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A kind of synthetic method of aliphatic epoxy compound

An aliphatic epoxy and synthesis method technology, which is applied in the field of synthesis of aliphatic epoxy compounds, can solve the problems of difficult control of the reaction process, easy ring opening of epoxy bonds, expensive catalysts, etc., and achieve the effect of easy implementation

Active Publication Date: 2021-01-26
北京水木滨华科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to improve the deficiencies in the prior art, the purpose of the present invention is to provide a synthetic method of aliphatic epoxy compounds, which has the advantages of easy to obtain raw materials, simple and flexible operation, simple equipment, low cost, no need to add additional solvents, fast reaction rate High, high product quality, high conversion rate, etc., the prepared product can meet the requirements of high-end epoxy resin, and can solve the problem of large amount of reaction solvent, expensive catalyst, difficult to control the reaction process, and easy ring opening of epoxy bonds in the existing process. , poor product quality, low conversion rate, etc.

Method used

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  • A kind of synthetic method of aliphatic epoxy compound

Examples

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[0033] The preparation method of the present invention will be further described in detail in conjunction with specific examples below. It should be understood that the following examples are only for illustrating and explaining the present invention, and should not be construed as limiting the protection scope of the present invention. All technologies realized based on the above contents of the present invention are covered within the scope of protection intended by the present invention.

[0034] The experimental methods used in the following examples are conventional methods unless otherwise specified; the reagents and materials used in the following examples can be obtained from commercial sources unless otherwise specified.

[0035] The reaction apparatus used in the following examples is as figure 1 As shown, it does not limit the protection scope of the present invention, and all reaction bottle devices and reactor type devices having the same process function reactio...

Embodiment 1

[0038] In the there-necked flask of 500ml, add 25.37g 3,4-cyclohexene-1-carboxylic acid-3,4-cyclohexene-1-yl methyl ester and 100.63g TBHP-TBA solution (TBHP mass percent content is 46.05 wt%). Add 3.20g of catalyst molybdenum trioxide (400 mesh), heat up to 90-100°C to start extracting fractions such as by-product tert-butanol, react for 15min, continue to heat up to 100°C-110°C for about 70min and continue to extract by-product tert-butanol Butanol and other fractions were sampled to monitor the reaction progress. After the reaction, a total of 67 g of by-products such as tert-butanol were extracted, the temperature was lowered to 80° C., and 42.11 g of a crude reaction liquid was obtained by filtration.

[0039] Under the vacuum of -0.095MPa, the filtered reaction solution was distilled under reduced pressure at 120°C for 1.5 hours to obtain 28.87g of a colorless and transparent product. The resulting product was detected, and the epoxy equivalent was 130Gm / Eq, and the visco...

Embodiment 2

[0041] 42.00 bis((3,4-cyclohexenyl)methyl)adipate and 100.63g TBHP-TBA solution (the mass percentage of TBHP is 46.05wt%) was added to a 500ml three-necked flask. Add 3.50g catalyst molybdenum trioxide (400 mesh), heat up to 90-100°C and start to extract by-product tert-butanol and other fractions, react for 15min, continue to heat up to 100°C-110°C for about 70min and continue to extract by-product tert-butanol Butanol and other fractions were sampled to monitor the reaction progress. After the reaction, a total of 64.30 g of by-products such as tert-butanol were extracted, the temperature was lowered to 80° C., and 70.11 g of crude reaction liquid was obtained by filtration.

[0042] Under the vacuum of -0.095MPa, the filtered reaction solution was distilled under reduced pressure at 125°C for 1.5 hours to obtain 46.07g of a light yellow product. The resulting product was detected, and the epoxy equivalent was 194Gm / Eq, and the viscosity was 540mPa.s (25 ℃).

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Abstract

The invention provides a synthesis method of an aliphatic epoxy compound. The synthesis method comprises the following steps: mixing an aliphatic olefin, a molybdenum-containing solid epoxidation catalyst and an oxidant, and reacting to prepare the aliphatic epoxy compound; wherein by-products are continuously removed in the reaction process, and the by-products at least comprise by-products fromthe oxidant; the oxidant is selected from organic hydroperoxides, and the boiling point of the aliphatic olefin is higher than the boiling point of the by-products from the oxidant. The method has thecharacteristics of easily available raw materials, simple and flexible operation, simple equipment, low cost, no need of adding extra solvents, high reaction rate, high product quality, high conversion rate and the like; the prepared product can satisfy the requirements of high-end epoxy resin, and can solve the problems of large reaction solvent consumption, expensive catalyst price, easy ring opening of epoxy bonds, poor product quality, low conversion rate and the like in the prior art.

Description

technical field [0001] The invention belongs to the technical field of aliphatic epoxy compounds, and in particular relates to a synthesis method of aliphatic epoxy compounds. Background technique [0002] Aliphatic epoxy compounds can be used to prepare epoxy resins. Compared with traditional bisphenol A epoxy resins, they have good thermal stability, high weather resistance, and excellent electrical insulation performance because they do not contain residual chlorine and aromatic groups. and other characteristics, so the epoxy resin prepared by the aliphatic epoxy compound is widely used in coatings, packaging, electronics, automobiles and other fields. [0003] The commercially produced aliphatic diepoxides are mainly 3,4-epoxycyclohexylmethyl-3,4-epoxycyclohexyl carboxylate and bis((3,4-epoxycyclohexyl) Methyl) adipate, the peracid method (referring to U.S. patent document US2716123) that adopts the peracid method (referring to U.S. Patent Document US2716123) of U.S. Un...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/19C07D303/44C08G59/24
CPCC07D301/19C07D303/44C08G59/24
Inventor 解淑民马敏郑虓
Owner 北京水木滨华科技有限公司
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