Clean production method of alkoxylation glycerol triacrylate
A technology of glycerol triacrylate and alkoxylation, applied in chemical instruments and methods, separation/purification of carboxylate, preparation of carboxylate, etc., can solve the problems of rising cost, intractable treatment and high treatment cost
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Embodiment 1
[0061] In the 3000L reactor, drop into 600 kilograms of toluene, normal hexane 350, ethoxylated glycerin (C 9 h 20 o 6 , molecular weight 224) 618 kilograms, 655 kilograms of acrylic acid, 8 kilograms of p-hydroxyanisole, 9 kilograms of sodium hypophosphite, 55 kilograms of methanesulfonic acid; Open stirring, pass into compressed air continuously in the still by distributor at the bottom of the still, be heated up to Start reflux dehydration at 85-90°C, esterification reaction for 9-10 hours, kettle temperature 90-105°C, when reflux dehydration until no water comes out, the acid value is 25-30mgKOH / g, after the reaction is completed, cool to 40°C; add 25 kg of caustic soda and 60 kg of water, stirred for 30 minutes; added 6 kg of magnesium polysilicate, stirred and adsorbed for 30 minutes; then the water and solvent were distilled under reduced pressure at 50-95 ° C under a vacuum degree of -0.098 MPa, and the recovered water After stratification with the solvent, the water ca...
Embodiment 2
[0063] In the 3000L reactor, drop into 585 kilograms of cyclohexane, propoxylated glycerin (C 15 h 32 o 7 , molecular weight 324) 750 kilograms, 550 kilograms of acrylic acid, 9 kilograms of hydroxyanisole, 10 kilograms of hypophosphorous acid, 55 kilograms of p-toluenesulfonic acid; Stirring is started, and compressed air is continuously fed into the kettle by a distributor at the bottom of the kettle, and the temperature is raised to 80 Start reflux dehydration at -86°C, esterification reaction for 10-12 hours, kettle temperature 88-92°C, when the reflux dehydration until no water comes out, the acid value is 30-35mgKOH / g, the reaction is over, cool to room temperature; add 32 Kg of caustic soda and 75 kg of water, stirring for 30 minutes; adding 6.5 kg of magnesium polysilicate, stirring and adsorbing for 30 minutes; After the solvent is separated, the water can be used directly in the next neutralization without any treatment, and the solvent can be used directly in the ...
Embodiment 3
[0065] In the 3000L reactor, drop into 406 kilograms of methylcyclohexanes, 696 kilograms of cyclohexanes, ethoxylated glycerin (C 9 h 20 o 6 , molecular weight 224) 495 kilograms, 541 kilograms of acrylic acid, 13.3 kilograms of p-hydroxyanisole, 11 kilograms of sodium hypophosphite, 110 kilograms of p-toluenesulfonic acid; Stirring is started, and compressed air is continuously introduced into the kettle through the distributor at the bottom of the kettle to heat up Start reflux dehydration at 80-85°C, esterification reaction for 9-10 hours, kettle temperature 85-100°C, when reflux dehydration until anhydrous, detect acid value 25-30mgKOH / g, the reaction is over, cool to 40°C; Add 68 kg of caustic soda and 205 kg of water, stir for 30 minutes; add 22.7 kg of magnesium polysilicate, stir and absorb for 30 minutes; After the water and the solvent are separated, the water can be used directly in the next neutralization without any treatment, and the solvent can be used direct...
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