반응 #344419

반응 방정식

acryloyloxyethyltrimethylammonium

methyl chloride

dimethylaminoethyl acrylate

hydroquinone methyl ether

acrylate

acrylate

dimethylaminoethyl acrylate

oxygen

water acrylate

→

final product

Acryloyloxyethyltrimethylammonium Chloride

용매

water

water

반응 조건

후처리

1. 1
   기타Throughout the reaction the temperature
2. 2
   기타is kept at 47° C.
3. 3
   workup.WAIT0.5 Nl/h of air is then injected continuously into the reactor and over a period of 1 hour
4. 4
   workup.ADDITIONintroduced lower than 15)
5. 5
   기타80% in water are recovered
6. 6
   workup.WAITThe final product is then subjected to an injection of air at a flow rate of 7 Nl/h for 1/2 hour
7. 7
   workup.WAIThot and then for 1/2 hour at room temperature

실험 절차

78 g of liquid methyl chloride are charged with stirring into a jacketed reactor. The temperature is raised to 47° C. and the pressure of the system equilibrates at 9.6 bars absolute. In the first stage 33 g of dimethylaminoethyl acrylate stabilized with the aid of 700 ppm of hydroquinone methyl ether are injected into the reactor over a period of 20 minutes (that is 16% of the total quantity of acrylate necessary for reaction) In a second stage the complement of the acrylate and the water are injected simultaneously and continuously in a water/acrylate weight ratio of the order of 0.4 over a period of 2 hours. Throughout the reaction the temperature is kept at 47° C. and the pressure in the reactor drops to 3.2 bars absolute at the end of the injection of reactants. 0.5 Nl/h of air is then injected continuously into the reactor and over a period of 1 hour the reactor pressure is returned progressively to atmospheric pressure while a blow-off exit flow rate lower than 1.5 Nl/h is maintained (whence a ratio of the blow-off volumetric flow rates to the oxygen introduced lower than 15). 71 g of water and 205 g of dimethylaminoethyl acrylate have been employed in this operation and 343 g of acryloyloxyethyltrimethylammonium at a concentration of. 80% in water are recovered. The final product is then subjected to an injection of air at a flow rate of 7 Nl/h for 1/2 hour hot and then for 1/2 hour at room temperature. The final product obtained has the following characteristics: water: 20.3% acrylic acid: 0.23% dimethylaminoethyl acrylate: 0.15% methyl chloride: 10 ppm polymer: nil storage stability: longer than 1 year.

출처