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Method for preparing pentaerythritol triacrylate

A pentaerythritol triacrylate and pentaerythritol technology are applied in the field of preparation of pentaerythritol triacrylate, can solve the problems of troublesome by-product treatment of waste water, serious environmental impact, poor activity and flexibility, etc., achieve low shrinkage and chromaticity, reduce Good effect of production cost, activity and flexibility

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

Synthetic pentaerythritol triacrylate mainly uses concentrated sulfuric acid as catalyzer at present in industry, is prepared through esterification reaction by acrylic acid and pentaerythritol, and the product that this technique obtains has following defects: 1. poor product quality, chromaticity, acidity and viscosity are higher , and easily turbid; 2. The activity and flexibility are poor, and the shrinkage rate is high; 3. The waste water and by-products after the reaction are troublesome to deal with, and the environmental impact is serious; 4. The product process is complex and the equipment is seriously corroded

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] The preparation method of this pentaerythritol triacrylate, the catalyst can be one of p-toluenesulfonic acid, methanesulfonic acid or silicotungstic acid; the selected solvent is one of toluene, benzene, n-hexane, cyclohexane Or several kinds, or a mixture of two or more kinds, and several kinds of solvents can be mixed and used in any proportion when preparing the solvent. The polymerization inhibitor selected here is one of hydroquinone, p-hydroxyanisole, phenothiazine, copper sulfate, or a mixture of two or more, and the addition amounts are:

[0027] Hydroquinone 100—250ppm;

[0028] p-Hydroxyanisole 100—500ppm;

[0029] Phenothiazine 50—300ppm;

[0030] Copper sulfate 300-800ppm.

[0031] While adding the polymerization inhibitor in the reactor, 50-500ppm of decolorizing agent activated carbon can be added.

Embodiment 1

[0033] A preparation method of pentaerythritol triacrylate, the steps of the preparation method are:

[0034] (1).Put 350g of pentaerythritol, 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, phenothiazine 50ppm, copper sulfate 300ppm, and at the same time add 50ppm of activated carbon in the reaction system to form a mixed solution after fully mixing and stirring;

[0035] (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 30 minutes to react;

[0036] (3). Continue to heat the mixed solution, and reflux for 3 hours when the temperature rises to 80°C, and the reaction ends;

[0037] (4). Adding a concentration of 10% soda ash aqueous solution and a 20% sodium chloride aqueous solution to the mixed solution...

Embodiment 2

[0041] A preparation method of pentaerythritol triacrylate, wherein the steps of the preparation method are:

[0042] (1).Put 400g of pentaerythritol, 650g of acrylic acid, 100g of catalyst and 600g of solvent 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. liquid;

[0043] (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 90°C within 1h and maintain this temperature for 40 minutes to react;

[0044] (3). Continue to heat the mixed solution, and reflux for 5 hours when the temperature rises to 115°C, and the reaction ends;

[0045] (4). Adding a concentration of 10% soda ash aqueous solution and a concentration of 20% sodium chloride aqueous solution to the mixed solution, washing 4 times and standing for stratification, and taking the upper organic phase...

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Abstract

The invention belongs to a method for preparing pentaerythritol trimethylacrylate, comprising the steps as follows: (1) pentaerythritol, acrylic acid, catalyst, solvent and polymerization inhibitor are put into a reaction kettle to be fully mixed and stirred so as to form a miscible liquid; (2) a steam valve of the reaction kettle is opened to slowly heat the miscible liquid, and the temperature is controlled and maintained at 70-90 DEG C for a 20-40min reaction; (3) the mixture is continued to be heated, when the temperature is 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 filter pressing is carried out to obtain the end product. The method has simple process, good quality, activity and flexibility, low shrinking percentage and color intensity and high yield coefficient, and produces few by-products or little waste water.

Description

technical field [0001] The invention belongs to the field of diluents, in particular to a preparation method of pentaerythritol triacrylate. Background technique [0002] Pentaerythritol triacrylate (PETA) is an important acrylic acid trifunctional ester monomer, its molecular weight is 298, and its appearance is colorless or light yellow liquid. The characteristics of this product are high cross-linking density, fast curing and good flexibility. , low volatility, scratch resistance, fire resistance, chemical resistance, mainly used in many fields such as coatings, adhesives, electronics and composite materials. The industrial synthetic pentaerythritol triacrylate mainly uses concentrated sulfuric acid as catalyzer at present, is prepared through esterification reaction by acrylic acid and pentaerythritol, and the product that this technique obtains has following defects: 1. poor product quality, chromaticity, acidity and viscosity are higher , and easily turbid; 2. The act...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/04
Inventor 牟国光
Owner TIANJIN CHEM REAGENT RES INST
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