CN103435499B - Novel preparation method for mono ethanol diisopropanolamine - Google Patents
Novel preparation method for mono ethanol diisopropanolamine Download PDFInfo
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- CN103435499B CN103435499B CN201310359544.2A CN201310359544A CN103435499B CN 103435499 B CN103435499 B CN 103435499B CN 201310359544 A CN201310359544 A CN 201310359544A CN 103435499 B CN103435499 B CN 103435499B
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- propylene oxide
- thanomin
- diisopropanolamine
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- epoxy propane
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Abstract
A novel preparation method for mono ethanol diisopropanolamine comprises the following steps: weighing ethanolamine, epoxy propane and mass modifier (quinones) according to design proportion; adding ethanolamine and mass modifier, as well as certain amount of epoxy propane, into a reactor with a strong mixing device; mixing uniformly without a heat source; when the reaction temperature reaches a certain value, opening a circulation condensing unit, and adding dropwise the residual epoxy propane; controlling the reaction temperature at 40-80 DEG C, mixing during the reaction for 1-4 h, and obtaining the product mono ethanol diisopropanolamine, wherein the molar ratio of ethanolamine and epoxy propane is (0.5-1.5):(1.5-2.5), the amount of the mass modifier is 0.01%-0.015% of the total mass of ethanolamine and epoxy propane. The method is simple in technology, low in manufacturing cost, high in productivity, and suitable for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of novel monoethanolamine diisopropanolamine (DIPA) (EDIPA), belong to organic synthesis field.
Background technology
Alcamines material is the important organic compound of a class, and the structure of its uniqueness and charge distribution, be used as surfactant usually, is widely used in industrial chemicals, each fields such as dyestuff, medicine, material of construction.The existing method preparing monoethanolamine diisopropanolamine (DIPA) has and there is such as complicated process of preparation, the defect such as cost is high, productive rate is low.
Summary of the invention
The invention provides the synthetic method of the monoethanolamine diisopropanolamine (DIPA) that a kind of preparation technology is simple, cost is low, product yield is higher.
The technical scheme that the present invention solves the employing of its technical problem is: a kind of preparation method of monoethanolamine diisopropanolamine (DIPA), comprises the following steps:
After taking thanomin, propylene oxide and quality adjustment agent in setting ratio, first add in the reactor of intense stirring device thanomin, quality adjustment agent and 10% ~ 50% propylene oxide, without the need to thermal source, stir, question response temperature rises to 40 ~ 80 DEG C, opens circulation condensation device; Then drip remainder propylene oxide, control temperature of reaction at 40 ~ 80 DEG C, stirring reaction 1 ~ 4h, obtains monoethanolamine diisopropanol amine product;
The mol ratio of described thanomin and propylene oxide is: (0.5 ~ 1.5): (1.5 ~ 2.5) (;
The consumption of described quality adjustment agent is 0.01% ~ 0.15% of thanomin and propylene oxide quality sum.
Reaction equation of the present invention is as follows:
The present invention adopts thanomin and propylene oxide to be reaction raw materials, because propylene oxide boiling point is low, easy ring-opening polymerization, the features such as reaction process heat release, select to add quality adjustment agent, carry out reacting and improve reaction yield under making normal temperature, the method is easy and simple to handle, production cost is low, productive rate high (can reach more than 95.2%), is applicable to suitability for industrialized production.
Specific implementation method
Embodiment 1
24.4g thanomin, the agent of 0.021g quality adjustment, 9.3g propylene oxide is added in the 125ml four-hole bottle that mechanical stirring device, circulation condensation device, thermometer, pear shape separatory funnel are housed, uniform stirring, question response temperature is between 50 ~ 60 DEG C, open circulation condensation device, by separating funnel, drip 37.2g propylene oxide in four-hole bottle, in control reaction flask, temperature is at 50 ~ 60 DEG C, after treating that propylene oxide drips, namely insulation 1.5h obtains monoethanolamine diisopropanolamine (DIPA) finished product.Gas chromatographic analysis is carried out in sampling, and productive rate is 97.6%.
Embodiment 2
24.4g thanomin, the agent of 0.042g quality adjustment, 9.3g propylene oxide is added in the 125ml four-hole bottle that mechanical stirring device, circulation condensation device, thermometer, pear shape separatory funnel are housed, uniform stirring, question response temperature is between 50 ~ 60 DEG C, open circulation condensation device, by separating funnel, drip 37.2g propylene oxide in four-hole bottle, in control reaction flask, temperature is at 50 ~ 60 DEG C, after treating that propylene oxide drips, namely insulation 1.5h obtains monoethanolamine diisopropanolamine (DIPA) finished product.Gas chromatographic analysis is carried out in sampling, and productive rate is 95.2%.
