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Cyclohexyl-hydrogen-peroxide-free cyclohexane oxidation liquid deacidification method for alkali liquid circulation

A technology of cyclohexane oxidation liquid and cyclohexane, which is applied in chemical instruments and methods, purification/separation of oxygenated compounds, preparation of organic compounds, etc., can solve the problem of consumption of NaOH, alkali cannot be closed and recycled, and the formation of large Alkali slag and other problems

Inactive Publication Date: 2016-06-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, there is the technical problem that the alkali used cannot be closed and recycled in the existing technology. In addition to consuming a large amount of NaOH in production, and forming a large amount of alkali slag

Method used

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  • Cyclohexyl-hydrogen-peroxide-free cyclohexane oxidation liquid deacidification method for alkali liquid circulation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 50 g of cyclohexane oxidation solution without passing through and 1.22 g of 15% sodium carbonate aqueous solution into a 100 ml reaction flask, stir and neutralize at 60° C. for 5 minutes. The aqueous solution of the lower layer was separated at rest, and the pH value of the lower layer solution was detected to be 9.1. The solution was evaporated in an oil bath at 120° C. to a concentration of 55%, and then calcined at 600° C. in air for 1 hour to obtain 0.19 g of off-white powder.

[0036] The separated upper organic solution was analyzed by GC for the contents of cyclohexanol and cyclohexanone, and the results are shown in Table 1.

Embodiment 2

[0038] The white powder obtained in Example 1 was dissolved in 0.76 g of water to make a suspension with a concentration of 20%, and filtered with filter paper to obtain clarified lye. Add 50 grams of cyclohexane oxidation solution and the filtered lye sodium carbonate solution to the 100 ml reaction bottle, and stir and neutralize at 80° C. for 5 minutes. The aqueous solution of the lower layer was separated at rest, and the pH value of the lower layer solution was detected to be 9.5. The solution was evaporated in an oil bath at 120° C. to a concentration of 50%, and then calcined at 700° C. in air for 1 hour to obtain 0.20 g of off-white powder.

[0039] The separated upper organic solution was analyzed by GC for the contents of cyclohexanol and cyclohexanone, and the results are shown in Table 1.

Embodiment 3

[0041] The white powder obtained in Example 2 was dissolved in 0.80 g of water to make a suspension with a concentration of 20%, and filtered with filter paper to obtain clarified lye. Add 50 grams of cyclohexane oxidation solution and the filtered lye sodium carbonate solution to the 100 ml reaction bottle, and stir and neutralize at 80° C. for 5 minutes. The aqueous solution of the lower layer was separated at rest, and the pH value of the lower layer solution was detected to be 9.5. The solution was evaporated in an oil bath at 120° C. to a concentration of 50%, and then calcined at 800° C. in air for 1 hour to obtain 0.21 g of off-white powder.

[0042] The separated upper organic solution was analyzed by GC for the contents of cyclohexanol and cyclohexanone, and the results are shown in Table 1.

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Abstract

The present invention relates to a cyclohexyl-hydrogen-peroxide-free cyclohexane oxidation liquid deacidification method for alkali liquid circulation. The method specifically comprises: mixing an alkali liquid and a cyclohexyl-hydrogen-peroxide-free cyclohexane oxidation liquid, carrying out standing separation to obtain a neutralized waste alkali liquid, and carrying out evaporation concentration, calcination, dissolution and filtration on the waste alkali liquid so as to achieve the alkali liquid circulation during the oxidation liquid deacidification treatment process after the alkali-free catalytic decomposition of cyclohexyl hydrogen peroxide, wherein the cyclohexyl-hydrogen-peroxide-free cyclohexane oxidation liquid is the cyclohexane oxidation liquid obtained by decomposing cyclohexyl hydrogen peroxide according to the cyclohexyl hydrogen peroxide decomposition technology in the patent CN201010284602.6, and the cyclohexane oxidation liquid is derived from the non-catalytic cyclohexane air oxidation method. According to the present invention, the method for alkali-free catalytic decomposition of the cyclohexyl hydrogen peroxide is developed, such that the new alkali neutralization technology is required to be researched and is combined with the patent CN201010284602.6 alkali-free catalytic decomposition of the cyclohexyl hydrogen peroxide so as to remove the organic acid in the obtained oxidation liquid, and the problems of alkali use efficiency and the alkali residue emission eliminating are solved so as to achieve alkali circulation, eliminate alkali residue emission and eliminate net alkali consumption.

Description

technical field [0001] The present invention relates to the development and application of a new process in the field of petrochemical industry, in particular to the development of a new process for the deacidification of a cyclohexane oxidized liquid without cyclohexyl hydroperoxide by circulation of lye, through neutralization The raw material cost for producing cyclohexanone and cyclohexanol is reduced by the regeneration cycle of alkali. Background technique [0002] The oxidation of cyclohexane to produce cyclohexanol and cyclohexanone is an important petrochemical process for the production of caprolactam and adipic acid. Cyclohexane is firstly oxidized by air to obtain an oxidized solution containing cyclohexyl hydroperoxide. This oxidized solution must undergo a further decomposition reaction to decompose the cyclohexyl hydroperoxide into final cyclohexanol and cyclohexanone. In the oxidation reaction of cyclohexane and the decomposition reaction of cyclohexyl hydro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/26C07C29/88C07C45/85C07C35/08C07C49/403
Inventor 孙志强徐杰马红石松苗虹郑玺高进
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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