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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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  • Abstract
  • Description
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  • Application Information

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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 hydroxide are used alternately or dimethylamine is added at the same time. The feeding method impurity There are many and there is a temperature limit, generally requiring 0 ~ 5 ℃, which increases the production cost of the process

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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Embodiment 1

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

[0064] (2) Alternately add 0.4mol allyl chloride and 0.8mol sodium hydroxide dropwise at a temperature of 10°C. After 1h, the second stage reaction is carried out. The reaction temperature is 10°C. After 3 hours of reaction, the substances in the system are basically When tertiary amine starts to carry out next step operation;

[0065] (3) Continue to add 0.8mol allyl chloride dropwise at 25° C. After 1 hour of dripping, carry out the third-stage reaction. The reaction time is 7 hours, a...

Embodiment 2

[0076] (1) Take a 40% aqueous solution containing 0.8mol dimethylamine in a mass fraction, place it in a 500ml four-necked round bottom flask, add 0.4mol allyl chloride dropwise at a temperature of 10°C, drop it in 2 hours, and carry out the first Phase reaction, the reaction temperature is 10°C, and the gas chromatography is turned on to monitor the reaction process at the same time. After 2 hours of reaction, the content of allyl chloride in the system is monitored to be zero, and the next step is started;

[0077] (2) Add 0.4mol allyl chloride and 0.8mol sodium hydroxide dropwise at the same time at a temperature of 30°C. After 2 hours, the second stage reaction is carried out. The reaction temperature is 30°C. After 2 hours of reaction, the substances in the system are basically When tertiary amine starts to carry out next step operation;

[0078] (3) Continue to add 0.8mol allyl chloride dropwise at 25° C., drop it over 2 hours, and carry out the third stage reaction. The...

Embodiment 3

[0083] (1) Take a 40% aqueous solution containing 0.8mol dimethylamine in a mass fraction, place it in a 500ml four-neck round bottom flask, add 0.4mol allyl chloride dropwise at a temperature of 10°C, drop it in 3 hours, and carry out the first Phase reaction, the reaction temperature is 10°C, and the gas chromatograph is turned on to monitor the reaction process at the same time. After 1 hour of reaction, the content of allyl chloride in the system is monitored to be zero, and the next step is started;

[0084] (2) Add 0.4 mol allyl chloride and 0.8 mol sodium hydroxide alternately or simultaneously at 20°C, drop it in 3 hours, and proceed to the second stage reaction, the reaction temperature is 20°C, and the system is monitored after 1 hour of reaction When the substance in the middle is basically a tertiary amine, start to carry out the next step;

[0085] (3) Continue to add 0.8mol allyl chloride dropwise at 25° C., drop it over 2 hours, and carry out the third-stage rea...

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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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