Clean production method of bifunctional acrylic ester reactive diluent

A reactive diluent and clean production technology, applied in the fields of radiation-cured coatings, inks, and adhesives, can solve the problems of many post-processing steps and long operation time, and achieve the effect of no material loss and good economic benefits

Active Publication Date: 2016-05-11
HUNAN JINHAI SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alkali neutralization also lost the catalyst and excess acrylic acid; the filter residues such as magnesium polysilicate, alkaline calcium-based bentonite,...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 600KG of toluene, 536KG of dipropylene glycol, 605KG of acrylic acid, 9KG of p-hydroxyanisole, 15KG of p-toluenesulfonic acid, and 4KG of hypophosphorous acid aqueous solution into a 2-ton stainless steel reactor; , heat up 100-110 degrees to reflux and separate water, when basically no water comes out, take a sample to detect that the acid value is less than 30mgKOH / g, cool down to 50 degrees; add the esterification water generated in step 1, stir and stand for stratification, and separate The water layer containing catalyst and part of excess acid is used as the raw material for the next esterification reaction; the reaction solvent is vacuum distilled, and the acid value is detected after the distillation; add triphenylphosphine 5KG, glycidol 17.4KG, 100- React at 110°C for 5 hours, take a sample for detection, stop when the acid value is less than 1mgKOH / g, cool down and discharge to obtain dipropylene glycol diacrylate. Tested product indicators: clear and tran...

Embodiment 2

[0023] Add 600KG of cyclohexane, 600KG of polyethylene glycol (molecular weight 200), 453.6KG of acrylic acid, 6.8KG of p-hydroxyanisole, 12.5KG of p-toluenesulfonic acid, and 4KG of hypophosphorous acid aqueous solution into a 2-ton stainless steel reactor; Stir, use an air compressor to feed air into the bottom of the kettle, heat up 100-110 degrees to reflux and divide water, when basically no water comes out, take a sample to detect that the acid value is less than 30mgKOH / g, cool down to 50 degrees; add the esterification in step 1 Generate water, stir and stand for stratification, separate the water layer containing the catalyst and part of the excess acid, this water layer is used as the raw material for the next esterification reaction; the reaction solvent is vacuum distilled, and the acid value is detected after the distillation; add triphenylphosphine 9KG, 45KG of glycidyl methacrylate, react at 100-110°C for 5 hours, take samples for testing, stop when the acid valu...

Embodiment 3

[0025] Add 600KG of toluene, 590KG of 1,6-hexanediol, 756KG of acrylic acid, 11.4KG of p-hydroxyanisole, 16KG of p-toluenesulfonic acid, and 5KG of hypophosphorous acid aqueous solution into a 2-ton stainless steel reactor; Air is fed into the air compressor, and the temperature rises to 100-110 degrees to reflux and divide the water. When there is basically no water, the acid value is less than 30mgKOH / g by sampling, and the temperature is cooled to 50 degrees; add the esterification water in step 1, and stir Set the layers, separate the water layer containing the catalyst and part of the excess acid, this water layer is used as the raw material for the next esterification reaction; the reaction solvent is vacuum distilled, and the acid value is detected after the distillation; add 7KG of triphenylphosphine, epoxy chlorine Propane 25KG, react at 100-110°C for 5 hours, take samples for inspection, stop when the acid value is less than 1mgKOH / g, cool down and discharge to obtain...

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PUM

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Abstract

The invention discloses a clean production method of a bifunctional acrylic ester reactive diluent. The clean production method is characterized by comprising the following specific steps: (1) performing esterification reaction: adding dihydric alcohol and acrylic acid at a molar ratio of dihydric alcohol to acrylic acid being 1:2 to 2.2 into a reactor, further adding an aqueous solvent, a catalyst, a polymerization inhibitor and an antioxidant subtractive agent, inletting air or a mixed gas of nitrogen and air from the bottom of the reactor, heating to 80-120 DEG C for refluxing, esterifying and separating water, detecting the acid value when substantially no water is separated out, and after a qualified standard is reached, cooling to 50 DEG C; (2) adding esterified water in the step 1, stirring and leaving to stand for layering, separating out an aqueous layer, as a raw material for next esterification reaction, containing the catalyst and a part of excess acid; (3) distilling the reaction solvent in vacuum, and detecting the acid value after finish of distillation; (4) removing the remaining acid through epoxide ring-opening reaction; (5) detecting product indexes. In the clean production method, neither the conventional processing method, comprising neutralizing and washing, nor the processing method, comprising neutralizing, adsorbing by using an adsorbent and filtering, is used. By the clean production method, both organic wastewater and solid chemical waste residues are not generated, so that the clean production method can completely meet clean production requirements in the industry; in the production process, no material loss is caused, and all processes are completed in the same reactor, so that the economic benefits are high.

Description

technical field [0001] The invention belongs to the field of radiation curing paint, printing ink, adhesive and the like. The invention relates to a clean production method of a difunctional acrylate reactive diluent. Background technique [0002] Radiation curing is an advanced material surface treatment technology that uses ultraviolet light or electron beams to initiate rapid polymerization and crosslinking of chemically active liquid materials, and instantly solidifies them into solid materials. It has the characteristics of quick drying, energy saving and environmental friendliness. In recent years, with the enhancement of people's awareness of energy saving and environmental protection, the performance of radiation curing products has been continuously enhanced, the application fields have been continuously expanded, the output has increased rapidly, and the momentum has developed rapidly. Reactive diluent is a small organic molecule containing polymerizable function...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08C07C67/48C07C67/60
CPCC07C67/08C07C67/48C07C67/60C07C69/54
Inventor 刘立新唐慧敏黄利勇
Owner HUNAN JINHAI SCI & TECH
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