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Preparation method of composite epoxy plasticizer

A technology of plasticizer and composite ring, which is applied in the field of preparation of composite epoxy plasticizers, can solve the problems of difficult dehydration in the production process of epoxy soybean oil, the darkening of epoxy soybean oil, and the diving of international agricultural product prices. High cost adjustment flexibility, high epoxy value, and the effect of increasing profit margins

Active Publication Date: 2012-09-05
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

The implementation of these environmental regulations is a challenge and an opportunity for plasticizer companies
Moreover, phthalate plasticizers are derived from petroleum. In recent years, the energy crisis has intensified. The sharp rise in the price of crude oil has led to a sharp rise in the cost of plasticizers, and the development has slowed down significantly. Plasticizers are facing adjustments in product structure and varieties. Epoxidized soybean oil prepared from renewable plant resources, as a new environment-friendly plasticizer with superior performance, has been highly concerned by more and more plastic processing and plasticizer manufacturers, and is regarded as a phthalate ester additive. A good substitute for plasticizers, but due to the similar relative density of epoxy soybean oil and water at room temperature, the production process of epoxy soybean oil is difficult to dehydrate, so the production rate is reduced, and because epoxy soybean oil itself is easy to oxidize, high temperature distillation and dehydration If the temperature is too high or the time is too long, the color of epoxy soybean oil will become darker, which will affect the quality of finished products
[0004] In June 2007, with the rising trend of soybean oil prices, its increase in the spot market has risen from 25% to 43%. The price of agricultural products "dived" sharply, and the soybean oil market fell by the limit
It is not difficult to see that the price of epoxidized soybean oil will fluctuate with the price fluctuation of raw material soybean oil, which will bring great pressure to the sales of epoxidized soybean oil and directly affect the profit of the factory. The green environment-friendly plasticizer with similar physical and chemical properties of epoxidized soybean oil is imminent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 25% fatty acid methyl ester by weight and the remaining amount of soybean oil mixture, and formic acid accounting for 10% of the raw material mass proportion into the reactor, heat up and start stirring, heat up to 45 ° C to stop heating, stir for 15 minutes, and then dropwise add The hydrogen peroxide with a raw material mass proportion of 25%, because it is an exothermic reaction, the cold water circulation device is turned on during the dropping process, and the temperature of the reaction liquid is controlled at 40-60°C to reduce the occurrence of side reactions. Oxidation reaction fully carries out, thereby makes composite epoxy plasticizer initial product, and composite epoxy plasticizer initial product is washed to remove acid, and when sampling detection acid value (KOH mg / g) is less than 1, vacuum distillation again Dehydration treatment is carried out to obtain the finished composite epoxy plasticizer.

Embodiment 2

[0023] Embodiment 2: 90% by weight of fatty acid methyl ester and the soybean oil mixture of remainder, and the formic acid that accounts for 10% of raw material mass proportion are put into reactor, heat up and start stirring, be warming up to 40 ℃ and stop heating, stir 10 minutes, Then add hydrogen peroxide which accounts for 35% of the mass ratio of raw materials. Since it is an exothermic reaction, turn on the cold water circulation device during the dropping process, and control the temperature of the reaction liquid at 40-60 ° C to reduce the occurrence of side reactions. After the hydrogen peroxide drop is completed, keep warm Reflux to ensure that the epoxidation reaction is fully carried out, thereby making the first product of the composite epoxy plasticizer, washing the first product of the composite epoxy plasticizer to remove acid, sampling and detecting the acid value (KOH mg / g) is less than 1, Then carry out dehydration treatment by vacuum distillation to obtain...

Embodiment 3

[0025] Put 45% fatty acid methyl ester by weight and the remaining amount of soybean oil mixture, and formic acid accounting for 8% of the raw material mass proportion into the reactor, heat up and start stirring, heat up to 43 ° C to stop heating, stir for 20 minutes, and then dropwise add The hydrogen peroxide with a mass proportion of 30% of the raw material is an exothermic reaction. During the dropping process, the cold water circulation device is turned on. The temperature of the reaction liquid is controlled at 40-60°C to reduce the occurrence of side reactions. Oxidation reaction fully carries out, thereby makes composite epoxy plasticizer initial product, and composite epoxy plasticizer initial product is washed to remove acid, and when sampling detection acid value (KOH mg / g) is less than 1, vacuum distillation again Dehydration treatment is carried out to obtain the finished composite epoxy plasticizer.

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PUM

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Abstract

The invention relates to a preparation method of a composite epoxy plasticizer. The composite epoxy plasticizer is prepared by mixing raw materials of fatty acid methyl ester and soybean oil through one-step epoxidation reaction, wherein the fatty acid methyl ester accounts for 25-90% by mass, hydrogen peroxide is used as an oxygen supplier and accounts for 25-35% of the raw material by mass, andformic acid is used as an oxygen carrier and accounts for 5-10% of the raw material by mass. The composite epoxy plasticizer mainly comprises epoxy fatty acid methyl ester and epoxy soybean oil. The preparation method has the characteristics of no toxicity, environmental protection, soft hand feel, high epoxy value, good thermal stability and great cost adjustment elasticity.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing plastic additives, in particular to a method for preparing a composite 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 has also increased year by year. In addition, a certain amount of plasticizers is exported. [0003] With the gradual enhancement of people's awareness of environmental protection, countries all over the world have put forward higher hygiene requirements for plasticizers. The currently mainly used phthalate plasticizers are low-molecular substances, highly volatile, easy to dissipate in the environment, and have potential carcinogenic risks. In many countries, their production and application have been regulated by relevant regulations ( Such as the strict restrictions...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/12
Inventor 李祥庆
Owner 江苏向阳科技有限公司