CN102718667A - Method for preparing triethanolamine - Google Patents
Method for preparing triethanolamine Download PDFInfo
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- CN102718667A CN102718667A CN2012102148536A CN201210214853A CN102718667A CN 102718667 A CN102718667 A CN 102718667A CN 2012102148536 A CN2012102148536 A CN 2012102148536A CN 201210214853 A CN201210214853 A CN 201210214853A CN 102718667 A CN102718667 A CN 102718667A
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- trolamine
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Abstract
The invention belongs to the field of chemical synthesis, and in particular relates to a method for preparing triethanolamine. Aqueous ammonia and ethylene oxide are used as raw materials, wherein the ethylene oxide is not required to be vaporized, is directly supercharged by a metering tank and enters a reaction container to react with the aqueous ammonia; the materials in the reaction container are shifted out by means of an outer circulating pump, cooled through a heat exchanger and then sprayed into the reaction container through a static atomization ejector arranged on the reaction container, so that the materials quickly react; a stock solution of the triethanolamine is prepared approximately at normal temperature under normal pressure; and the stock solution is purified through a distillation kettle, and the triethanolamine product is prepared. Processes of liquid phase feeding, outer circulating cooling and atomization jet reaction are adopted in the method, so that the auto-agglutination of the ethylene oxide at a high temperature in the metering tank in the background technology is realized, and risk of steam heating vaporization is eliminated; and few auto-polymers are produced, and the metering tank is not required to be periodically purged. By the method, the materials react quickly and completely, the contact specific surface area of the reaction materials is enlarged, side reaction is reduced, the consumption of the raw materials is low, and the yield of the product is high.
Description
Technical field
The invention belongs to the field of chemical synthesis, be specifically related to a kind of preparation method of trolamine.
Background technology
Trolamine is to use more a kind of product, and it is widely used in cement industry, urethane industry and cosmetic industry and pharmaceutical industries.Demand to it is rise trend in recent years.Trolamine is to be made by ammoniacal liquor and reacting ethylene oxide; Among the present preparation technology; Oxyethane needs vaporization feeding at high temperature; Both consumed lot of energy, and had very high danger again, to promote quality and benefits very important so invent a kind of novel process novel method of producing trolamine.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of trolamine; Through changing the material feeding mode, and the process of accelerated reaction, the trolamine of preparation has advantages such as steady quality, yield are high, with short production cycle; And effectively reduce production cost, satisfied the market requirement.
The preparation method of a kind of trolamine of the present invention may further comprise the steps:
(1) according to the parts by weight meter, earlier 1 ~ 2 part of liquefied ammonia being mixed with concentration is that 20 ~ 25% ammonia soln injects reaction vessel, 5 ~ 10 parts oxyethane is directly got in the reaction vessel by test tank supercharging 0.1～0.2mpa react with ammonia soln again;
(2) outer recycle pump shifts out the material in the reaction vessel through interchanger and is cooled to temperature of reaction; The static spray nozzle of in reaction vessel, establishing again sprays in the reaction vessel, makes the material accelerated reaction, and reaction in 2 ~ 5 hours finishes; Make trolamine stoste; Wherein, the temperature in the reaction vessel is 30 ℃ ~ 60 ℃, reaction pressure 0 ~ 0.2mpa;
(3) the trolamine stoste that makes gets into still kettle, and the moisture content in the stoste is steamed, and processes trolamine.
The invention has the advantages that: (1) oxyethane need not be vaporized; Directly get into reaction vessel and ammoniacal liquor reaction by the test tank supercharging; Outer recycle pump shifts out the static spray nozzle that after interchanger cooling, on reaction vessel, is provided with again with the material in the reaction vessel and sprays in the reaction vessel, makes the material accelerated reaction, makes trolamine stoste under normal temperature, the normal pressure being similar to; Purify through still kettle again, promptly make the trolamine product.(2) the present invention adopts liquid phase feeding, outer circulation cooling, atomised jet reaction process, has both solved in the background technology under the oxyethane high temperature autohemagglutination problem in test tank, has eliminated the danger of steam heating vaporization again; Autopolymer is few, and test tank need not regularly purge.(3) adopt technology of the present invention can make material reaction quick and complete, increased the reaction mass contacted specific surface area, reduced side reaction, make raw material consumption low, product yield is high.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
Embodiment 1:
Prepare trolamine according to following steps:
(1) according to the parts by weight meter, earlier 1 part of liquefied ammonia being mixed with concentration is that 25% ammonia soln injects reaction vessel, nitrogen replacement 3 times, side oxygen level＜150ppm.Again 10 parts oxyethane is directly got in the reaction vessel by test tank supercharging 0.1mpa and react with ammonia soln;
(2) outer recycle pump shifts out the material in the reaction vessel through interchanger and is cooled to temperature of reaction; The static spray nozzle of in reaction vessel, establishing again sprays in the reaction vessel, makes the material accelerated reaction, and reaction in 3 hours finishes; Make trolamine stoste; Wherein, the temperature in the reaction vessel is 45 ℃, reaction pressure 0.1mpa;
(3) the trolamine stoste that makes gets into still kettle, and the moisture content in the stoste is steamed, and processes trolamine.
