Cleaning production method for di-trimethylolpropane tetra-acrylic ester or pentaerythritol tetra-acrylic ester

Abstract

The invention belongs to the field of photo-curing material, and relates to a cleaning production method for di-trimethylolpropane tetra-acrylic ester or pentaerythritol tetra-acrylic ester. The method specifically comprises the following steps of: (1) dehydrating di-trimethylolpropane / pentaerythritol, crylic acid, catalyst, solvent, polymerization inhibitor and antioxygen by means of esterification and backflow; (2) adding sheet alkali and a small quantity of water to neutralize; (3) adding magnesium polysilicate adsorbent to adsorb and neutralize the generated salt; (4) dehydrating in a pressure reducing way, and removing solvent; (5) carrying out filter pressing, filtering out the magnesium polysilicate and salt adsorbed by the magnesium polysilicate; (6) adding alkaline calcium bentonite and calcium oxide, to remove color, trace moisture and trace acid; (7) carrying out filter pressing; and (8) detecting the indexes of a product. The invention belongs to a cleaning production method for the di-trimethylolpropane tetra-acrylic ester or the pentaerythritol tetra-acrylic ester, which is good in economic benefit and environmental benefit, so that the problem of organic waste water pollution when the di-trimethylolpropane tetra-acrylic ester or the pentaerythritol tetra-acrylic ester is produced can be basically solved.

Description

technical field

[0001] The invention belongs to the field of light-curing materials, and relates to a clean production method of ditrimethylolpropane tetraacrylate or pentaerythritol tetraacrylate. 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. Di-trimethylolpropane tetraacrylate (Di-TMPTA) or pentaerythritol tetraacrylate (PETA) is a new type of photocurable material - a four-functional photocurable monomer with low irritation, fast curing speed, and high cross-linking properties. Excellent properties such as joint density, high hardness, wear ...

Examples

Embodiment 1

[0039]Put 500 kg of toluene, 290 kg of cyclohexane, 452.57 kg of ditrimethylolpropane, 547.43 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; 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 25-45mgKOH / 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 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 directly in the next ester...

Embodiment 2

[0041] Put 585 kilograms of cyclohexane into the 3000L reactor, 441.52 kilograms of pentaerythritol, 1028.48 kilograms of acrylic acid, 6 kilograms of p-hydroxyanisole, 3 kilograms of sodium hypophosphite, and 30 kilograms of methanesulfonic acid; Continuously feed compressed air inside, raise the temperature to 80-85°C and start reflux dehydration. The esterification reaction takes 10-12 hours. 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; 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, press filter; add 60 One kilogram of alkaline calcium-based bentonite and 25 kilograms of calcium oxide were stirred for 30 minutes, and ...

Embodiment 3

[0043] 162 kilograms of methylcyclopentane, 198 kilograms of toluene, 775 kilograms of ditrimethylolpropane, 960 kilograms of acrylic acid, 7.2 kilograms of p-hydroxyanisole, 1.8 kilograms of hypophosphorous acid, and 25.6 kilograms of methanesulfonic acid were put into the 3000L reactor; Turn on the 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 until no water comes out , the detection acid value is 25-45mgKOH / 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 absorb for 30 minutes; Above 0.098MPa, water and solvent are distilled under reduced pressure at 50-95°C. After the recovered water and solvent are separated, the water can be u...

technical field

[0001] The invention belongs to the field of light-curing materials, and relates to a clean production method of ditrimethylolpropane tetraacrylate or pentaerythritol tetraacrylate. 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. Di-trimethylolpropane tetraacrylate (Di-TMPTA) or pentaerythritol tetraacrylate (PETA) is a new type of photocurable material - a four-functional photocurable monomer with low irritation, fast curing speed, and high cross-linking properties. Excellent properties such as joint density, high hardness, wear ...

Examples

Embodiment 1

[0039]Put 500 kg of toluene, 290 kg of cyclohexane, 452.57 kg of ditrimethylolpropane, 547.43 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; 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 25-45mgKOH / 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 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 directly in the next ester...

Embodiment 2

[0041] Put 585 kilograms of cyclohexane into the 3000L reactor, 441.52 kilograms of pentaerythritol, 1028.48 kilograms of acrylic acid, 6 kilograms of p-hydroxyanisole, 3 kilograms of sodium hypophosphite, and 30 kilograms of methanesulfonic acid; Continuously feed compressed air inside, raise the temperature to 80-85°C and start reflux dehydration. The esterification reaction takes 10-12 hours. 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; 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, press filter; add 60 One kilogram of alkaline calcium-based bentonite and 25 kilograms of calcium oxide were stirred for 30 minutes, and ...

Embodiment 3

[0043] 162 kilograms of methylcyclopentane, 198 kilograms of toluene, 775 kilograms of ditrimethylolpropane, 960 kilograms of acrylic acid, 7.2 kilograms of p-hydroxyanisole, 1.8 kilograms of hypophosphorous acid, and 25.6 kilograms of methanesulfonic acid were put into the 3000L reactor; Turn on the 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 until no water comes out , the detection acid value is 25-45mgKOH / 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 absorb for 30 minutes; Above 0.098MPa, water and solvent are distilled under reduced pressure at 50-95°C. After the recovered water and solvent are separated, the water can be u...

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