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Method for preparing polydiallyl itaconate and dimer acid

A technology of dimer acid methyl ester and fatty acid methyl ester, which is applied in the field of mixed unsaturated fatty acid methyl ester, can solve the problems affecting the yield and quality of dimer acid methyl ester, increase the difficulty of separation, oxidation reaction, etc., and achieve the goal of equipment The effect of reduced requirements, simple method and fast separation speed

Active Publication Date: 2011-06-29
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction temperature of heterogeneous catalysis is generally above 250°C. Unsaturated fatty acids and their methyl esters become unstable at high temperatures for a long time, and oxidation reactions and side reactions (generation of polymer products) are prone to occur during the reaction process. , affecting the yield and quality of dimer acid methyl ester, but also increasing the difficulty of separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: in 0.5L reactor, add rapeseed oil fatty acid methyl ester (main component is methyl oleate, methyl linoleate, methyl linolenate, acid value 1.58mgKOH / g oil), cocatalyst thick The amount of sulfuric acid added is 0.15%, and mechanically stirred at about 50-55°C for about 1 hour. Then add 3.5% anhydrous aluminum trichloride, and rapidly heat up to about 170 ℃ for polymerization reaction, the polymerization reaction ends (5 hours), the reaction mixture is added the dilute solution (pH=7.5) of weak base sodium carbonate, sedimentation 10 hours (or direct centrifugation), separate the lower layer of aluminum hydroxide and a small amount of impurities, the upper layer is thick dimer acid methyl ester (iodine value 67), after warm water washing treatment to neutrality, the thick dimer acid methyl ester is obtained, The yield was 83.0%.

[0025] Gained thick dimer acid methyl ester enters molecular distillation device, and condition is vacuum tightness 4-10Pa, di...

Embodiment 2

[0026] Embodiment 2: in 0.5L reactor, add safflower seed oil fatty acid methyl ester (main component is methyl oleate, methyl linoleate, methyl linolenate, acid value 2.38mgKOH / g oil), cocatalyst The added amount of concentrated sulfuric acid is 0.2%, and mechanically stirred at about 50-55°C for about 1.5 hours. Then add 4.5% anhydrous zinc trichloride, and rapidly heat up to about 200°C for polymerization reaction, the polymerization reaction ends (6 hours), the reaction mixture is added a dilute solution of weak alkali sodium carbonate (pH=7.5), and settles for 10 hours (or direct centrifugation), separate the lower layer of zinc hydroxide and a small amount of impurities, the upper layer is thick dimer acid methyl ester (iodine value 66), after warm water washing treatment to neutrality, the thick dimer acid methyl ester is obtained, producing The rate is 85.0%.

[0027] Gained thick dimer acid methyl ester enters molecular distillation device, and condition is vacuum tig...

Embodiment 3

[0028] Embodiment 3: in 0.5L reactor, add mixed unsaturated fatty acid methyl ester (the total content of oleic acid methyl ester, linoleic acid methyl ester, linolenic acid methyl ester is 92%, acid value 0.75mgKOH / g oil), Concentrated sulfuric acid as a cocatalyst is added in an amount of 0.2%, and mechanically stirred at about 50-55°C for about 0.5 hours. Then add 4.0% anhydrous aluminum trichloride, and rapidly heat up to about 190°C for polymerization reaction, the polymerization reaction ends (5 hours), the reaction mixture is added a dilute solution of weak alkali sodium carbonate (pH=7.5), and settles for 10 hours (or direct centrifugation), separate the lower layer of zinc hydroxide and a small amount of impurities, the upper layer is thick dimer acid methyl ester (iodine value 65), after warm water washing and processing to neutrality, the thick dimer acid methyl ester is obtained, producing The rate is 85.2%.

[0029] Gained thick dimer acid methyl ester enters mol...

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Abstract

The invention relates to a method for preparing dimeric acid methyl ester and dimer acid thereof. The method comprises the following steps: performing dimerization reaction of mixed fatty acid methyl ester having high unsaturated fatty acid methyl ester content or mixed fatty acid in the presence of concentrated sulfuric acid as co-catalyst and anhydrous aluminum chloride or anhydrous zinc chloride as catalyst using two step catalytic method; and solving with weak alkali diluted solution (the pH value is 7-8), washing for removing the catalyst to obtain coarse dimmer (yield of more than 80%),and further performing molecular distillation of coarse dimeric fatty acid methyl ester or coarse dimeric fatty acid in certain condition for removing monomer to reach dimmer content of greater than 90%. The method is carried out at normal pressure with less catalyst which can be removed easily. The coarse product is separated using an advanced molecular distillation device to avoid dimmer decomposition and occurrence of other byproducts at high temperature, and improve product purity. The method has simple process, easy operation, reduced energy source and reduced cost.

Description

technical field [0001] The invention relates to a method for preparing dimer acid methyl ester and its dimer acid. It adopts mixed fatty acid methyl ester with relatively high content of unsaturated fatty acid methyl ester as a raw material, and prepares dimer acid methyl ester in two steps by using a homogeneous catalysis method. Esters, the mixed unsaturated fatty acid methyl esters, specifically refer to mixed unsaturated fatty acid methyl esters corresponding to mixed fatty acids with higher content of oleic acid, linoleic acid and linolenic acid. And the present invention adopts mixed fatty acid as raw material, dimer acid can be prepared by the same method. Background technique [0002] Dimer acid methyl ester is an acyclic dimer or monocyclic dimer generated by unsaturated fatty acid methyl ester under the action of a catalyst. It is an important chemical intermediate. Generally speaking, dimer acid methyl ester mainly refers to A dimer formed by the polymerization o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/58C07C67/333
Inventor 李为民姚超王车礼宋丽
Owner 溧阳常大技术转移中心有限公司
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