Embodiment 2:
Prepare trolamine according to following steps:
(1) according to the parts by weight meter, earlier 1 part of liquefied ammonia being mixed with concentration is that 20% ammonia soln injects reaction vessel, nitrogen replacement 3 times, side oxygen level＜150ppm.Again 9 parts oxyethane is directly got in the reaction vessel by test tank supercharging 0.2mpa and react with ammonia soln;
(2) outer recycle pump shifts out the material in the reaction vessel through interchanger and is cooled to temperature of reaction; The static spray nozzle of in reaction vessel, establishing again sprays in the reaction vessel, makes the material accelerated reaction, and reaction in 5 hours finishes; Make trolamine stoste; Wherein, the temperature in the reaction vessel is 30 ℃, vacuum reaction;
(3) the trolamine stoste that makes gets into still kettle, and the moisture content in the stoste is steamed, and processes trolamine.
Embodiment 3:
Prepare trolamine according to following steps:
(1) according to the parts by weight meter, earlier 1.3 parts of liquefied ammonia being mixed with concentration is that 20% ammonia soln injects reaction vessel, nitrogen replacement 3 times, side oxygen level＜150ppm.Again 10 parts oxyethane is directly got in the reaction vessel by test tank supercharging 0.2mpa and react with ammonia soln;
(2) outer recycle pump shifts out the material in the reaction vessel through interchanger and is cooled to temperature of reaction; The static spray nozzle of in reaction vessel, establishing again sprays in the reaction vessel, makes the material accelerated reaction, and reaction in 2 hours finishes; Make trolamine stoste; Wherein, the temperature in the reaction vessel is 60 ℃, reaction pressure 0.2mpa;
(3) the trolamine stoste that makes gets into still kettle, and the moisture content in the stoste is steamed, and processes trolamine.
Claims (1)
1. the preparation method of a trolamine is characterized in that may further comprise the steps:
(1) according to the parts by weight meter, earlier 1 ~ 2 part of liquefied ammonia being mixed with concentration is that 20 ~ 25% ammonia soln injects reaction vessel, 5 ~ 10 parts oxyethane is directly got in the reaction vessel by test tank supercharging 0.1～0.2mpa react with ammonia soln again;
(2) outer recycle pump shifts out the material in the reaction vessel through interchanger and is cooled to temperature of reaction; The static spray nozzle of in reaction vessel, establishing again sprays in the reaction vessel, makes the material accelerated reaction, and reaction in 2 ~ 5 hours finishes; Make trolamine stoste; Wherein, the temperature in the reaction vessel is 30 ℃ ~ 60 ℃, reaction pressure 0 ~ 0.2mpa;
(3) the trolamine stoste that makes gets into still kettle, and the moisture content in the stoste is steamed, and processes trolamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102148536A CN102718667A (en) | 2012-06-27 | 2012-06-27 | Method for preparing triethanolamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102148536A CN102718667A (en) | 2012-06-27 | 2012-06-27 | Method for preparing triethanolamine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102718667A true CN102718667A (en) | 2012-10-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012102148536A Pending CN102718667A (en) | 2012-06-27 | 2012-06-27 | Method for preparing triethanolamine |
Country Status (1)
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644576A (en) * | 2004-04-27 | 2005-07-27 | 抚顺佳化化工有限公司 | Production of triethanolamine products |
| CN101100433A (en) * | 2007-07-25 | 2008-01-09 | 辽宁华丰化工（集团）有限公司 | Method for producing pure triethanolamine containing micro-water |
| CN101735077A (en) * | 2009-12-11 | 2010-06-16 | 广西壮族自治区化工研究院 | Production method and production equipment for synthesizing ethanolamine by ethylene oxide |
| WO2011082967A1 (en) * | 2009-12-17 | 2011-07-14 | Basf Se | Method for producing higher ethanolamines |
-
2012
- 2012-06-27 CN CN2012102148536A patent/CN102718667A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644576A (en) * | 2004-04-27 | 2005-07-27 | 抚顺佳化化工有限公司 | Production of triethanolamine products |
| CN101100433A (en) * | 2007-07-25 | 2008-01-09 | 辽宁华丰化工（集团）有限公司 | Method for producing pure triethanolamine containing micro-water |
| CN101735077A (en) * | 2009-12-11 | 2010-06-16 | 广西壮族自治区化工研究院 | Production method and production equipment for synthesizing ethanolamine by ethylene oxide |
| WO2011082967A1 (en) * | 2009-12-17 | 2011-07-14 | Basf Se | Method for producing higher ethanolamines |
Non-Patent Citations (1)
| Title |
|---|
| FENG, RUMING等: "Shape-selective amination of EO over HZSM-5 for MEA and DEA", 《CATALYSIS COMMUNICATIONS》, vol. 11, no. 15, 31 December 2010 (2010-12-31), pages 1220 - 1223, XP027249801 * |
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Application publication date: 20121010 |