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Epoxy plant oil and preparation method thereof

A technology of epoxy vegetable oil and vegetable oil, which is applied in the direction of fatty acid production and fatty acid chemical modification, can solve the problems of easy production of by-products, easy ring-opening of epoxy groups, cumbersome process, etc., to avoid ring-opening side reactions and good industrial application Foreground, the effect of high selective oxidation

Inactive Publication Date: 2011-04-20
SOUTHWEST FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation of epoxy vegetable oil mainly adopts a two-step method and a one-step method. The main process of the two-step method is that an organic acid (formic acid or acetic acid) reacts with hydrogen peroxide under the action of a catalyst to generate a peroxyacid epoxy oxidant, and then drips it The method of oxyacid epoxidation agent makes the vegetable oil undergo epoxidation reaction. After the reaction, it needs to undergo alkali washing, water washing, vacuum distillation and other treatment processes to finally obtain epoxy vegetable oil. This method is cumbersome; the one-step method is The epoxidation of vegetable oil can be realized at the same time as the oxyacid, and the direct generation of peroxyacid and the synthesis of downstream products are integrated into one reactor. This method has short production process, simple operation, low cost, and eliminates the need to use peroxyacid. has become the main method in industrial production, but there are still many deficiencies
Most of the catalysts used in these two methods are concentrated sulfuric acid and organic acids, etc., which are easy to corrode equipment, and the resulting products have darker colors, easy to produce by-products, low epoxy value, and poor thermal stability.
Moreover, there is also the problem that the reaction solution and the catalyst are in the same phase and are not easy to separate, and the resulting epoxy group is easy to open the ring.
In addition, using strongly acidic cation exchange resin as a catalyst to prepare epoxy vegetable oil can avoid the shortcomings of catalytic preparation of epoxy vegetable oil, but the ion exchange resin must be strictly pretreated before the reaction, the operation is complicated, and the epoxidation time is long, and the energy consumption is high. Big, high cost;

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 20g of soybean oil and 10g of ethyl acetate into the reaction kettle, and stir at 50°C for 20 minutes. After the system is evenly mixed, add 1g of titanium-silicon molecular sieve (the carrier is MCM-41, the same below; the molar ratio of titanium to silicon is 0.005 , pore size 2nm, surface area 1200m 2 / g), and stirred for 20 minutes, then added 6.8g of hydrogen peroxide, and maintained the reaction temperature for 3 hours. The phase material was washed to neutral. Then the liquid phase material was moved to a vacuum rotary distillation pot, and the moisture was removed by vacuum distillation at a temperature of 80° C. until the water content was lower than 0.5%, and the temperature was lowered to room temperature to obtain epoxidized soybean oil.

[0023] Measured: the epoxy value is 3.7%, the iodine value is 18.1%; the acid value is 4.2KOH mg / g.

Embodiment 2

[0025] Put 20g of soybean oil and 30g of ethyl acetate into the reaction kettle, and stir at 90°C for 20 minutes. After the system is evenly mixed, add 2g of titanium-silicon molecular sieve (titanium-silicon molar ratio is 0.01, pore size is 2.6nm, surface area is 1150m 2 / g), and stirred for 20 minutes, then added 7g of tert-butyl hydroperoxide, maintained the reaction temperature for 30 hours, after the reaction was completed, cooled to 40°C, filtered with suction, separated the catalyst and the liquid phase material, and then deionized water Wash the liquid phase material to neutrality. Then the liquid phase material is moved to a vacuum rotary distillation kettle, and the moisture is removed by vacuum distillation under the condition of a temperature of 80° C. until the water content is lower than 0.5%, and the temperature is lowered to room temperature to obtain epoxidized soybean oil;

[0026] Measured: the epoxy value is 6.3%, the iodine value is 3.1%; the acid value i...

Embodiment 3

[0028] Put 20g of soybean oil and 30g of ethyl acetate into the reaction kettle and stir at 100°C for 20 minutes. After the system is evenly mixed, add 3g of titanium-silicon molecular sieve (the molar ratio of titanium to silicon is 0.03, the pore size is 5nm, and the surface area is 1000m 2 / g), and stirred for 20 minutes, then added 9g of tert-butyl hydroperoxide, maintained the reaction temperature for 30 hours, after the reaction was completed, cooled to 40°C, filtered with suction, separated the catalyst and the liquid phase material, and then deionized water Wash the liquid phase material to neutrality. Then the liquid phase material is moved to a vacuum rotary distillation kettle, and the moisture is removed by vacuum distillation under the condition of a temperature of 80° C. until the water content is lower than 0.5%, and the temperature is lowered to room temperature to obtain epoxidized soybean oil;

[0029] Measured: the epoxy value is 5.8%, the iodine value is 3....

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PUM

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Abstract

The invention relates to epoxy plant oil and a preparation method thereof. In the preparation method, the epoxy plant oil is synthesized by taking soybean oil, caster oil, rubber seed oil, palm oil, cotton seed oil, rap oil, corn oil and the like as raw materials, using mesoporous titanium-silicon molecular sieve as a catalyst and utilizing hydroperoxides for reaction, wherein the epoxy value of the epoxy plant oil is 3.1-6.3%, the iodine value of the epoxy plant oil is 3.0-18.1% and the acid value of the epoxy plant oil is 0.6-4.3 KOH mg / g. The reaction process is carried out in the presence of no carbosylic acid and no protonic acid, thereby generating no acid waste water and being friendly to environment.

Description

technical field [0001] The invention relates to an epoxy vegetable oil which can be used as a plasticizer in plastics and rubber and a preparation method thereof. Background technique [0002] Epoxy vegetable oil is mainly used as polyvinyl chloride plasticizer and stabilizer. It has good thermal and light stability, water resistance and oil resistance, and has good compatibility, low volatility and small migration. It has developed into the first Three types of plasticizers. Epoxy vegetable oil has very little toxicity, and can also be used as food and drug packaging materials, as additives for toys and home decoration materials, among which epoxy soybean oil has been approved by the US Food and Drug Administration as an epoxy resin that can be used in food packaging materials. class of plasticizers. [0003] At present, the preparation of epoxy vegetable oil mainly adopts a two-step method and a one-step method. The main process of the two-step method is that an organic ...

Claims

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Application Information

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IPC IPC(8): C11C3/00C08K5/1515
Inventor 黄元波郑志锋郑云武
Owner SOUTHWEST FORESTRY UNIVERSITY
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