Clean production method of dipentaerythritol hexaacrylate

Abstract

The invention belongs to the field of a photo-curing material and relates to a clean production method of dipentaerythritol hexaacrylate. The method comprises the following concrete steps: (1) carrying out esterification and reflux dehydration on dipentaerythritol, acrylic acid, a catalyst, a solvent, a polymerization inhibitor and an antioxidant; (2) adding caustic soda flakes and a little amount of water to neutralize; (3) adding a magnesium polysilicate adsorbent to absorb salt generated by neutralization; (4) dewatering and removing the solvent at reduced pressure; (5) carrying out filter pressing to filter out magnesium polysilicate and absorbed salt thereof; (6) adding alkaline Ca-bentonite and calcium oxide, destaining, and removing trace water and trace acid; (7) carrying out filter pressing; and (8) detecting a product index. The clean production method disclosed by the invention is the clean production method of dipentaerythritol hexaacrylate, with high yield, economic benefit and environmental benefit, so the pollution problem of organic waste water in the production process of dipentaerythritol hexaacrylate is fundamentally solved.

Description

technical field

[0001] The invention belongs to the field of photocurable materials and relates to a clean production method of dipentaerythritol hexaacrylate. 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. Dipentaerythritol hexaacrylate (DPHA) is a new type of light-curing material - hexafunctional light-curing monomer, with low irritation, fast curing speed, high cross-linking density, high hardness, wear resistance, scratch resistance, high transparency It is widely used in light-curable inks, coatings, adhesives and other fields, and is wide...

Examples

Embodiment 1

[0037] Put 500 kg of toluene, 290 kg of cyclohexane, 348.3 kg of dipentaerythritol, 651.7 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; The bottom distributor continuously feeds compressed air into the kettle, raises the temperature to 85-95°C and starts reflux dehydration, the esterification reaction lasts for 9-10 hours, the kettle temperature is 95-105°C, when the reflux dehydration reaches anhydrous, the acid value is detected to be 30 ~60mgKOH / 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; Water and solvent are distilled 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 re...

Embodiment 2

[0039]162 kilograms of methylcyclopentane, 198 kilograms of toluene, 550 kilograms of dipentaerythritol, 1185 kilograms of acrylic acid, 7.2 kilograms of p-hydroxyanisole, 1.8 kilograms of hypophosphorous acid, and 25.6 kilograms of methanesulfonic acid were dropped into the 3000L reactor; The sparger at the bottom of the kettle continuously feeds compressed air into the kettle, raises the temperature to 85-95°C and starts reflux dehydration, the esterification reaction lasts for 9-10 hours, the kettle temperature is 95-105°C, and when the reflux dehydration reaches anhydrous, the acid value is detected 30~60mgKOH / g, after the reaction is over, cool to 40°C; add 43 kg of caustic soda and 108 kg of water, stir for 30 minutes; add 17.3 kg of magnesium polysilicate, stir and adsorb for 30 minutes; Distill water and solvent at 50-95°C under reduced pressure. After the recovered water and solvent are separated, the water can be used directly in the next neutralization without any tr...

Embodiment 3

[0041] Put 630 kg of cyclohexane, 570 kg of methylcyclohexane, 295.5 kg of dipentaerythritol, 603 kg of acrylic acid, 15 kg of p-hydroxyanisole, 15 kg of hypophosphorous acid, and 150 kg of benzenesulfonic 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 80-85°C and start reflux dehydration, the esterification reaction is 10-12 hours, the kettle temperature is 85-92°C, when the reflux dehydration reaches no water, the detection The acid value is 30-60 mgKOH / g, after the reaction is over, cool to 40°C; add 68 kg of caustic soda and 205 kg of water, and stir for 30 minutes; add 6.8 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 sol...

technical field

[0001] The invention belongs to the field of photocurable materials and relates to a clean production method of dipentaerythritol hexaacrylate. 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. Dipentaerythritol hexaacrylate (DPHA) is a new type of light-curing material - hexafunctional light-curing monomer, with low irritation, fast curing speed, high cross-linking density, high hardness, wear resistance, scratch resistance, high transparency It is widely used in light-curable inks, coatings, adhesives and other fields, and is wide...

Examples

Embodiment 1

[0037] Put 500 kg of toluene, 290 kg of cyclohexane, 348.3 kg of dipentaerythritol, 651.7 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; The bottom distributor continuously feeds compressed air into the kettle, raises the temperature to 85-95°C and starts reflux dehydration, the esterification reaction lasts for 9-10 hours, the kettle temperature is 95-105°C, when the reflux dehydration reaches anhydrous, the acid value is detected to be 30 ~60mgKOH / 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; Water and solvent are distilled 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 re...

Embodiment 2

[0039]162 kilograms of methylcyclopentane, 198 kilograms of toluene, 550 kilograms of dipentaerythritol, 1185 kilograms of acrylic acid, 7.2 kilograms of p-hydroxyanisole, 1.8 kilograms of hypophosphorous acid, and 25.6 kilograms of methanesulfonic acid were dropped into the 3000L reactor; The sparger at the bottom of the kettle continuously feeds compressed air into the kettle, raises the temperature to 85-95°C and starts reflux dehydration, the esterification reaction lasts for 9-10 hours, the kettle temperature is 95-105°C, and when the reflux dehydration reaches anhydrous, the acid value is detected 30~60mgKOH / g, after the reaction is over, cool to 40°C; add 43 kg of caustic soda and 108 kg of water, stir for 30 minutes; add 17.3 kg of magnesium polysilicate, stir and adsorb for 30 minutes; Distill water and solvent at 50-95°C under reduced pressure. After the recovered water and solvent are separated, the water can be used directly in the next neutralization without any tr...

Embodiment 3

[0041] Put 630 kg of cyclohexane, 570 kg of methylcyclohexane, 295.5 kg of dipentaerythritol, 603 kg of acrylic acid, 15 kg of p-hydroxyanisole, 15 kg of hypophosphorous acid, and 150 kg of benzenesulfonic 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 80-85°C and start reflux dehydration, the esterification reaction is 10-12 hours, the kettle temperature is 85-92°C, when the reflux dehydration reaches no water, the detection The acid value is 30-60 mgKOH / g, after the reaction is over, cool to 40°C; add 68 kg of caustic soda and 205 kg of water, and stir for 30 minutes; add 6.8 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 sol...

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