Pollution-free production method of lauryl alcohol acrylate, hexadecanol acrylate or stearyl alcohol acrylate

Abstract

The invention belongs to the field of photo-curing materials, and relates to a pollution-free production method of lauryl alcohol acrylate, hexadecanol acrylate or stearyl alcohol acrylate. The production method comprises the specific steps as follows: (1) carrying out esterification, refluxing and dehydration on lauryl alcohol / hexadecanol / stearyl alcohol, acrylic acid, a catalyst, a solvent, a polymerization inhibitor and an antioxidant; (2) adding flake caustic soda and a small amount of water for neutralizing; (3) adding magnesium silicate adsorbent to adsorb salt generated by neutralizing; (4) decompressing to dehydrate and desolventize; (5) carrying out filter pressing to filter out magnesium silicate and the adsorbed salt; (6) adding alkaline Ca-bentonite and calcium oxide for decolouring, and removing trace water and acid; (7) carrying out filter pressing; and (8) detecting the product index. The invention provides the pollution-free production method of lauryl alcohol acrylate, hexadecanol acrylate or stearyl alcohol acrylate, which has high yield as well as economic and environmental benefits, and fundamentally solves the problem of organic wastewater pollution in the production process of lauryl alcohol acrylate, hexadecanol acrylate or stearyl alcohol acrylate.

Description

technical field

[0001] The invention belongs to the field of light-curing materials, and relates to a clean production method of lauryl alcohol acrylate, palmityl alcohol acrylate or stearyl alcohol 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. Lauryl alcohol acrylate (LA), palmityl acrylate (HA) or stearyl acrylate (SA) is a new type of photocurable material - monofunctional photocurable monomer with low viscosity, low stimulation, low Polarity, strong dilution, good flexibility, high transparency and other excellent properties, are ...

Examples

Embodiment 1

[0041]In the 3000L reactor, drop into 500 kilograms of toluene, 290 kilograms of cyclohexane, 711 kilograms of lauryl alcohol (molecular weight 186), 289 kilograms of acrylic acid, 8 kilograms of p-hydroxyanisole, 4 kilograms of hypophosphorous acid, 55 kilograms of p-toluenesulfonic acid; 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 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 trea...

Embodiment 2

[0043] In the 3000L reactor, drop 585 kilograms of cyclohexane, 1108 kilograms of palmitic alcohol (molecular weight 242.5), 362 kilograms of acrylic acid, 6 kilograms of p-hydroxyanisole, 3 kilograms of sodium hypophosphite, 30 kilograms of methanesulfonic acid; The bottom distributor 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 detected to be 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 dire...

Embodiment 3

[0045] 162 kg of methylcyclopentane, 198 kg of toluene, 1345 kg of stearyl alcohol (molecular weight 270.5), 390 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 ; Turn on 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 anhydrous When the acid value is 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 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 used directly in the next neutralization with...

technical field

[0001] The invention belongs to the field of light-curing materials, and relates to a clean production method of lauryl alcohol acrylate, palmityl alcohol acrylate or stearyl alcohol 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. Lauryl alcohol acrylate (LA), palmityl acrylate (HA) or stearyl acrylate (SA) is a new type of photocurable material - monofunctional photocurable monomer with low viscosity, low stimulation, low Polarity, strong dilution, good flexibility, high transparency and other excellent properties, are ...

Examples

Embodiment 1

[0041]In the 3000L reactor, drop into 500 kilograms of toluene, 290 kilograms of cyclohexane, 711 kilograms of lauryl alcohol (molecular weight 186), 289 kilograms of acrylic acid, 8 kilograms of p-hydroxyanisole, 4 kilograms of hypophosphorous acid, 55 kilograms of p-toluenesulfonic acid; 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 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 trea...

Embodiment 2

[0043] In the 3000L reactor, drop 585 kilograms of cyclohexane, 1108 kilograms of palmitic alcohol (molecular weight 242.5), 362 kilograms of acrylic acid, 6 kilograms of p-hydroxyanisole, 3 kilograms of sodium hypophosphite, 30 kilograms of methanesulfonic acid; The bottom distributor 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 detected to be 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 dire...

Embodiment 3

[0045] 162 kg of methylcyclopentane, 198 kg of toluene, 1345 kg of stearyl alcohol (molecular weight 270.5), 390 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 ; Turn on 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 anhydrous When the acid value is 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 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 used directly in the next neutralization with...

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