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Multiphase catalytic oxidation cyclohexane catalyst for cyclohexanone and cyclohexanol and preparation method thereof

A heterogeneous catalyst and catalytic oxidation technology are applied in the preparation of oxidation reaction, chemical instruments and methods, preparation of organic compounds, etc., which can solve the problems of high price, clogging of the reactor, and high price, and achieve high conversion rate of cyclohexane, Mild reaction conditions and low-cost effects

Inactive Publication Date: 2008-06-25
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the performance of this type of catalyst is unstable, the synthesis of the catalyst is difficult, and the price is relatively high.
Using a homogeneous catalyst to oxidize cyclohexane to KA oil, the common problem is that it is difficult to separate and recycle the catalyst and the reaction mixture after the reaction, resulting in viscous black oil and the resulting clogging of the reactor and residual catalyst A series of problems affecting the downstream process
However, this type of catalyst is expensive due to the use of noble metal elements, which limits its industrial application.

Method used

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  • Multiphase catalytic oxidation cyclohexane catalyst for cyclohexanone and cyclohexanol and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: The ZSM-5 (silicon-aluminum ratio is 50) powder that takes 2g joins in the copper nitrate solution that 40ml concentration is 0.1mol / L, stirs at room temperature for 3 hours, then leaves standstill for 5 hours, centrifuges After separation, the solid sample was dried at 90°C, and then baked in a high-temperature furnace at 400°C for 2.5 hours. Cu-ZSM-5 with a Cu content of 2.1% was prepared.

[0025] 10 ml of cyclohexane, 10 ml of acetic acid, 1 ml of butanone, and 0.02 g of the Cu-ZSM-5 catalyst prepared above were added to a 50 ml tank reactor. Molecular oxygen was introduced to keep the pressure at 0.85 MPa, the reaction temperature was 130° C., and the reaction time was 5 hours. Reaction result: the conversion rate of cyclohexane is 4.88%, the selectivity of cyclohexanone is 56.10%, the selectivity of cyclohexanol is 9.60%, the rest is cyclohexanol acetate, and no carbon dioxide and black oil are produced.

Embodiment 2

[0026] Embodiment 2: The ZSM-5 (silicon-aluminum ratio is 50) powder that takes 2g joins in the cobalt nitrate solution that 40ml concentration is 0.05mol / L, stirs at room temperature for 3 hours, then leaves standstill for 5 hours, centrifuges After separation, the solid sample was dried at 90°C, and then baked in a high-temperature furnace at 400°C for 2.5 hours. Co-ZSM-5 with a Co content of 1.8% was prepared.

[0027] 10 ml of cyclohexane, 10 ml of acetic acid, 1 ml of butanone, and 0.02 g of the Co-ZSM-5 catalyst prepared above were added into a 50 ml tank reactor. Molecular oxygen was introduced to keep the pressure at 1.2 MPa, the reaction temperature was 110° C., and the reaction time was 10 hours. Reaction results: the conversion rate of cyclohexane is 4.23%, the selectivity of cyclohexanone is 59.40%, the selectivity of cyclohexanol is 9.42%, the rest is cyclohexanol acetate, and no carbon dioxide and black oil are produced.

Embodiment 3

[0028] Embodiment 3: the ZSM-5 (silicon-aluminum ratio is 50) powder that takes 2g joins in the ferric nitrate solution that 40ml concentration is 0.1mol / L, is placed on stirring at room temperature 3 hours, then leaves standstill 5 hours, After centrifugal separation, the solid sample was dried at 90°C, and then baked in a high-temperature furnace at 400°C for 2.5 hours. Using the obtained Fe-ZSM-5 as a starting material, add ferric nitrate solution, repeat the preparation procedure once according to the aforementioned conditions and steps, and obtain Fe-ZSM-5 with an Fe content of 1.9%.

[0029] 10 ml of cyclohexane, 10 ml of acetic acid, 1 ml of butanone, and 0.02 g of the Fe-ZSM-5 catalyst prepared above were added to a 50 ml tank reactor. Molecular oxygen was introduced to keep the pressure at 0.5 MPa, the reaction temperature was 150° C., and the reaction time was 5 hours. . The reaction results are as follows: the conversion rate of cyclohexane is 2.55%, the selectivi...

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Abstract

The invention provides a heterogeneous catalysis used for preparing cyclohexanone and cyclohexanol by catalytic oxidation of cyclonexane and a preparation method thereof. The technical process thereof is that: according to a certain proportion, a carrier is mixed with a certain proportion of active metal nitrate solution. The carrier is aluminosilicate molecular sieve or silicon dioxide. The active metal is one or more transition metal element of IVB-VIIIB Group. The mixture is stirred for 1 to 3 hours at room temperature and then treated with standing impregnation for 5 to 12 hours, or stirred back flow at boiling temperature for 5 to 8 hours. The catalyst with active metal is obtained by that a supernatant is removed and a filter cake is dried at 80 to 120 DEG C, baked at 400 to 600 DEG C for 2 to 6 hours. The catalyst of the invention has the advantages of low price, gentle reaction condition, and high conversion efficiency of cyclonexane; cyclohexanol and cyclohexanone are with good selectivity; no carbon dioxide or black oil is generated from the reaction process; the catalyst is easily separated from reaction system after reaction.

Description

technical field [0001] The invention relates to a heterogeneous catalyst used in the process of preparing cyclohexanone and cyclohexanol by cyclohexane oxidation and a preparation method thereof. Background technique [0002] The oxidation of cyclohexane to cyclohexanone and cyclohexanol (referred to as KA oil) is an important representative of the industrial process of alkane oxidation, and its oxidation product cyclohexanone is mainly used as the raw material for the production of nylon-6 and nylon-66 caprolactam and adipic acid intermediate. At the same time, KA oil is also an important industrial solvent, and is used in resins, polyurethane foams, medicines, paints, coatings, rubber, plasticizers, pesticides, advanced lubricants, adhesives, synthetic leather materials, synthetic dyes, spices, yeast purification, etc. Industrial processes as well as in printing and plastic recycling have extremely wide applications. [0003] At present, there are three main industrial p...

Claims

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Application Information

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IPC IPC(8): B01J29/064B01J29/42C07C27/12C07C29/50C07C35/08C07C45/32C07C49/11
Inventor 晁自胜梁海军凡美莲付薪菱黄彩娟袁渭康
Owner HUNAN UNIV
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