Method for preparing 1,4-butanediol diacrylate

A diacrylate and butanediol technology, which is applied in the field of preparation of 1,4-butanediol diacrylate, can solve the problems of high color, acidity and viscosity, poor activity and flexibility, by-products and waste water, etc. , to achieve low viscosity and shrinkage, good activity and flexibility, less by-products and waste water

Inactive Publication Date: 2009-06-24
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing production method is mainly alkyd direct esterification method, with excess acrylic acid, toluene or benzene are water-carrying solvent, and sulfuric acid is catalyzer and makes final product, but this preparation method has following deficiency: 1. by-product and waste water of generation More, more serious environmental pollution; 2. Poor activity and flexibility; 3. Large chroma, acidity and viscosity, and easy to turbid; 4. High shrinkage, low yield, poor quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of preparation method of 1,4-butanediol diacrylate, the step of its preparation method is:

[0027] (1). Put 350g of 1,4-butanediol, 600g of acrylic acid, 10g of p-toluenesulfonic acid and 400g of toluene into the reaction kettle, and add polymerization inhibitor hydroquinone 100ppm, p-hydroxyanisole 100ppm, phen Thiazine 50ppm, copper sulfate 300ppm, and decolorizing agent activated carbon 50ppm are added to the reaction system and mixed thoroughly to form a mixed solution;

[0028] (2). Open the steam valve of the reactor to heat slowly, control the heating speed to keep the steam pressure at 0.3Mpa, control the temperature at 70°C within 1h and maintain this temperature for 20 minutes to react;

[0029] (3). Continue to heat the mixture, wait for the temperature to rise to 80°C for 3 hours, then reflux for 5 hours, keep the temperature at 80°C, and the reaction ends;

[0030] (4). Adding a concentration of 10% soda ash aqueous solution and a concentration of ...

Embodiment 2

[0034] A kind of preparation method of 1,4-butanediol diacrylate, the step of its preparation method is:

[0035] (1). 400g of 1,4-butanediol, 650g of acrylic acid, 100g of p-toluenesulfonic acid and 600g of toluene are put into the reaction kettle, and 250ppm of polymerization inhibitor hydroquinone is added, and 500ppm of decolorizing agent activated carbon is added at the same time The reaction system is fully mixed and stirred to form a mixed solution;

[0036] (2). Open the steam valve of the reaction kettle to heat slowly, control the heating speed to keep the steam pressure at 0.5Mpa, control the temperature at 80°C within 1 hour and maintain this temperature for 40 minutes to react;

[0037] (3). Continue to heat the mixture, wait for the temperature to rise to 120°C for 4 hours, then reflux for 7 hours, control the temperature at 120°C, and the reaction ends;

[0038] (4). Adding a concentration of 10% soda ash aqueous solution and a concentration of 20% sodium chlor...

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PUM

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Abstract

The invention belongs to a method for preparing 1, 4-butanediol diacrylate ester, comprising the steps as follows: (1) 1, 4-butanediol, acrylic acid, catalyst, solvent and polymerization inhibitor are put into a reaction kettle to be fully mixed and stirred, so as to form a mixture; (2) a steam valve of the reaction kettle is opened to slowly heat the mixture, the temperature is controlled and maintained at 70-90 DEG C for a 20-40min reaction; (3) the mixture is continued to be heated to react for 3-4h, then reflow is carried out for 5-7h and then the reaction is finished; (4) soda water solution and sodium chloride water solution are added into the mixture and after washing the upper organic phase is extracted; (5) the upper organic phase is separated from the solvent; (6) then cooling and pressing are carried out to obtain the end product. The method is simple in process, produces few by-products or little waste water, has good activity and flexibility, low color intensity, acidity, viscosity and shrinking percentage, high yield coefficient and good quality.

Description

technical field [0001] The invention belongs to the field of fine chemicals, in particular to a preparation method of 1,4-butanediol diacrylate. Background technique [0002] 1,4 Butanediol Diacrylate (BDDA) is an acrylic functional monomer capable of rapid curing, weak skin irritation and good flexibility. Its molecular weight is 198 and its appearance is transparent liquid. It is mainly used in inks, adhesives Mixtures, coatings, electronics and composite materials and many other fields. Existing production method is mainly alkyd direct esterification method, with excess acrylic acid, toluene or benzene are water-carrying solvent, and sulfuric acid is catalyzer and makes final product, but this preparation method has following deficiency: 1. by-product and waste water of generation 2. Poor activity and flexibility; 3. Large chroma, acidity and viscosity, and easy to turbid; 4. High shrinkage, low yield, and poor quality. Contents of the invention [0003] The purpose o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/08
Inventor 牟国光
Owner TIANJIN CHEM REAGENT RES INST
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