A kind of preparation method of n,n-bis(2-hydroxyethyl)aminomethylphosphonic acid diethyl ester

A technology of diethyl aminomethylphosphonate and diethyl phosphite, applied in the field of N, can solve problems affecting product quality and later application, increasing energy consumption of production process, unfavorable formation of intermediates, etc., and achieve product yield High, less catalyst consumption, short time effect

Active Publication Date: 2011-12-14
WANHUA CHEM NINGBO RONGWEI POLYURETHANE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process also uses a formaldehyde solution containing a large amount of water, which is not conducive to the formation of intermediates. The high-temperature dehydration step after the first step of reaction has a poor dehydration effect, and it is difficult to reduce the moisture in the entire system even at 80°C. to a reasonable range, and the presence of moisture will directly affect the next step of the reaction, affecting the quality of the product and later application
If the high temperature water removal time is prolonged, it will not only affect the quality of the intermediate, but also increase the energy consumption of the production process, which is not conducive to industrial production

Method used

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  • A kind of preparation method of n,n-bis(2-hydroxyethyl)aminomethylphosphonic acid diethyl ester
  • A kind of preparation method of n,n-bis(2-hydroxyethyl)aminomethylphosphonic acid diethyl ester
  • A kind of preparation method of n,n-bis(2-hydroxyethyl)aminomethylphosphonic acid diethyl ester

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 1. Weigh 360 parts of n-propanol in a 2L three-neck flask equipped with a magnetic stirrer, a constant pressure dropping funnel and a thermometer, raise the temperature to 70°C, add 180 parts of paraformaldehyde solid, and adjust the polyformaldehyde with sodium hydroxide solution The pH of the formaldehyde solution is 9-11, until the paraformaldehyde is completely dissolved, and the temperature is lowered to 30°C.

[0033] 2. Weigh 78 parts of anhydrous sodium sulfate into a three-necked flask, weigh 573 parts of diethanolamine in a constant pressure dropping funnel, slowly add diethanolamine under stirring, the reaction is an exothermic reaction, control the reaction temperature at 40°C , after the dropwise addition of diethanolamine was completed, the temperature was kept at 40° C., and the reaction was continued for 1 hour. Then the temperature was lowered to 30°C, and the sodium sulfate after absorbing water was removed by filtration.

[0034]3. Raise the temperat...

Embodiment 2

[0047] 1. Weigh 222 parts of n-butanol in a 2L three-neck flask with a magnetic stirrer, a constant pressure dropping funnel and a thermometer, raise the temperature to 80°C, add 180 parts of paraformaldehyde solid, and adjust the polyformaldehyde with sodium hydroxide solution The pH of the formaldehyde solution is 9-11, until the paraformaldehyde is completely dissolved, and the temperature is lowered to 30°C.

[0048] 2. Weigh 100 parts of calcium oxide into a three-necked flask, weigh 623.8 parts of diethanolamine in a constant pressure dropping funnel, slowly add diethanolamine under stirring, the reaction is an exothermic reaction, control the reaction temperature at 40°C, After the ethanolamine was added dropwise, the temperature was raised to 50° C., and the reaction was continued for 0.5 hours. Then the temperature was lowered to 30°C, and the calcium oxide after absorbing water was removed by filtration.

[0049] 3. Raise the temperature to 45-50°C, under the condit...

Embodiment 3

[0053] 1. Weigh 700 parts of isopropanol in a 2L three-neck flask equipped with a magnetic stirrer, a constant pressure dropping funnel and a thermometer, raise the temperature to 60°C, add 180 parts of paraformaldehyde solid, and adjust the polyformaldehyde with sodium hydroxide solution The pH of the formaldehyde solution is 9-11, until the paraformaldehyde is completely dissolved, and the temperature is lowered to 30°C.

[0054] 2. Weigh 80 parts of anhydrous calcium sulfate into a three-necked flask, weigh 519.8 parts of diethanolamine in a constant pressure dropping funnel, slowly add diethanolamine under stirring, the reaction is an exothermic reaction, control the reaction temperature at 30°C , after the addition of diethanolamine was completed, the temperature was kept at 30° C., and the reaction was continued for 2 hours. Calcium sulfate after absorbing water was removed by filtration.

[0055] 3. Raise the temperature to 45-50°C, under the condition that the degree ...

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Abstract

The invention provides a preparation method of diethyl N,N-bis(2- hydroxyethyl) aminomethylphosphonate, comprising the following steps: (1) carrying out depolymerization on paraformaldehyde; (2) carrying out ring formation on formaldehyde and diethanol amine to prepare 3-(2- hydroxyethyl)-1,3-oxazolidine; (3) reacting 3-(2- hydroxyethyl)-1,3-oxazolidine with diethyl phosphite in the presence of anhydrous Lewis acid catalysts; and (4) filtering and recovering the catalysts to obtain a yellow transparent liquid product. The overall yield of the whole process reaches more than 99 %, and the content of diethyl N,N-bis(2- hydroxyethyl) aminomethylphosphonate in the product is 94 %-96 %. The preparation method disclosed in the invention is simple and efficient, has the advantages of high product yield, high content of effective components in the product, reduction of temperature in dehydration process, shortening of time, and low energy consumption, reduces the water content of the final product to 0.1-0.2 %, and reduces the dosage of the catalysts by 20-50%. The preparation method is suitable for large-scale industrial production.

Description

Technical field: [0001] The invention relates to a preparation method of a phosphite halogen-free flame retardant, in particular to a preparation method of N,N-bis(2-hydroxyethyl)aminomethylphosphonic acid diethyl ester. Background technique: [0002] With the development of the synthetic material industry, flame retardant has become an important content of synthetic material modification, and the research on flame retardant materials has also attracted the attention of scientific researchers all over the world. At present, the most commonly used flame retardants in the world are halogen-containing flame retardants, especially brominated flame retardants, which are added in a small amount and have high flame retardant efficiency, but because they emit a large amount of toxic smoke and corrosive gases when burning, causing Environmental pollution and endanger human life safety, so its application range is more and more restricted. In recent years, halogen-free flame-retardan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38C08K5/5353
Inventor 华卫琦鞠昌讯陈海波丁建生刘瑞阳
Owner WANHUA CHEM NINGBO RONGWEI POLYURETHANE
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