Clean production method of dipropylene glycol diacrylate (DPGDA) or tripropylene glycol diacrylate (TPGDA)

Abstract

The invention which belongs to the light-cured material field relates to a clean production method of DPGDA or TPGDA. The method concretely comprises the following steps: 1, carrying out esterification reflux dehydration on dipropylene glycol / tripropylene glycol, acrylic acid, a catalyst, a solvent, a polymerization inhibitor and an antioxidant; 2, adding sodium hydroxide and a small amount of water to neutralize; 3, adding a magnesium polysilicate adsorbent to adsorb a salt generated through neutralization; 4, carrying out reduced pressure dehydration and desolventization; 5, press-filtering to filter out magnesium polysilicate and the salt absorbed thereby; 6, adding alkaline calcium bentonit and calcium oxide to decolor, remove trace water and remove trace acids; 7, press-filtering; and 8, carrying out product index detection. The clean production method of the DPGDA or the TPGDA of the invention, which has the advantages of high yield, economic benefit possessing and environmental benefit possessing, fundamentally solves an organic wastewater pollution problem in the production process of the DPGDA or the TPGDA.

Description

technical field

[0001] The invention belongs to the field of light-curing materials, and relates to a clean production method of dipropylene glycol diacrylate or tripropylene glycol diacrylate. 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. Dipropylene glycol diacrylate (DPGDA) and tripropylene glycol diacrylate (TPGDA) are a new class of light-curing materials—multifunctional light-curing monomers with low viscosity, low irritation, fast curing speed, and strong dilution , high transparency and other excellent properties, widely used in light-c...

Examples

Embodiment 1

[0061] In the 3000L reactor, drop into 500 kilograms of toluene, 290 kilograms of cyclohexane, 545 kilograms of tripropylene glycol, 455 kilograms of acrylic acid, 8 kilograms of p-hydroxyanisole, 4 kilograms of hypophosphorous acid, 55 kilograms of p-toluenesulfonic acid; Open 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 temperature of the kettle is 95-105°C, when the reflux dehydration until no water comes out, the acid is detected Value 25~30mgKOH / g, after the reaction is over, cool to 40°C; add 25 kg of caustic soda and 60 kg of water, stir for 30 minutes; add 6 kg of magnesium polysilicate, stir and absorb for 30 minutes; , 50-95°C distilled water and solvent under reduced pressure. After the recovered water and solvent are separated, the water can be used directly in the next neutralization without...

Embodiment 2

[0063] In the 3000L reactor, drop 585 kilograms of cyclohexane, 670 kilograms of dipropylene glycol, 800 kilograms of acrylic acid, 6 kilograms of p-hydroxyanisole, 3 kilograms of sodium hypophosphite, and 30 kilograms of methanesulfonic acid; Continuously feed compressed air into the kettle, raise the temperature to 80-85°C and start reflux dehydration. The esterification reaction takes 10-12 hours. The kettle temperature is 85-92°C. When the reflux dehydration reaches anhydrous, the acid value is 20-35mgKOH / 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; Water and solvent are distilled out under pressure; 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 comple...

Embodiment 3

[0065] Put 162 kilograms of methylcyclopentane, 198 kilograms of toluene, 981 kilograms of tripropylene glycol, 754.2 kilograms of acrylic acid, 7.2 kilograms of p-hydroxyanisole, 1.8 kilograms of hypophosphorous acid, and 25.6 kilograms of methanesulfonic acid into the 3000L reactor; , 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 25-30mgKOH / 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, 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 neutralizatio...

technical field

[0001] The invention belongs to the field of light-curing materials, and relates to a clean production method of dipropylene glycol diacrylate or tripropylene glycol diacrylate. 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. Dipropylene glycol diacrylate (DPGDA) and tripropylene glycol diacrylate (TPGDA) are a new class of light-curing materials—multifunctional light-curing monomers with low viscosity, low irritation, fast curing speed, and strong dilution , high transparency and other excellent properties, widely used in light-c...

Examples

Embodiment 1

[0061] In the 3000L reactor, drop into 500 kilograms of toluene, 290 kilograms of cyclohexane, 545 kilograms of tripropylene glycol, 455 kilograms of acrylic acid, 8 kilograms of p-hydroxyanisole, 4 kilograms of hypophosphorous acid, 55 kilograms of p-toluenesulfonic acid; Open 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 temperature of the kettle is 95-105°C, when the reflux dehydration until no water comes out, the acid is detected Value 25~30mgKOH / g, after the reaction is over, cool to 40°C; add 25 kg of caustic soda and 60 kg of water, stir for 30 minutes; add 6 kg of magnesium polysilicate, stir and absorb for 30 minutes; , 50-95°C distilled water and solvent under reduced pressure. After the recovered water and solvent are separated, the water can be used directly in the next neutralization without...

Embodiment 2

[0063] In the 3000L reactor, drop 585 kilograms of cyclohexane, 670 kilograms of dipropylene glycol, 800 kilograms of acrylic acid, 6 kilograms of p-hydroxyanisole, 3 kilograms of sodium hypophosphite, and 30 kilograms of methanesulfonic acid; Continuously feed compressed air into the kettle, raise the temperature to 80-85°C and start reflux dehydration. The esterification reaction takes 10-12 hours. The kettle temperature is 85-92°C. When the reflux dehydration reaches anhydrous, the acid value is 20-35mgKOH / 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; Water and solvent are distilled out under pressure; 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 comple...

Embodiment 3

[0065] Put 162 kilograms of methylcyclopentane, 198 kilograms of toluene, 981 kilograms of tripropylene glycol, 754.2 kilograms of acrylic acid, 7.2 kilograms of p-hydroxyanisole, 1.8 kilograms of hypophosphorous acid, and 25.6 kilograms of methanesulfonic acid into the 3000L reactor; , 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 25-30mgKOH / 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, 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 neutralizatio...

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