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Epoxy plasticizer synthesis method based on perrhenate ionic liquid

A technology of epoxy plasticizer and ionic liquid, which is applied in the fields of fatty acid oxidation, chemical instruments and methods, and fatty acid production. The effect of simple processing

Active Publication Date: 2017-11-07
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional inorganic acids and strongly acidic cation exchange resins are commonly used catalysts for the epoxidation of fatty acid esters and soybean oil. During the use of such catalysts, a large amount of acidic wastewater is generated, causing serious environmental pollution.

Method used

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  • Epoxy plasticizer synthesis method based on perrhenate ionic liquid
  • Epoxy plasticizer synthesis method based on perrhenate ionic liquid
  • Epoxy plasticizer synthesis method based on perrhenate ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 1-butyl-3-methylimidazolium perrhenate ionic liquid ([Bmim]ReO 4 ) Catalyzed Synthesis of Epoxy Soybean Oil Plasticizer

[0023] [Bmim]ReO 4 The structural formula is as follows:

[0024]

[0025] Weigh 0.5g[Bmim]ReO 4 Catalyst and 20g refined soybean oil are housed in the 50mL three-necked flask of reflux condenser, thermometer, under stirring, slowly drop 5g H 2 o 2 (30%), and slowly warming up to 60°C, stirring at 60°C for 6h. After the reaction is finished, after the reaction solution is cooled to room temperature, the catalyst is separated by centrifugation, the reaction solution is washed with water to neutrality, and dried to obtain a yellow oily product, which is an epoxidized soybean oil plasticizer.

[0026] According to GB / T 1677-2008, the epoxy value of the epoxidized soybean oil plasticizer is 6.35%, and according to GB / T 1668-2008, the acid value of the epoxidized soybean oil plasticizer is 0.45 mg KOH / g.

[0027] The separated catalyst ...

Embodiment 2

[0028] Example 2 1-butyl-3-methylimidazolium perrhenate ionic liquid ([Bmim]ReO 4 ) Catalyzed Synthesis of Epoxy Fatty Acid Methyl Ester Plasticizer

[0029] [Bmim]ReO 4 The structural formula is as follows:

[0030]

[0031] Weigh 0.5g[Bmim]ReO 4 Catalyst and 20g fatty acid methyl esters are housed in the 50mL three-necked flask of reflux condenser, thermometer, under stirring, slowly add dropwise 5g H 2 o 2 (30%), and slowly warming up to 60°C, stirring at 60°C for 6h. After the reaction is finished, after the reaction solution is cooled to room temperature, the catalyst is separated by centrifugation, the reaction solution is washed with water until neutral, and dried to obtain a yellow oily product, which is an epoxy fatty acid methyl ester plasticizer.

[0032] According to GB / T 1677-2008, the epoxy value of the epoxy fatty acid methyl ester plasticizer is 6.46%, and according to GB / T1668-2008, the acid value of the epoxy fatty acid methyl ester plasticizer is 0.4...

Embodiment 3

[0034] Example 3 1-hexyl-3-methylimidazolium perrhenate ionic liquid ([Hmim]ReO 4 ) Catalyzed Synthesis of Epoxy Soybean Oil Plasticizer

[0035] [Hmim] ReO 4 The structural formula is as follows:

[0036]

[0037] Weigh 0.5g[Hmim]ReO 4 Catalyst and 20g refined soybean oil are equipped with in the 50mL three-necked flask of reflux condenser, thermometer, under stirring condition, slowly drop 5g H 2 o 2 (30%), and slowly warming up to 60°C, stirring at 60°C for 6h. After the reaction is finished, after the reaction solution is cooled to room temperature, the catalyst is separated by centrifugation, the reaction solution is washed with water to neutrality, and dried to obtain a yellow oily product, which is an epoxidized soybean oil plasticizer.

[0038] According to GB / T 1677-2008, the epoxy value of the epoxidized soybean oil plasticizer is 6.25%, and according to GB / T 1668-2008, the acid value of the epoxidized soybean oil plasticizer is 0.44 mg KOH / g.

[0039] The s...

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Abstract

The invention relates to an epoxy plasticizer synthesis method based on perrhenate ionic liquid. The method is characterized in that the perrhenate ionic liquid with the negative ions being ReO4<-> is used as a catalyst; H2O2 is directly used as an oxidizing agent; a solvent-free method is used for catalyzing soybean oil or fatty acid methyl ester to perform epoxidation reaction, and the epoxy plasticizer is synthesized. The reaction temperature is 30 to 60 DEG C; the reaction time is 2 to 6h. After the reaction is completed, centrifugal separation is performed to separate the catalyst; an oil phase is washed to a neutral state by de-ionized water; distillation is performed, thus an epoxy product can be obtained. The used catalyst is insoluble in raw material oil; the recovery and the use are easy; the environment pollution is avoided; the quality of the obtained epoxy plasticizer is higher.

Description

technical field [0001] The invention belongs to the field of chemical synthesis methods, and in particular relates to a method for synthesizing an epoxy plasticizer based on perrhenate ionic liquid. Background technique [0002] Epoxy plasticizer is a compound with an epoxy group in its molecular structure. It is an excellent plasticizer and stabilizer. Compared with phthalates on the market, its outstanding advantage is that it is non-toxic , Heat resistance and light resistance are good. In the industrial polyvinyl chloride resin processing industry, it not only has a plasticizing effect on PVC, but also stabilizes the active chlorine atoms on the polyvinyl chloride chain. The epoxy group in the structure can absorb hydrogen chloride degraded by light and heat. , thus preventing the continuous decomposition of PVC, acting as a stabilizer, and prolonging the service life of PVC products. Epoxy plasticizers have excellent water resistance and oil resistance, and are also g...

Claims

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Application Information

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IPC IPC(8): C11C3/00B01J31/02C07D301/12C07D303/42C08K5/1515
CPCB01J31/0279B01J31/0284B01J31/0298B01J2231/72C07D301/12C07D303/42C08K5/1515C11C3/006Y02P20/584
Inventor 周明东白雪门楠王景芸
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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