Method for synthesizing dimethyl diallyl ammonium chloride cationic monomer

A technology of dimethyl diallyl ammonium chloride and cationic monomers, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of hydroxyl compounds, etc. It can solve the problem of not doing too much research on feeding methods and increasing the production cost of the process , There are problems such as temperature limitations, to achieve the effect of increased stability, reduced loss, and reduced loss rate

Inactive Publication Date: 2011-07-20
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0035] It can be seen from the above literature that the improvement of the synthesis process is basically limited to temperature adjustment, and the feeding method has not been explored too much. Allyl chloride and sodium hydr

Method used

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  • Method for synthesizing dimethyl diallyl ammonium chloride cationic monomer
  • Method for synthesizing dimethyl diallyl ammonium chloride cationic monomer
  • Method for synthesizing dimethyl diallyl ammonium chloride cationic monomer

Examples

Experimental program
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Example Embodiment

[0062] Example 1

[0063] (1) Take a 40% aqueous solution containing 0.8 mol of dimethylamine and place it in a 500ml four-necked round bottom flask. Add 0.4 mol of allyl chloride dropwise at 0°C. After 1 hour of dropping, proceed to the first Stage reaction, the reaction temperature is 0°C, and gas chromatography is turned on to monitor the reaction process. After 3 hours of reaction, it is monitored that the content of allyl chloride in the system is zero and the next step is started;

[0064] (2) Alternately add 0.4 mol of allyl chloride and 0.8 mol of sodium hydroxide at a temperature of 10°C. After 1 hour of dropping, proceed to the second stage of the reaction. The reaction temperature is 10°C. After 3 hours of reaction, it is monitored that the substance in the system is basically When tertiary amine, proceed to the next step;

[0065] (3) Continue to add 0.8 mol of allyl chloride at 25°C. After 1 hour of dropping, proceed to the third stage of the reaction. The reaction time...

Example Embodiment

[0075] Example 2

[0076] (1) Take a 40% aqueous solution containing 0.8 mol of dimethylamine and place it in a 500 ml four-neck round bottom flask. Add 0.4 mol of allyl chloride dropwise at 10°C. After the drop is completed in 2 hours, proceed to the first Stage reaction, the reaction temperature is 10℃, and the gas chromatography is turned on to monitor the reaction process. After 2 hours of reaction, it is monitored that the allyl chloride content in the system is zero and the next step is started;

[0077] (2) Add 0.4mol of allyl chloride and 0.8mol of sodium hydroxide at the same time at a temperature of 30℃. After 2h, the second stage reaction is carried out. The reaction temperature is 30℃. After the reaction for 2h, the substance in the system is basically When tertiary amine, proceed to the next step;

[0078] (3) Continue to add 0.8 mol of allyl chloride at 25°C. After 2 hours of dropping, proceed to the third stage reaction. The reaction time is 6h and the reaction temper...

Example Embodiment

[0082] Example 3

[0083] (1) Take a 40% aqueous solution containing 0.8 mol of dimethylamine and place it in a 500ml four-neck round bottom flask. Add 0.4 mol of allyl chloride dropwise at 10°C. After 3 hours of dropping, proceed to the first Stage reaction, the reaction temperature is 10℃, and the gas chromatography is turned on to monitor the reaction process. After 1 hour of reaction, it is monitored that the allyl chloride content in the system is zero and the next step is started;

[0084] (2) Add 0.4mol of allyl chloride and 0.8mol of sodium hydroxide alternately or at the same time at a temperature of 20℃. After 3 hours of dripping, proceed to the second stage reaction. The reaction temperature is 20℃. The system is monitored after 1 hour of reaction. When the middle substance is basically tertiary amine, proceed to the next step;

[0085] (3) Continue to add 0.8 mol of allyl chloride at 25°C. After 2 hours of dropping, proceed to the third stage of the reaction. The reactio...

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Abstract

The invention discloses a method for synthesizing a dimethyl diallyl ammonium chloride cationic monomer. In the method, a change is made to the conventional feeding mode that dimethylamine and allyl chloride are fed according to a ratio of 1:1, and the feeding mode that dimethylamine and allyl chloride are fed according to a ratio of 1:1 in a first stage is divided into two steps on the basis of the conventional one-step method, wherein in the first step, dimethylamine and allyl chloride are fed first according to a ratio of 1:0.5; and in the second step, allyl chloride and sodium hydroxide are fed according to a ratio of 0.5:1. After reaction for a certain time period, allyl chloride in the same amount is dripped continuously and thus the cationic monomer product is obtained. The cationic monomer product is distilled under reduced pressure to remove volatile impurities, sodium chloride is removed by suction filtration, an alkali is added to remove involatile impurities, and thus, thehigh-purity dimethyl diallyl ammonium chloride cationic monomer is obtained. In the invention, the dimethylamine loss caused by volatilization at normal temperature is avoided, the reaction is performed under a low pH value condition, the generation of impurities is reduced, and thus, high-purity cationic monomer is obtained.

Description

technical field [0001] The invention belongs to the field of surfactants, and in particular relates to a synthesis method of a quaternary ammonium salt cationic monomer, that is, a synthesis method of the cationic monomer dimethyl diallyl ammonium chloride. Background technique [0002] 1. Brief introduction of cationic monomer: [0003] Dimethyldiallylammonium Chloride (DMDAAC) is a cationic monomer with a wide range of uses, and its polymer has the advantages of high positive charge density, low cost, good water solubility and low toxicity, and is widely used It is used in industries such as mining, daily chemical industry, petroleum treatment and sewage treatment, so it has been paid more and more attention by researchers. [0004] 2. Cationic monomer one-step and two-step synthesis process [0005] Many researchers have begun to explore the synthesis process of this cationic monomer. According to previous studies, the overall reaction equation for the synthesis of DMDA...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C211/20C07C209/12C07C33/03C07C29/124C07C47/22C07C45/29
Inventor 哈成勇魏续瑞沈敏敏胡志忠岑学杨于静张延奎
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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