Cleaning production method of 2-(Ethoxyethoxy) ethyl acrylate (EOEOEA) or phenoxyethyl acrylate (PHEA)

A technology of ethoxy ethoxy ethyl acrylate and ethoxy phenyl acrylate, which is applied in the field of light-curing materials, can solve the problems of high manufacturing costs, water environmental pollution, and high treatment costs, and achieve excellent environmental benefits, The effect of high yield

Active Publication Date: 2012-08-15
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 usually removed by neutralization, water washing, and layering methods, which will produce a large amount of industrial organic wastewater with high COD, which is difficult to treat and has high treatment costs. The problem makes the product more expensive to manufacture;
[0006] ③While neutralizing and washing with water, some acrylate products will be taken away, which will reduce the yield and increase the cost

Method used

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  • Cleaning production method of 2-(Ethoxyethoxy) ethyl acrylate (EOEOEA) or phenoxyethyl acrylate (PHEA)
  • Cleaning production method of 2-(Ethoxyethoxy) ethyl acrylate (EOEOEA) or phenoxyethyl acrylate (PHEA)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]Put 500 kg of toluene, 290 kg of cyclohexane, 646 kg of ethylene glycol phenyl ether, 354 kg of acrylic acid, 8 kg of p-hydroxyanisole, 4 kg of hypophosphorous acid, and 55 kg of p-toluenesulfonic acid into the 3000L reactor; start stirring , continuously feed compressed air into the kettle through the distributor at the bottom of the kettle, raise the temperature to 85-95°C and start reflux dehydration, the esterification reaction is 9-10 hours, the kettle temperature is 95-105°C, when the reflux dehydration reaches no water, the detection The acid value is 10-25mgKOH / g. After the reaction is over, cool to 40°C; add 25 kg of caustic soda and 60 kg of water, and stir for 30 minutes; add 6 kg of magnesium polysilicate, stir and absorb for 30 minutes; Above, water and solvent are distilled under reduced pressure at 50-95°C. After the recovered water and solvent are separated, the water can be used directly in the next neutralization without any treatment, and the solvent ca...

Embodiment 2

[0041] Put 585 kg of cyclohexane, 923.92 kg of diethylene glycol ether, 546.08 kg of acrylic acid, 6 kg of p-hydroxyanisole, 3 kg of sodium hypophosphite, and 30 kg of methanesulfonic acid into the 3000L reactor; The sparger continuously feeds compressed air into the kettle, raises the temperature to 80-85°C and starts reflux dehydration, the esterification reaction lasts for 10-12 hours, the kettle temperature is 85-92°C, when the reflux dehydration reaches anhydrous, the acid value is 10~ 25mgKOH / g, after the reaction is over, cool to 40°C; add 32 kg of caustic soda and 75 kg of water, and stir for 30 minutes; add 6.5 kg of magnesium polysilicate, stir and absorb for 30 minutes; Distill water and solvent under reduced pressure at 95°C; after the recovered water and solvent are separated, the water can be used directly in the next neutralization without any treatment, and the solvent can be used directly in the next esterification reaction; after the distillation is completed,...

Embodiment 3

[0043] 162 kg of methylcyclopentane, 198 kg of toluene, 1109.8 kg of ethylene glycol phenyl ether, 625.37 kg of acrylic acid, 7.2 kg of p-hydroxyanisole, 1.8 kg of hypophosphorous acid, and 25.6 kg of methanesulfonic acid were put into the 3000L reactor; Stir, continuously feed compressed air into the kettle through the distributor at the bottom of the kettle, heat up to 85-95°C and start reflux dehydration, esterification reaction for 9-10 hours, kettle temperature 95-105°C, when reflux dehydration until no water comes out, Detect the acid value of 10-25mgKOH / g, after the reaction is over, cool to 40°C; add 43 kg of caustic soda and 108 kg of water, and stir for 30 minutes; add 17.3 kg of magnesium polysilicate, stir and adsorb for 30 minutes; Above MPa, water and solvent are distilled under reduced pressure at 50-95°C. After the recovered water and solvent are separated, the water can be used directly in the next neutralization without any treatment, and the solvent can be used ...

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Abstract

The invention belongs to the field of photocuring materials and relates to a cleaning production method of 2-(Ethoxyethoxy) ethyl acrylate (EOEOEA) or phenoxyethyl acrylate (PHEA). The method comprises the following steps: (1) carrying out esterification, backflow and dehydration on diethylene Glycol monoethylether or ethylene glycol phenyl ether, acrylic acid, a catalyst, a solvent, a polymerization inhibitor and an antioxidant; (2) adding caustic soda flakes and little water for neutralization; (3) adding a polymagnesium silicate adsorbent for adsorbing and neutralizing the generated salt; (4) reducing pressure for dehydration and removing the solvent; (5) carrying out filter pressing so as to filter polymagnesium silicate and the salt adsorbed by polymagnesium silicate; (6) adding alkaline Ca-based bentonite and calcium oxide for decoloration, micro water removal and trace acid removal; (7) carrying out filter pressing; and (8) detecting product indexes. The cleaning production method disclosed by the invention has high yield and social and environmental benefits, thus thoroughly solving the organic waste water pollution problem during the production process of EOEOEA or PHEA.

Description

technical field [0001] The invention belongs to the field of light-curing materials and relates to a clean production method of ethoxyethoxyethyl acrylate or ethoxyphenyl acrylate. 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. Ethoxy ethoxy ethyl acrylate (EOEOEA) and ethoxy phenyl acrylate (PHEA) are a new class of photocurable materials——monofunctional photocurable monomers with low viscosity, low irritation, and curable High speed, strong dilution, high transparency and other excellent properties, widely used in photo-curable inks, coatings,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/08C07C67/56
Inventor 胡剑飞张丽丽马怀祥王保俊
Owner JIANGSU LITIAN TECH
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