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

Active Publication Date: 2012-06-20
JIANGSU LITIAN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] ①Most of the catalysts used are sulfuric acid, p-toluenesulfonic acid, methanesulfonic acid and other catalysts, which are usually removed by neutralization, water washing, and layering methods, which will produce a large amount of industrial organic wastewater and pollute the water environment;
[0005] ② During the reaction process, the excess (8%-15%) acrylic acid is completely washed away by water, and is

Method used

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  • Clean production method of alkoxylation glycerol triacrylate
  • Clean production method of alkoxylation glycerol triacrylate
  • Clean production method of alkoxylation glycerol triacrylate

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention belongs to the field of photocuring materials and relates to a clean production method of alkoxylation glycerol triacrylate. The method comprises the following steps that: (1) ethoxylation glycerol/propoxylation glycerol, acrylic acid, catalysts, solvents, polymerization inhibitors and antioxidants are subjected to esterification backflow dehydration; (2) soda flakes and a small quantity of water are added for neutralization; (3) magnesium polysilicate absorbing agents are added for absorbing salt generated during the neutralization; (4) the pressure reduction dehydration is carried out, and solvents are removed; (5) press filtering is carried out, and the magnesium polysilicate and the salt absorbed by the magnesium polysilicate are filtered away; (6) alkaline calcium bentonite and calcium bentonite are added, and decoloration, trace moisture removal and trace acid removal are carried out; (7) press filtering is carried out; and (8) product index detection is carried out. The method belongs to the high-yield clean production method of the ethoxylation glycerol triacrylate and propoxylation glycerol triacrylate and has the advantages that economic benefits and environment benefits are realized, and the problem of organic waste water pollution in the production process of the ethoxylation glycerol triacrylate and the propoxylation glycerol triacrylate is fundamentally solved.

Description

technical field [0001] The invention belongs to the field of light-curing materials, and relates to a clean production method of alkoxylated glycerin triacrylate. Background technique [0002] With the rapid development of science and technology and the strict restrictions on solvents in environmental protection regulations, more and more people pay attention to photocurable polymer materials. Light-curing materials have excellent properties such as fast curing, low energy consumption, less pollution, and high efficiency, so they are widely used in coatings, printing, and electronics industries, and have developed rapidly in recent years. Ethoxylated glycerin triacrylate and propoxylated glycerin triacrylate are a new type of light-curing material-multifunctional light-curing monomer with low viscosity, low stimulation, fast curing speed, strong dilution and high transparency It is widely used in light-curable inks, coatings, adhesives and other fields, and is widely used i...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08C07C67/56C07C67/48
Inventor 胡剑飞张本田张丽丽张兵
Owner JIANGSU LITIAN TECH
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