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Synthetic method for 1,2-epoxybutane

A technology of butylene oxide and synthesis method, applied in the direction of organic chemistry and the like, can solve the problems of uncontinuous reaction, low selectivity, low yield, etc., and achieve the effect of overcoming serious equipment corrosion and simple process

Inactive Publication Date: 2014-10-15
NANJING RED SUN NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, hydrogen peroxide is basically used as the oxygen source for epoxidation reaction. The main disadvantages are the low selectivity and low yield of 1,2-epoxybutane, and the continuous reaction cannot be carried out.

Method used

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  • Synthetic method for 1,2-epoxybutane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Inject a mixture of toluene, tributyl phosphate, and 30% (mass concentration) hydrogen peroxide with a molar ratio of 1:0.5:0.8 into the water separator to obtain a working fluid after dehydration under reduced pressure, and fill the working fluid with 1-butyl Alkene, reacted for 2h in the presence of catalyst silicotungstic heteropolyacid at temperature 50℃, pressure 0.1Mpa, catalyzed oxidation of 1-butene to generate 1,2-epoxybutane. Wherein, the molar ratio of 1-butene and 30% hydrogen peroxide is 2:1, and the mass concentration of the catalyst is 1% (relative to the working fluid). The obtained product was analyzed by chromatography, and the selectivity of 1,2-epoxybutane was 99.2%, and the yield of 1,2-epoxybutane to hydrogen peroxide was 95.6%.

Embodiment 2

[0018] Inject a mixture of toluene, tributyl phosphate, and 50% (mass concentration) hydrogen peroxide with a molar ratio of 1:1.5:2.6 into the water separator to obtain a working fluid after dehydration under reduced pressure, and fill the working fluid with 1-butyl Alkene, at a temperature of 70°C, a pressure of 0.3Mpa, and a catalyst mixture of silicotungstic heteropolyacid and phosphotungstic heteropolyacid (mass ratio 1:1) for 4 hours to catalyze the oxidation of 1-butene to generate 1,2-cyclo Oxybutane. Wherein, the molar ratio of 1-butene and 50% hydrogen peroxide is 4:1, and the mass concentration of the catalyst is 1.5% (relative to the working fluid). The obtained product was analyzed by chromatography, and the selectivity of 1,2-epoxybutane was 99.5%, and the yield of 1,2-epoxybutane to hydrogen peroxide was 96.3%.

Embodiment 3

[0020] Inject a mixture of toluene, tributyl phosphate, and 50% (mass concentration) hydrogen peroxide with a molar ratio of 1:0.8:1.5 into the water separator to obtain a working fluid after dehydration under reduced pressure, and fill the working fluid with 1-butyl At a certain temperature of 70°C, under a pressure of 0.5Mpa and in the presence of a catalyst, phosphotungstic heteropolyacid, react for 5 hours to catalyze the oxidation of 1-butene to generate 1,2-epoxybutane. Wherein, the molar ratio of 1-butene and 50% hydrogen peroxide is 3:1, and the mass concentration of the catalyst is 2.0% (relative to the working fluid). The obtained product was analyzed by chromatography, and the selectivity of 1,2-epoxybutane was 99.6%, and the yield of 1,2-epoxybutane to hydrogen peroxide was 96.8%.

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Abstract

The invention discloses a synthetic method for 1,2-epoxybutane. The method mainly comprises the step that the 1,2-epoxybutane is prepared through an one-step oxidation method, wherein an oxidizing agent is hydrogen peroxide. The synthetic method is simple in technological process, high in reaction yield, relatively low in preparation cost, and environmentally friendly in the whole process.

Description

technical field [0001] The invention relates to a synthesis process of an organic chemical intermediate, in particular to a new synthesis process of 1,2-epoxybutane. Background technique [0002] 1,2-Butylene oxide (BO), also known as butylene oxide, is an important organic chemical intermediate with a wide range of uses. It is mainly used to manufacture intermediates and polymers, and to replace acetone as a diluent for lacquer It can also be used as an antioxidant for chlorine-containing compounds, an anti-corrosion agent for the production of vinyl chloride resin, a surfactant, a gasoline additive, 1,1,1-trichloroethane (CH 3 -CCl 3 ) and stabilizers for other chlorinated solvents, etc. [0003] The production routes of 1,2-epoxybutane include chlorohydrin method, direct oxidation method and indirect oxidation method. The main production method of 1,2-epoxybutane in the industry still adopts the chlorohydrin process, that is, firstly use hypochlorous acid to chlorohydr...

Claims

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Application Information

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IPC IPC(8): C07D301/12C07D303/04
CPCC07D301/12C07D303/04
Inventor 李健张开炳方红新葛九敢薛谊
Owner NANJING RED SUN NEW MATERIAL