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Method for preparing non-toxic environmental-friendly epoxy plasticizer

An epoxy plasticizer, non-toxic and environmentally friendly technology, used in organic chemistry and other directions, can solve the problems of long production cycle, easy to cause explosion, increase in sewage volume, etc., to reduce production costs, reduce sewage treatment burden, and eliminate chemical factors. Effect

Active Publication Date: 2010-12-15
江苏向阳科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] So far, epoxy plasticizers have been synthesized by solvent-free methods. Most of the epoxidation reactions use formic acid as the organic acid and concentrated sulfuric acid as the catalyst. Slowly add hydrogen peroxide dropwise under stirring. Hours, the production cycle is too long, in addition concentrated sulfuric acid and formic acid are medium-strong acids, the acid value of the finished product is difficult to control, the amount of effluent increases and the production cost increases, because the epoxidation reaction is a fast exothermic reaction, once the temperature of the reaction solution is not properly controlled explode

Method used

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  • Method for preparing non-toxic environmental-friendly epoxy plasticizer

Examples

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Effect test

Embodiment 1

[0028] In a 3000L reactor, put fatty acid methyl ester and glacial acetic acid (accounting for 15% by weight of fatty acid methyl ester) into the reactor in a corresponding proportion, heat up, start stirring and operate a closed cooling cycle device, heat up to 45°C and stop heating, Open the cooling water valve of the reaction kettle, add hydrogen peroxide (accounting for 35% of the mass proportion of fatty acid methyl ester) dropwise at a speed of 65g / s, the temperature of the reaction solution is controlled at 40-60°C, and the dropping time is 2 hours. Insulate and reflux for 2 hours to ensure that the epoxidation reaction is sufficient. Wash, neutralize, and distill under reduced pressure for 1.5 hours the crude epoxy plasticizer product, stop stirring and close the closed cooling cycle device, and dehydrate under reduced pressure to obtain non-toxic and environmentally friendly type epoxy plasticizer.

[0029] The closed cooling cycle device means that the reactor needs ...

Embodiment 2

[0033] In a 3000L reactor, put fatty acid methyl ester and glacial acetic acid (accounting for 10% by weight of fatty acid methyl ester) into the reactor in corresponding proportions, heat up, start stirring and operate a closed cooling cycle device, and heat up to 40°C to stop heating , open the cooling water valve of the reaction kettle, drip hydrogen peroxide (accounting for 35% of the mass proportion of fatty acid methyl ester) at a speed of 55g / s, the temperature of the reaction solution is controlled at 40-60°C, and the dropping time is 3 hours, and the hydrogen peroxide dripping ends Afterwards, heat preservation and reflux for 3 hours to ensure that the epoxidation reaction is sufficient, wash, neutralize, and distill under reduced pressure for 1.5 hours to the thick product of epoxy plasticizer, stop stirring and close the closed cooling cycle device, and dehydrate under reduced pressure to obtain non-toxic Environmentally friendly epoxy plasticizer.

Embodiment 3

[0035] In a 3000L reactor, put fatty acid methyl esters and glacial acetic acid (accounting for 15% by mass of fatty acid methyl esters) into the reactor in corresponding proportions, heat up and start stirring, heat up to 43°C to stop heating, and open the cooling water valve of the reactor , drip hydrogen peroxide (accounting for 35% of methyl formate mass proportion) with the speed of 20g / s, the temperature of reaction solution is controlled at 40-60 ℃, and the time of dropping is 6 hours. The oxidation reaction is sufficient, and the crude product of the epoxy plasticizer is washed with water, neutralized, distilled under reduced pressure for 2.5 hours, and dehydrated under reduced pressure to obtain a non-toxic and environment-friendly epoxy plasticizer.

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Abstract

The invention relates to a method for preparing a non-toxic environmental-friendly epoxy plasticizer, which is characterized by preparing the non-toxic environmental-friendly epoxy plasticizer by adopting fatty acid methyl ester as a raw material, hydrogen peroxide as oxidant and organic acid as an oxygen carrier. A non-toxic environmental-friendly epoxy plasticizer rough product is prepared by adopting a closed-end cooling circulation device through a one-step method without using any solvent, stabilizer and acid catalyst; and by water-washing, distilling, distributing and neutralizing with soda ash or calcium carbonate solution (pH is adjusted to 6.5-7.0), a chemical factor which probably pollutes the product is eliminated, a sewage treatment load is greatly reduced, and simultaneously, the production cost is also reduced. The preparation method of the invention has no poison, environmental protection, safety, water saving, stability, short production cycle and low energy consumption.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing plastic additives, in particular to a method for preparing a non-toxic and environment-friendly epoxy plasticizer. (2) Background technology [0002] In recent years, various parts of my country have successively invested in the construction of large-tonnage ethylene projects. Therefore, the demand for plasticizers in the entire plastics processing industry is also increasing year by year. In addition, a certain number of plasticizer products are exported. [0003] Foreign research on plasticizers is now mainly focused on non-toxic plasticizers such as terephthalates, phosphates, epoxy esters, fatty acid esters, polyesters, and trimellitates. ; In the selection of catalysts, traditional concentrated sulfuric acid is also abandoned, and catalysts such as solid ion superacids, organic acids, and heteropolyacids, which have little corrosion to equipment and produce less pollution, are used. However, ...

Claims

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Application Information

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IPC IPC(8): C07D303/42C07D301/16C08K5/1515
Inventor 李祥庆
Owner 江苏向阳科技有限公司
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