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Method for preparing tri(propylene glycol) diacrylate

A technology of tripropylene glycol diacrylate and tripropylene glycol is applied in the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc. Many problems, poor activity and flexibility, etc., to achieve the effect of low viscosity and shrinkage, less by-products and waste water, and good activity and flexibility

Active 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 to adopt alkyd esterification method, with acrylic acid excess, toluene or benzene are water-carrying solvent, and sulfuric acid is catalyzer to make final product, but there are following deficiencies: 1. the by-product and waste water that generate are more, to The environmental pollution is serious; 2. Poor activity and flexibility; 3. Large chroma, acidity and viscosity, and easy to turbid; 4. High shrinkage, low yield, and poor quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of tripropylene glycol diacrylate, the steps of its preparation method are:

[0027] (1). Put 500g of tripropylene glycol, 400g of acrylic acid, 10g of p-toluenesulfonic acid and 400g of toluene into the reaction kettle, and add 100ppm of hydroquinone, 100ppm of p-hydroxyanisole, and 50ppm of phenothiazine , copper sulfate 300ppm, add decolorizing agent active carbon 50ppm at the same time in the reaction system and form a mixed solution after fully mixing and stirring;

[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 mixed solution, and reflux for 3 hours when the temperature rises to 80°C, and the reaction ends;

[0030] (4). Adding a concentration of 10% soda ash aqueous solution and a concentration of 20% sodium chloride aqueous soluti...

Embodiment 2

[0034] A preparation method of tripropylene glycol diacrylate, the steps of its preparation method are:

[0035] (1). Put 600g of tripropylene glycol, 500g of acrylic acid, 100g of methanesulfonic acid and 600g of n-hexane into the reaction kettle, and add 250ppm of hydroquinone as a polymerization inhibitor, and 500ppm of activated carbon as a decolorizing agent in the reaction system Mix well to form a mixture;

[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 mixed solution, and reflux for 5 hours when the temperature rises to 115°C, and the reaction ends;

[0038] (4). Adding a concentration of 10% soda ash aqueous solution and a concentration of 20% sodium chloride aqueous solution to the mixed solution, washing for 3 times and standing for stratifica...

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PUM

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Abstract

The invention belongs to a method for preparing tripropylene glycol diacrylate ester, comprising the steps as follows: (1) tripropylene glycol, 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 to the temperature of 70-90 DEG C for a 20-40min reaction; (3) when the temperature is continued to be increased to 80-115 DEG C, reflow is carried out for 3-5h 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) and then cooling and filter 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 diluents, in particular to a preparation method of tripropylene glycol diacrylate. Background technique [0002] Tripropylene glycol diacrylate (TPGDA) is a bifunctional functional monomer with the molecular formula C 15 h 24 o 6 , with a molecular weight of 300, easily soluble in organic solvents such as low-carbon alcohols and aromatic hydrocarbons, insoluble in water, and generally appear as a colorless or light yellow transparent oily liquid. The tripropylene glycol diacrylate is used as a reactive diluent for UV and In the radiation crosslinking of EB, it can become a crosslinked polymer composition, and can endow the photocured film with better flexibility and stability, as well as stronger wear resistance and corrosion resistance. Existing production method is to adopt alkyd esterification method, with acrylic acid excess, toluene or benzene are water-carrying solvent, and sulfuric acid is catalyzer to ma...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/08
Inventor 牟国光
Owner TIANJIN CHEM REAGENT RES INST
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