Preparation method of tert-butyl hydroperoxide

A technology of tert-butyl hydroperoxide and tert-butanol, which is applied in the direction of preparation of peroxy compounds, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of harmful emissions and high yield of tert-butyl hydroperoxide, etc. Achieve the effect of simple production process, high yield, and overcome the complex production process

Active Publication Date: 2013-07-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] Compared with the traditional method, the method provided by the present invention overcomes the problems of complex traditional production process, equipment corrosion, and harmful...

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  • Preparation method of tert-butyl hydroperoxide
  • Preparation method of tert-butyl hydroperoxide

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preparation example Construction

[0010] In the preparation method provided by the present invention, it can be realized under solvent-free conditions. The inventors found that the reaction performance can be improved when a certain solvent is introduced during the implementation process. Therefore, in the preparation method provided by the present invention, a solvent can also be introduced as required, and the solvent is preferably introduced. Described solvent is selected from the ketones such as methanol, ethanol or acetone, methyl ethyl ketone or the nitriles such as acetonitrile, propionitrile, benzyl nitrile or their mixture, preferably acetonitrile, acetone, methanol or their mixture, more preferably acetone, methanol and / or acetonitrile.

[0011] In the method provided by the present invention, the preferred ratio of raw materials is as follows: the molar ratio of tert-butanol to oxidant is preferably 1:1-5, and the mass ratio of solvent to catalyst is preferably 0-150:1. The amount between the raw m...

Embodiment 1

[0030] The mol ratio of tert-butanol, hydrogen peroxide, solvent and catalyst (molar ratio 0.2: 1 of titanium silicon molecular sieve and zinc nitrate) is 1: 2 according to the mol ratio of tert-butanol and hydrogen peroxide, and the mass ratio of solvent acetonitrile and catalyzer is 20:1, the mass ratio of tert-butanol to catalyst is 10:1, and the reaction is carried out at a temperature of 50° C. and a pressure of 1.5 MPa. The results of the reaction for 2 hours were as follows: the conversion rate of tert-butyl alcohol was 34%; the selectivity of tert-butyl hydroperoxide was 94%.

Embodiment 2

[0032] The mol ratio of tert-butanol, hydrogen peroxide, solvent and catalyst (molar ratio 1: 1 of titanium silicon molecular sieve and zinc phosphate) is 1: 3 according to the mol ratio of tert-butanol and hydrogen peroxide, and the mass ratio of solvent acetone and catalyzer is 50:1, the mass ratio of tert-butanol to catalyst is 20:1, and the reaction is carried out at a temperature of 60° C. and a pressure of 2.5 MPa. The results of the reaction for 2 hours were as follows: the conversion rate of tert-butyl alcohol was 45%; the selectivity of tert-butyl hydroperoxide was 96%.

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Abstract

The invention discloses a preparation method of tert-butyl hydroperoxide. Under oxidation reaction conditions, tert-butyl alcohol, an oxidant, a solvent and a catalyst are subjected to mixed contact. The method is characterized in that the catalyst is a soluble zinc salt modified heteroatom molecular sieve.

Description

technical field [0001] The present invention relates to a method for preparing tert-butyl hydroperoxide, and more particularly to a method for catalytically oxidizing tert-butyl alcohol to prepare tert-butyl hydroperoxide. Background technique [0002] Tert-butyl hydroperoxide is a colorless transparent or yellow liquid, which is miscible with organic solvents such as ethanol and ether. It is stable below 75°C, loses oxygen at 90-100°C, and explodes at 250°C. Tert-butyl hydroperoxide is mainly used as a catalyst for polymerization reactions, and as an introduction agent for peroxide groups in substituent reactions. It is used for dyeing and printing cotton, viscose, silk, nylon and other fibers and their fabrics. Used for polyester / viscose blended fabric dyeing. Tert-butyl hydroperoxide can also be used as a drying agent for unsaturated melamine resin coatings, a polymerization initiator, and an intermediate in organic synthesis. The existing preparation methods mainly in...

Claims

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Application Information

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IPC IPC(8): C07C409/04C07C407/00
Inventor 林民史春风朱斌汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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