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Method and device for preparing hydrogen peroxide p-menthane by non-catalytic oxidation of p-menthane

A technology of hydrogen peroxide and p-menthane, which is applied in the non-catalytic oxidation of p-menthane to prepare hydrogen peroxide p-menthane and the field of equipment, which can solve the problem that the continuous menthane oxidation process is not widely used in industrial production, expensive catalyst loss, catalyst Cleaning is complicated and other problems, to achieve the effect of overcoming low production efficiency, easy control, and high effective utilization rate

Active Publication Date: 2018-06-12
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the method that Chinese patent application CN101225067A discloses catalytic air oxidation p-menthane to prepare hydrogen peroxide p-menthane, the method of adding catalyst liquid-phase oxidation p-menthane to obtain hydrogen peroxide p-menthane is introduced; Chinese patent application CN101962352A The continuous production method and device thereof for preparing hydrogen peroxide from menthane are disclosed in Menthane, but the continuous process of Menthane oxidation process is not widely used in industrial production, and large-scale industrial production mainly uses non-catalytic oxidation intermittent craft-based
Batch oxidation needs to re-add catalyst before adding the reaction raw materials each time. If the reaction is not separated and recovered at the end of the reaction, the residual catalyst will flow into the next section with the mixed liquid, reducing the purity of the product, causing the loss of expensive catalyst, and the waste liquid discharged at the same time also affect the environment
However, the removal of the catalyst requires a huge separation process, and the steps are quite complicated, requiring a lot of manpower, material and financial resources
In addition to gas-liquid oxidation, there is also a fixed-bed reaction process involving gas-liquid-solid three-phase, which puts strict requirements on the rational use of reaction equipment and the safety of production. At the same time, the cleaning of the catalyst is also a complicated step.

Method used

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  • Method and device for preparing hydrogen peroxide p-menthane by non-catalytic oxidation of p-menthane

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Effect test

Embodiment 1

[0018] At a temperature of 100°C and a pressure of 0.3 MPa, with oxygen as the oxidant, the alkaline washing solution NaCO 3 The mass fraction of the solution is 2%, the gas flow is 3 L / min, and the p-menthane and hydrogen peroxide are reacted at a molar ratio of 50:1 to p-menthane. The result of reacting for 5 hours is as follows: the conversion rate of p-menthane is 24%; the mass fraction of hydrogen peroxide to menthane is 19%.

Embodiment 2

[0020] At a temperature of 110°C and a pressure of 0.3 MPa, with oxygen as the oxidant, the alkaline washing solution NaCO 3 The mass fraction of the solution is 2%, the gas flow is 3 L / min, and the p-menthane and hydrogen peroxide are reacted at a molar ratio of 50:1 to p-menthane. The result of reacting for 5 hours is as follows: the conversion rate of p-menthane is 30%; the mass fraction of hydrogen peroxide to menthane is 20%.

Embodiment 3

[0022] At a temperature of 120°C and a pressure of 0.3 MPa, oxygen is used as an oxidant, the mass fraction of initiator hydrogen peroxide to menthane is 2%, and the ventilation rate is 3L / min. The reaction was carried out at a molar ratio of 50:1. The result of reacting for 5 hours is as follows: the conversion rate of p-menthane is 33%; the mass fraction of hydrogen peroxide to menthane is 23%.

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Abstract

The invention relates to a method and apparatus for non-catalytic air oxidation of liquid phase p-menthane to generate hydrogen peroxide p-menthane. The method is characterized in that: 0-3% of the product hydrogen peroxide p-menthane is adopted as the initiator, an alkaline solution is employed for continuous washing of inflow gas, and oxidation reaction is carried out at a temperature of 50DEG C-140DEG C and under a pressure of 0-0.5MPa. The method has the advantages of no use of catalyst, fast reaction speed, high product yield, and simplifies the follow-up complicated purification process.

Description

technical field [0001] The invention relates to a method and a device for preparing hydrogen peroxide p-menthane through non-catalytic oxidation of p-menthane. Background technique [0002] P-menthane (PM) is a fully saturated hydrogenated monocyclic monoterpenoid, which is generally obtained from forestry products by hydrogenation of dipentene. [0003] P-menthane hydroperoxide (PMHP) is an excellent initiator for the polymerization of olefins, such as butadiene and styrene. Compared with other organic hydroperoxides, PMHP has good performance, less dosage and excellent stability. It is widely used as an initiator for low-temperature emulsion polymerization of styrene-butadiene rubber. The industrial production of p-menthane hydroperoxide is mainly Air oxidation of Menthane. [0004] In the method that Chinese patent application CN101225067A discloses catalytic air oxidation p-menthane to prepare hydrogen peroxide p-menthane, the method of adding catalyst liquid-phase oxi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C407/00C07C409/14C07C409/06
Inventor 孙伟振赵玲许志美刘明鑫
Owner EAST CHINA UNIV OF SCI & TECH
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