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ChemicalBook CAS DataBase List Diallyldimethylammonium chloride
7398-69-8

Diallyldimethylammonium chloride synthesis

2synthesis methods
Dimethylamine

124-40-3

Allyl chloride

107-05-1

Diallyldimethylammonium chloride

7398-69-8

1. 150 parts of a 33% solution of dimethylamine are added to the reactor, heated and stirred until foaming starts at 30°C. Subsequently, 43 parts of 33% dimethylamine solution were added from the receiving tank and the temperature was controlled at 7°C. 2. Two parts of 50% sodium hydroxide solution were added, stirred and heated to 85°C to promote evaporation of the dimethylamine. Continue heating to 100 °C to end this step. An incomplete product of 83.4 parts with 2.2% dimethylamine content was obtained; and 103 parts of dimethylamine solution (including the absorbent) with 56.4% dimethylamine content. 3. In a three-necked flask equipped with a stirrer, a thermometer, a condenser tube and a titration funnel, 100 parts of a 56.4% solution of dimethylamine were added and 30% allyl chloride was slowly added at 0 °C. 4. 180 parts of allyl chloride and 100 parts of 50% sodium hydroxide solution were added dropwise simultaneously at 3°C to 5°C to control the pH between 9.5 and 10.5. 5. After completion of the addition, the temperature was raised to 44°C for refluxing until the pH of the reaction dropped to 6.4, the heating was stopped and cooling was carried out. 6. The reaction mixture was filtered to obtain 64.8 parts of NaCl and 325.3 parts of an aqueous solution of dimethyldiallylammonium chloride. The content of dimethyldiallylammonium chloride was determined to be 60.8% and the yield was 97.65% (based on amine calculations).

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Yield:7398-69-8 97.65%

Reaction Conditions:

with sodium hydroxide at 0 - 44; pH=6.4;Concentration;

Steps:

1 Example 1

The sump by adding 33% dimethylamine solution 150 parts, heating, stirring for 30 °C bubble started from the, receiving tank by adding 43 parts 33% dimethylamine solution, the temperature is controlled at 7 °C. Stirring to 85 °C by adding the 2 concentrations in order to 50% of sodium hydroxide solution, free of the dimethylamine more easily is to boil off, continue to heating, stirring for 100 °C end of the. To obtain: the incomplete 83.4 parts, dimethylamine content 2.2% ; dimethylamine solution concentration of 103 parts (including the absorption liquid, in order to with), dimethylamine content 56.4%. In the is provided with a stirrer, thermometer, condenser tube, dropping funnel of the three-port flask after adding the concentration of 56.4% dimethylamine solution 100 parts, in 0 °C slowly adding 30 allyl chloride ; for 3 °C -5 ° C at the same time dropping 180 allyl chloride and 50% sodium hydroxide solution of 100 parts, to control the pH value of 9.5-10.5 between; material feeding is finished, the temperature is increased to 44 °C reflux, the reaction to the pH value equal to 6.4, stop heating, and cooling; filtering, receive nacl 64.8 parts, dimethyl diallyl ammonium chloride aqueous solution 325.3 parts, through determining, dimethyl diallyl ammonium chloride is in a content of 60.8%, the yield is 97.65% (according to b a amine idea ).

References:

CN104557569,2016,B Location in patent:Paragraph 0031; 0032; 0033

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