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Method for synthesizing (methyl) acrylate glyceride through catalysis of calcium glyceroxide

A technology of glycerol acrylate and alkyl acrylate, which is applied in chemical instruments and methods, catalytic reactions, catalysts for physical/chemical processes, etc., can solve the problem of low activity selectivity of basic catalysts, difficult separation and purification of products, and poisoning and deactivation of dosage. and other problems, to achieve the effect of stable and easy separation of products, short process flow, and not easy to polymerize

Inactive Publication Date: 2016-10-12
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The direct esterification method uses a strong acid such as concentrated sulfuric acid as a catalyst for the direct esterification of alkyds. The strong acid catalyst not only causes many side reactions, difficulties in product separation and purification, and high requirements for equipment, but also leads to the discharge of a large amount of waste water, causing environmental pollution; the acid chloride method is The acid is first chlorinated into acid chloride and then esterified with alcohol, but the chlorination process will increase the reaction steps; the synthesis of (meth)acrylate can be carried out under the action of a catalyst, using alkyl (meth)acrylate and alcohol as raw materials Produced by transesterification, the pure product can be obtained after rectification
[0006] Catalysts for synthesizing (meth)acrylic esters by transesterification can be p-toluenesulfonic acid, calcium oxide and titanate, etc., but acidic catalysts will corrode equipment, and basic catalysts have low activity selectivity, and the amount of neutral organometallic catalysts should be considered Problems and inactivation problems

Method used

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  • Method for synthesizing (methyl) acrylate glyceride through catalysis of calcium glyceroxide

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Experimental program
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Effect test

Embodiment 1

[0031] The preparation of embodiment 1 glyceryl acrylate

[0032] In the there-necked flask equipped with electromagnetic stirring, thermometer, rectifying column, receiving tube, and receiving bottle, add 77.5g (0.9mol) methyl acrylate, 9.2g (0.1mol) of glycerol and 0.5g calcium glycerol, heat and reflux and stir, Make the methanol produced by the reaction continue to be azeotropically distilled from the upper end of the rectifying column, and react until no methanol is distilled off, then filter the reaction solution, reclaim the catalyst, distill off the raw material methyl acrylate, and obtain 28.3 g of the product, in which glyceryl diacrylate and The glycerol triacrylate content was 22.5% and 42.3%, respectively.

Embodiment 2

[0033] The preparation of embodiment 2 glyceryl acrylate

[0034] Add a magnetic stirrer bar in a 250mL four-necked flask equipped with an air inlet, a copper mesh packing rectification column and a temperature measuring device, add 9.2g (0.1mol) glycerol, 0.50g (0.5% glycerol mass) and 0.05g glycerol calcium For p-hydroxyanisole, raise the temperature to the reaction liquid at 60°C, put 77.5g of methyl acrylate into the constant pressure dropping funnel and add it dropwise within 2-3 hours, let the air in and raise the temperature until the reaction liquid refluxes, and take samples regularly during the reaction The end point of the reaction was analyzed by gas chromatography. After the reaction reaches the end point, add 0.1g of neutral activated carbon and reflux at about 50°C for 0.5h-1h. After the end, the reaction solution is filtered under reduced pressure, and the filtrate is rotary evaporated to obtain 31.4g of the product. The contents of glyceryl diacrylate and glyc...

Embodiment 3

[0035] The preparation of embodiment 3 (meth) glyceryl acrylate

[0036] In a three-necked flask equipped with electromagnetic stirring, a thermometer, a rectifying column, a receiving tube, and a receiving bottle, add 90.1 g (0.9 mol) of methyl acrylate, 9.2 g (0.1 mol) of glycerol and 0.5 g of calcium glycerol, and heat to reflux and stir. Make the methanol produced by the reaction continue to be azeotropically distilled from the rectifying column upper end, react until no methanol is distilled off, filter the reaction solution, reclaim the catalyst, distill the raw material methyl acrylate to obtain 29.6 g of product glyceryl acrylate, di(methyl acrylate) Glyceryl) acrylate and glyceryl tri(meth)acrylate content were 37.5% and 40.4%, respectively.

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Abstract

The invention discloses a method for synthesizing glycerol (meth)acrylate with calcium glycerol catalysis, which belongs to the field of fine chemical industry. Reaction-distillation process is adopted, using a modified rectification column with copper wire mesh packing, adding alkyl (meth)acrylate, glycerin, polymerization inhibitor and catalyst, under stirring conditions, feeding air and raising the temperature to the reflux of the reaction solution, The temperature is 60-140°C. After the reaction, cool the reaction solution to 50°C, add activated carbon, and continue to heat and stir for 0.5h-1h. After the end, the reaction solution is filtered under reduced pressure, and the filtrate is rotary evaporated under reduced pressure to remove excess raw material ester to obtain (meth)acrylic acid Glyceride reactive diluent products. The invention overcomes many shortcomings of existing transesterification catalysts, and has high yield, simple post-treatment, and easy availability.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and relates to the preparation of glycerol (meth)acrylate by a solid base catalyst catalyzing glycerin and (meth)acrylate through a transesterification synthesis method. Background technique [0002] Glyceryl (meth)acrylate has the characteristics of high double bond content, low volatility, low toxicity, high crosslinking density, and fast curing speed. The cured film formed by it is wear-resistant and solvent-resistant. Functional acrylate reactive diluent, which has wide application prospects in many fields such as light-curing coatings, inks and polymer modification and crosslinking agents [0003] [0004] Formula 1 (meth)acrylic acid glycerides reactive diluent chemical structure [0005] According to existing literature reports, the synthesis of (meth)acrylate reactive diluents can be through direct esterification, acid chloride and transesterification. The direct esterification ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C69/54B01J31/02
CPCC07C67/03B01J31/0212B01J2231/49
Inventor 冯筱晴李贝贝宋国强
Owner CHANGZHOU UNIV
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