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A kind of method for preparing tert-butyl hydroperoxide by oxidation of isobutane

A technology of tert-butyl hydroperoxide and isobutane, which is applied to the preparation of peroxide compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of reaction temperature, high pressure, low conversion rate of isobutane, TBHP Instability and other problems, to achieve the effect of mild reaction conditions, high catalytic activity, and cost saving of raw materials

Active Publication Date: 2019-04-16
HUIZHOU YUSSEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent US4059598 discloses that under the reaction conditions of 137°C and 3.15MPa, isobutane and molecular oxygen generate TBHP and TBA, the selectivities are 53.4% ​​and 40.2% respectively, and the conversion rate of isobutane is 36.9%. Friendly, but it needs to be carried out under high temperature and high pressure, the equipment cost is high, and TBHP is unstable when it is above 75°C, it is easy to decompose, there are safety hazards, and the device capacity is low
Patent US4408082 has studied that in the direct oxidation reaction of isobutane, adding very little oxygen (less than 0.1% molar ratio) will speed up the reaction rate and improve the selectivity of TBHP. The reaction temperature is 140-170 ° C, and the reaction pressure is higher than that of isobutane. Butane critical pressure, isobutane conversion rate of 20%, this method also has the problem of high reaction temperature and pressure, and low isobutane conversion rate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dissolve 0.7g of catalyst NHPI and 0.1g of β-cyclodextrin (β-CD) in 17.4g of acetonitrile to obtain solution A, and add solution A into the autoclave. 17.4 g of isobutane cooling liquid under normal temperature and back pressure state was passed through. After being airtight, the temperature was raised to 75°C, and oxygen was continuously fed in with isobutane and oxygen at a molar ratio of 1:1 and stirred to carry out the isobutane oxidation reaction. The results of the reaction for 4 hours were as follows: the conversion rate of isobutane was 12.4%, and the tert-butyl The selectivity of hydrogen peroxide is 60.1%, and the selectivity of tert-butanol is 37.2%.

Embodiment 2

[0030] Dissolve 0.7g of catalyst NHPI and 0.1g of β-cyclodextrin (β-CD) in 13.9g of acetonitrile to obtain solution A, and add solution A into the autoclave. 17.4 g of isobutane cooling liquid under normal temperature and back pressure state was passed through. After being airtight, the temperature was raised to 75°C, and oxygen was continuously fed in with isobutane and oxygen at a molar ratio of 2:1 and stirred to carry out the isobutane oxidation reaction. The results of the reaction for 4 hours were as follows: the conversion rate of isobutane was 15.5%, and the tert-butyl The selectivity of hydrogen peroxide is 55.2%, and the selectivity of tert-butanol is 42.8%.

Embodiment 3

[0032] Dissolve 0.7g of catalyst NHPI and 0.28g of β-cyclodextrin (β-CD) in 17.4g of ethanol to obtain solution A, and add solution A into the autoclave. 17.4 g of isobutane cooling liquid under normal temperature and back pressure state was passed through. After being airtight, the temperature was raised to 75°C, and oxygen was continuously fed in with isobutane and oxygen at a molar ratio of 2:1 and stirred to carry out the isobutane oxidation reaction. The results of the reaction for 4 hours were as follows: the conversion rate of isobutane was 20.4%, and the tert-butyl The selectivity of hydrogen peroxide is 42.1%, and the selectivity of tert-butanol is 54.9%.

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PUM

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Abstract

The invention discloses a method used for preparing tert-butyl hydroperoxide via oxidation of isobutane. The method comprises following steps: a, N-hydroxyphthalimide (NHPI) is taken as a catalyst, beta-cyclodextrin is taken as a catalyst modifier, and the catalyst and the catalyst modifier are dissolved in a polar organic solvent so as to obtain a solution A; b, the solution A is delivered into a high pressure reaction kettle which is provided with a stirrer; c, liquid phase isobutane is introduced into the high pressure reaction kettle at normal pressure backpressure; d, the temperature in the high pressure reaction kettle is increased to a needed temperature, and then oxygen is introduced into the high pressure reaction kettle; e, at a certain reaction pressure and a certain temperature, oxidation of isobutane is carried out so as to obtain tert-butyl hydroperoxide. According to the method, NHPI is taken as a catalyst; conversion rate and selectivity are high; the method is friendly to the environment; beta-CD is taken as the catalyst modifier, so that catalyst activity is increased; and the conversion of isobutane is increased obviously without influencing the selectivity.

Description

technical field [0001] The invention relates to a method for preparing tert-butyl hydroperoxide, in particular to a method for preparing tert-butyl hydroperoxide by oxidation of isobutane. Background technique [0002] Isobutane mainly comes from catalytic cracking units or ethylene production units. my country is rich in isobutane resources. At present, it is mainly used as industrial or civil fuel with low added value. How to make full use of excess isobutane resources has become a top priority. [0003] Tert-butyl hydroperoxide (abbreviated as TBHP) is an important branch of peroxides, mainly used as initiators for polymerization reactions (such as polyvinyl chloride, polyacrylic emulsion polymerization, monomer elimination, etc.), unsaturated polyester It is also widely used in the synthesis of other organic peroxides as a crosslinking agent, emulsion polymerization, natural coke sulfur addition, diesel additives, paint industry, etc. [0004] The production methods of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C407/00C07C409/04
CPCC07C407/00C07C409/04
Inventor 夏志强余良军湛明
Owner HUIZHOU YUSSEN CHEM CO LTD
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