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Method of producing 3,4-epoxy-1-butylene

A technology of butene and epoxy, applied in the direction of organic chemistry, etc., can solve the problems of low conversion rate of raw materials, wasteful product yield, etc.

Active Publication Date: 2016-02-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that the prior art has the problems of low raw material conversion rate, serious waste and low product yield, and a new method for producing 3,4-epoxy-1-butene is provided

Method used

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Examples

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Effect test

Embodiment 1

[0035] Under the condition of 105 DEG C and 0.4 MPa, and the volume content of tail oxygen is controlled to be less than 5%, the cumene and air are oxidized to obtain cumene hydroperoxide (CHP) oxidation solution with a weight concentration of 20-24%.

[0036] Wash the cumene hydroperoxide oxidation solution with an aqueous solution with a weight content of 2% NaOH, wherein the volume ratio of the oxidation solution to the alkali solution is 3:1, and remove the organic acid therein. Then wash the oxidizing solution with deionized water to remove the residual Na due to alkaline washing + , wherein the volume ratio of oxidizing solution to deionized water is 3:1. According to the needs of the epoxidation reaction, vacuum concentration is carried out to it, the concentration temperature is 75° C., and the cumene hydroperoxide concentration is obtained to be 50% by weight of the oxidation solution, and the residual water due to washing is also to a certain extent when concentratio...

Embodiment 2

[0041]Under the condition of 100 DEG C and 0.3 MPa, and the volume content of tail oxygen is controlled to be less than 5%, cumene and air are oxidized to obtain cumene hydroperoxide (CHP) oxidation solution with a weight concentration of 20-24%.

[0042] Using Na 2 CO 3 Wash the cumene hydroperoxide oxidation solution with an aqueous solution with a weight content of 5%, wherein the volume ratio of the oxidation solution to the alkali solution is 4:1, and remove the organic acid therein. Then wash the oxidizing solution with deionized water to remove the residual Na due to alkaline washing + , wherein the volume ratio of oxidizing solution to deionized water is 4:1. According to the needs of the epoxidation reaction, it is concentrated in vacuum, the concentration temperature is 70°C, and the cumene hydroperoxide concentration is obtained to be 40% by weight of the oxidation solution, and the residual water due to washing is also to a certain extent when the concentration i...

Embodiment 3

[0047] Under the conditions of 98° C. and 0.3 MPa and controlling the volume content of tail oxygen to be lower than 5%, the cumene and air are oxidized to obtain a cumene hydroperoxide (CHP) oxidation solution with a weight concentration of 20-24%.

[0048] Wash the cumene hydroperoxide oxidation solution with an aqueous solution with a weight content of 2% NaOH, wherein the volume ratio of the oxidation solution to the alkali solution is 3:1, and remove the organic acid therein. Then wash the oxidizing solution with deionized water to remove the residual Na due to alkaline washing + , wherein the volume ratio of oxidizing solution to deionized water is 4:1. According to the needs of the epoxidation reaction, vacuum enrichment is carried out to it, and the enrichment temperature is 80° C., and the cumene hydroperoxide concentration is obtained to be 60% by weight of the oxidized liquid. When enriching, the residual water due to washing is also to a certain extent above is re...

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Abstract

The invention relates to a method of producing 3,4-epoxy-1-butylene and mainly solves the problem that a method in the prior art is low in raw material conversion rate, is serious in waste and is low in production yield. The synthetic method includes the following steps: a) performing a reaction to isopropyl benzene and air to obtain a hydrogen peroxide isopropyl benzene oxidized liquid; b) controlling the weight percentage ratio of organic acid to be not more than 0.3%, the weight percentage ratio of alkali metal ions or alkali earth metal ions to be not more than 0.1% and the weight percentage ratio of water to be not more than 0.5% in the hydrogen peroxide isopropyl benzene oxidized liquid; c) performing an epoxidation reaction to the hydrogen peroxide isopropyl benzene oxidized liquid with 1,3-butadiene to generate the 3,4-epoxy-1-butylene and [alpha],[alpha]-dimethyl benzyl alcohol; and d) performing a reaction between the [alpha],[alpha]-dimethyl benzyl alcohol and hydrogen to generate isopropyl benzene, and feeding the isopropyl benzene back to the step a) as the raw material for producing the hydrogen peroxide isopropyl benzene. The method can solves technical problems and can be used in industrial production of the 3,4-epoxy-1-butylene.

Description

technical field [0001] The present invention relates to a method for producing 3,4-epoxy-1-butene. Background technique [0002] 3,4-epoxy-1-butene (EPB) is a new type of fine chemical intermediate, which is synthesized by epoxidation of 1,3-butadiene, and has broad market potential. , and double bonds, is a rare intermediate containing two important functional groups, and few organic intermediates have such a wide range of uses. However, for a long time due to high production costs, it has not received market attention. [0003] Starting from 3,4-epoxy-1-butene, hundreds of important follow-up products can be prepared, involving various fields such as bulk chemicals, fine chemicals and specialty chemicals, and are various pharmaceutical intermediates and chiral compounds , new flame retardants, and the best synthetic raw materials for functional polymer materials are fine chemicals that are in short supply at home and abroad. For example, starting from 3,4-epoxy-1-butene...

Claims

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Application Information

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IPC IPC(8): C07D301/19C07D303/04
Inventor 金国杰康陈军高焕新杨洪云黄政丁琳
Owner CHINA PETROLEUM & CHEM CORP
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