane. column overhead extraction is up to more than 99.8%.The waste water that 2-aminopropane. tower tower reactor bottom is discharged
Middle diisopropylamine content about 0.56%, isopropanol content about 0.33%, the value of non-recovery purification, sewage disposal can be fed directly to
Discharge after device process up to standard.
Between deammoniation tower, 2-aminopropane. tower, pressure reduction maintains 0.6～0.7mpa.
Compared with the prior art, beneficial effects of the present invention are embodied in:
Isolation and purification method process route of the present invention is short, number of devices is few, energy consumption is low, and the purity of 2-aminopropane. can be made to reach
More than 99.8%.
4th, brief description
Fig. 1 is the process flow diagram of the present invention.
In figure, 1 pan feeding pump, 2 deammoniation towers, 3 deammoniation tower reboilers, 4 2-aminopropane. towers, 5 2-aminopropane. tower reboilers, 6 2-aminopropane .s
Overhead condenser, 7 2-aminopropane. tower return tanks, 8 2-aminopropane. tower reflux pumps, 9 self-adjusting valves, 10 pressure gauges, 11 temperature measurers.
5th, specific embodiment
The invention will be further described below in conjunction with the accompanying drawings.
As shown in figure 1, being derived from the thick 2-aminopropane. (isopropyl amine content 52% in thick 2-aminopropane .) of 2-aminopropane. synthesis system through entering
Material pump 1 pumps into and carries out deamination in deammoniation tower 2, with steam (1.2mpa, 190 DEG C) to the thick 2-aminopropane. thing in deammoniation tower reboiler 3
Material is heated, and to control tower top temperature to be 35 DEG C, bottom temperature is 140 DEG C, and in deammoniation tower 2, pressure is 0.98mpa (absolute pressure).
Directly go 2-aminopropane. synthesis system from deammoniation tower 2 top gas ammonia out, tower top supplements fresh liquefied ammonia and flows back as deammoniation tower 2
Liquid.Temperature is measured by temperature measurer 11, and pressure is measured by pressure gauge 10, and needs to be adjusted according to technique.
The material of deammoniation tower 2 bottom is delivered continuously in 2-aminopropane. tower 4 in the presence of pressure reduction, with steam (0.6mpa,
150 DEG C) material in p-isopopylaniline tower reboiler 5 heated, and to control tower top temperature to be 79 DEG C, bottom temperature is 120 DEG C,
In 2-aminopropane. tower 4, pressure is 0.35mpa (absolute pressure).From 2-aminopropane. tower 4 top gaseous substance out through 2-aminopropane. overhead condensation
After device 6 cooling becomes liquid phase, enter 2-aminopropane. tower return tank 7, need to be adjusted according to technique, in 2-aminopropane. tower reflux pump 8
In the presence of, a part is back to as backflow in 2-aminopropane. tower 4, and part extraction isopropyl amine product removes finished pot.Temperature
Measured by temperature measurer 11, pressure is measured by pressure gauge 10, and need to be adjusted according to technique.
The diisopropylamine content about 0.56% that 2-aminopropane. tower 4 bottom is discharged, the waste water of isopropanol content about 0.33% are straight
Pick and discharge to sewage-treatment plant process up to standard.
Claims (5)
1. a kind of isolation and purification method of thick 2-aminopropane. it is characterised in that:
It is that the thick 2-aminopropane. that acetone hydrogenation ammonification is obtained passes sequentially through deammoniation tower under pressure and 2-aminopropane. tower is continuous
Distillation, separates the isopropyl amine product obtaining purity more than 99.8%.
2. method according to claim 1 it is characterised in that:
Deammoniation tower bottom temperature is 120～200 DEG C, and tower top temperature is 35～70 DEG C, and tower pressure interior force controls in 0.8～0.3mpa.
3. method according to claim 1 it is characterised in that:
2-aminopropane. tower bottom temperature is 105～140 DEG C, and tower top temperature is 55～80 DEG C, tower pressure interior force controls 0.2～
0.6mpa.
4. the method according to claim 1,2 or 3 it is characterised in that:
Pressure reduction between deammoniation tower and 2-aminopropane. tower maintains 0.6～0.7mpa.
5. method according to claim 1 it is characterised in that:
The supplementary liquefied ammonia of deammoniation tower is as backflow.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610736843.7A CN106349085A (en) | 2016-08-26 | 2016-08-26 | Separation and purification method of crude isopropyl amine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610736843.7A CN106349085A (en) | 2016-08-26 | 2016-08-26 | Separation and purification method of crude isopropyl amine |
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| CN106349085A true CN106349085A (en) | 2017-01-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610736843.7A Pending CN106349085A (en) | 2016-08-26 | 2016-08-26 | Separation and purification method of crude isopropyl amine |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1130621A (en) * | 1995-03-06 | 1996-09-11 | 化学工业部北京化工研究院 | Process for producing isopropyl amine |
| CN101684073A (en) * | 2008-09-28 | 2010-03-31 | 中国石油化工股份有限公司 | Method for producing isopropylamine |
| CN201525814U (en) * | 2009-09-25 | 2010-07-14 | 山东华鲁恒升化工股份有限公司 | Isopropyl amine crude product purifying device |
-
2016
- 2016-08-26 CN CN201610736843.7A patent/CN106349085A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1130621A (en) * | 1995-03-06 | 1996-09-11 | 化学工业部北京化工研究院 | Process for producing isopropyl amine |
| CN101684073A (en) * | 2008-09-28 | 2010-03-31 | 中国石油化工股份有限公司 | Method for producing isopropylamine |
| CN201525814U (en) * | 2009-09-25 | 2010-07-14 | 山东华鲁恒升化工股份有限公司 | Isopropyl amine crude product purifying device |
Non-Patent Citations (2)
| Title |
|---|
| 殷振海: "异丙胺生产工艺", 《河北化工》 * |
| 王亮: "1500吨/年异丙胺分离精制工程设计", 《天津大学硕士论文集》 * |
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