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Dibasic acid modified epoxy stillingia oil methyl ester plasticizer and preparation method thereof

A technology of acid epoxy fatty acid ester and epoxy catalpa, which is applied in the field of oil utilization and plasticizer development, can solve the problems of low flash point, high energy consumption, poor effect, etc., and achieve the effect of increasing relative molecular weight and reducing content

Inactive Publication Date: 2017-11-24
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the shortcomings of low product flash point and existing modification technology, such as long process time consumption, high energy consumption and poor effect, the invention provides a method for dibasic acid modified epoxy catalphal methyl ester plasticizer

Method used

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  • Dibasic acid modified epoxy stillingia oil methyl ester plasticizer and preparation method thereof
  • Dibasic acid modified epoxy stillingia oil methyl ester plasticizer and preparation method thereof
  • Dibasic acid modified epoxy stillingia oil methyl ester plasticizer and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Raw materials: catalpa oil, methanol, hydrogen peroxide, potassium hydroxide, p-toluenesulfonic acid, maleic acid, N,N-dimethylbenzylamine;

[0031] Put methanol and catalpa oil into the reactor according to the proportion of 6:1, and add potassium hydroxide accounting for 0.6% of the mass fraction of catalpa oil, stir and reflux reaction at 65 ° C for 3 hours, remove methanol and Glycerol has obtained catalpa methyl ester; the gained catallyl methyl ester is put into the reactor, adds 15% formic acid and 1% p-toluenesulfonic acid accounting for the quality of the methyl ester, is heated to 55° C. and drips hydrogen peroxide (30 %), dripped in 40 minutes, and then heated up to 65 ° C for 4 hours. After cooling down, separate the liquid and remove the water, and then undergo conventional post-treatments such as alkali washing, water washing, distillation, etc. to obtain a light yellow transparent liquid epoxy catalphine methyl ester; put epoxy catalphine methyl ester and...

Embodiment 2

[0034] Raw materials: catalpa methyl ester, m-chloroperoxybenzoic acid, p-toluenesulfonic acid, maleic anhydride, N,N-dimethylbenzylamine;

[0035] Put catalphine methyl ester into the reactor, keep the temperature at 0-30°C, add 1.2 g of m-chloroperoxybenzoic acid solution dropwise, drop it within 1 hour, and then react for 5 hours. Finally, through certain conventional post-treatments such as filtration, alkali washing, water washing, dehydration, etc., the light yellow transparent intermediate product epoxy catalphal methyl ester is obtained; the ratio of epoxy catalphal methyl ester and maleic anhydride is 1:0.15 according to the amount of substance Put it into the reaction kettle, then add the catalyst N,N-dimethylbenzylamine accounting for 1% mass fraction of epoxy catalphine methyl ester, stir and heat up to 105°C for about 4 hours, and the acid value is 0.32mgKOH / g, Stop responding. The crude product is a reddish-brown transparent viscous liquid.

Embodiment 3

[0037] Raw materials: epoxy catalphine methyl ester, maleic anhydride, N,N-dimethylbenzylamine;

[0038] Put epoxy catalphine methyl ester and maleic anhydride in the ratio of 1:0.29 into the reaction kettle, and then add the catalyst N,N-dimethylbenzylamine which accounts for 1% mass fraction of epoxy catalphine methyl ester , stirring and raising the temperature to 120° C. for about 4 hours, the acid value was measured to be 0.51 mgKOH / g, and the reaction was stopped. The crude product is a reddish-brown transparent viscous liquid.

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Abstract

The invention relates to a dibasic acid modified epoxy stillingia oil methyl ester plasticizer and a preparation method thereof. Stillingia oil (or fatty acid methyl ester of stillingia oil), peroxides, and dibasic acid are taken as raw materials. At first, tallow seed oil is converted into epoxy stillingia oil methyl ester; and then catalytic ring opening and esterification of dibasic acid are carried out to generate epoxy fatty acid esters of dibasic acid. The preparation method can effectively reduce the content of short chain fatty acid esters (methyl 2,4-decadienoate) in stillingia oil methyl ester and increase the average molecular weight. The plasticizer has the characteristics of low volatility, mobility resistance, good durability, and high flash point. The plasticizer is suitable for being used as a co-plasticizer.

Description

technical field [0001] The invention relates to a method for modifying epoxy catalphine methyl ester plasticizer with dibasic acid, which belongs to the fields of grease utilization and plasticizer development. Background technique [0002] Plasticizers are high polymers such as rubber, plastics, coatings, etc., which are low-molecular compounds added to increase their fluidity and plasticity during molding and processing to make the finished product flexible. It is one of the indispensable additives in the processing of PVC and other plastics, and its consumption is huge. my country is the world's largest producer and consumer, and its production capacity has reached 4 million tons in 2015, and it continues to grow year by year. Among them, phthalates account for the vast majority. However, studies have shown that phthalic acid plasticizers are potentially carcinogenic, and developed countries such as Europe and the United States have banned them. The development of epoxy...

Claims

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Application Information

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IPC IPC(8): C08K5/00C08K5/11C08K5/12
CPCC08K5/0016C08K5/11C08K5/12
Inventor 李科聂小安蒋剑春黄金瑞胡芳芳
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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