Embodiment 3
24.4g thanomin, the agent of 0.021g quality adjustment, 11.6g propylene oxide is added in the 125ml four-hole bottle that mechanical stirring device, circulation condensation device, thermometer, pear shape separatory funnel are housed, uniform stirring, question response temperature is between 50 ~ 60 DEG C, open circulation condensation device, by separating funnel, drip 34.9g propylene oxide in four-hole bottle, in control reaction flask, temperature is at 50 ~ 60 DEG C, after treating that propylene oxide drips, namely insulation 1.5h obtains monoethanolamine diisopropanolamine (DIPA) finished product.Gas chromatographic analysis is carried out in sampling, and productive rate is 98.3%.
Embodiment 4
24.4g thanomin, the agent of 0.042g quality adjustment, 11.6g propylene oxide is added in the 125ml four-hole bottle that mechanical stirring device, circulation condensation device, thermometer, pear shape separatory funnel are housed, uniform stirring, question response temperature is between 50 ~ 60 DEG C, open circulation condensation device, by separating funnel, drip 34.9g propylene oxide in four-hole bottle, in control reaction flask, temperature is at 50 ~ 60 DEG C, after treating that propylene oxide drips, namely insulation 1.5h obtains monoethanolamine diisopropanolamine (DIPA) finished product.Gas chromatographic analysis is carried out in sampling, and productive rate is 96.7%.
Claims (2)
1. a preparation method for monoethanolamine diisopropanolamine (DIPA), is characterized in that, comprises the following steps:
After taking thanomin, propylene oxide and quality adjustment agent by predetermined proportion, there iing in intense stirring device reactor the propylene oxide first adding thanomin, quality adjustment agent and propylene oxide total mass 10% ~ 50%, without the need to thermal source, stir, question response temperature rises to 40 ~ 80 DEG C, opens circulation condensation device, then residual epoxide propane is dripped, control temperature of reaction at 40 ~ 80 DEG C, stirring reaction 1 ~ 4h, obtains monoethanolamine diisopropanol amine product;
The mol ratio of described thanomin and propylene oxide is: 0.5 ~ 1.5:1.5 ~ 2.5;
The consumption of described quality adjustment agent is 0.01% ~ 0.15% of thanomin and propylene oxide quality sum;
Described whole reaction is without the need to thermal source.
2. the preparation method of monoethanolamine diisopropanolamine (DIPA) according to claim 1, is characterized in that: described quality adjustment agent is for improving reaction yield, and its consumption is 0.01% ~ 0.15% of thanomin and propylene oxide quality sum.
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| CN201310359544.2A CN103435499B (en) | 2013-08-19 | 2013-08-19 | Novel preparation method for mono ethanol diisopropanolamine |
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| CN103435499A CN103435499A (en) | 2013-12-11 |
| CN103435499B true CN103435499B (en) | 2015-07-08 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112028779B (en) * | 2020-10-10 | 2022-05-24 | 安徽海螺新材料科技有限公司 | Preparation method of hydroxyethyl diisopropanolamine by using chloropropanol as raw material |
| CN115057787B (en) * | 2022-05-06 | 2024-05-14 | 史才军 | Preparation method of monoethanol diisopropanolamine |
Citations (6)
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| US2622099A (en) * | 1947-09-12 | 1952-12-16 | Carbochimique Sa | Process of preparing alkanolamines |
| CN101314533A (en) * | 2008-07-03 | 2008-12-03 | 南京红宝丽股份有限公司 | Method for continuously producing high-efficiency concrete grinding aid |
| CN102557960A (en) * | 2010-12-28 | 2012-07-11 | 苏州飞翔新材料研究院有限公司 | Method for producing alkyl alcohol amine |
| CN102924301A (en) * | 2012-11-01 | 2013-02-13 | 史才军 | Preparation method of N,N-bis(2-hydroxyethyl)isopropanolamine |
| CN103204779A (en) * | 2013-04-27 | 2013-07-17 | 弗克科技(苏州)有限公司 | Alkylol amine and preparation method |
| CN103242175A (en) * | 2013-03-28 | 2013-08-14 | 宁波市联凯化学有限公司 | Preparation method of monoethanol diisopropanolamine |
-
2013
- 2013-08-19 CN CN201310359544.2A patent/CN103435499B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2622099A (en) * | 1947-09-12 | 1952-12-16 | Carbochimique Sa | Process of preparing alkanolamines |
| CN101314533A (en) * | 2008-07-03 | 2008-12-03 | 南京红宝丽股份有限公司 | Method for continuously producing high-efficiency concrete grinding aid |
| CN102557960A (en) * | 2010-12-28 | 2012-07-11 | 苏州飞翔新材料研究院有限公司 | Method for producing alkyl alcohol amine |
| CN102924301A (en) * | 2012-11-01 | 2013-02-13 | 史才军 | Preparation method of N,N-bis(2-hydroxyethyl)isopropanolamine |
| CN103242175A (en) * | 2013-03-28 | 2013-08-14 | 宁波市联凯化学有限公司 | Preparation method of monoethanol diisopropanolamine |
| CN103204779A (en) * | 2013-04-27 | 2013-07-17 | 弗克科技(苏州)有限公司 | Alkylol amine and preparation method |
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