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Preparation method of molecular sieve for cyclohexane catalytic oxidation

A catalytic oxidation and molecular sieve technology, applied in the chemical industry, can solve the problems of large residue discharge, low resource utilization rate, less than 5%, and achieve the effect of increasing specific surface area, large specific surface area, and easy operation

Inactive Publication Date: 2018-08-24
ANHUI HAIDE PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, cobalt salts are mainly used as catalysts or no catalysts are used in industry for the catalytic oxidation of cyclohexane. The conversion rate of cyclohexane is less than 5%, and the total selectivity of cyclohexanone and cyclohexanol is about 78%. Technology leads to low resource utilization and large residue emissions. Therefore, the traditional catalytic oxidation process is difficult to meet the needs of sustainable development of human beings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of molecular sieves for catalytic oxidation of cyclohexane:

[0025] (1) 10kg of petroleum coke is pulverized through a 40-mesh sieve, and 6.52L of 90-98wt% H is added to the sieved petroleum coke powder 2 SO 4 solution, stirred and mixed for 30min, then filtered, and the filter residue was washed with deionized water until the pH value of the filtrate was 6.5, and then the filter residue was vacuum-dried to constant weight;

[0026] (2) Methyl orthosilicate, tin sulfate, tetraethylammonium hydroxide, sodium sulfate and water are mixed in proportion to obtain a molar ratio of SiO 2 : Sn: Tetraethylammonium hydroxide: Sodium sulfate: H 2 O=1:0.05:3.5:0.8:80 reaction mixture, then add sodium hydroxide solution to the reaction mixture to adjust the pH value to 10.5, then carry out the initial crystallization of the reaction mixture, keep the temperature of the reaction mixture at 130°C, crystallize The reaction time was 3 days, and the primary cryst...

Embodiment 2

[0030] A preparation method of molecular sieves for catalytic oxidation of cyclohexane:

[0031] (1) 10kg of petroleum coke is pulverized through a 40-mesh sieve, and 7.6L of 90-98wt% H is added to the sieved petroleum coke powder 2 SO 4 solution, stirred and mixed for 40min, then filtered, and the filter residue was washed with deionized water until the pH value of the filtrate was 7.0, and then the filter residue was vacuum-dried to constant weight;

[0032] (2) Methyl orthosilicate, tin sulfate, tetraethylammonium hydroxide, sodium sulfate and water are mixed in proportion to obtain a molar ratio of SiO 2 : Sn: Tetraethylammonium hydroxide: Sodium sulfate: H 2 O=1:0.01:2.3:0.005:50 reaction mixture, then add sodium hydroxide solution to the reaction mixture to adjust the pH value to 9.0, then carry out the initial crystallization of the reaction mixture, keep the temperature of the reaction mixture at 120°C, crystallize The reaction time was 2 days, and the primary cryst...

Embodiment 3

[0036] A preparation method of molecular sieves for catalytic oxidation of cyclohexane:

[0037] (1) 10kg of petroleum coke is pulverized through a 40-mesh sieve, and 8.1L of 90-98wt% H 2 SO 4 solution, stirred and mixed for 30min, then filtered, and the filter residue was washed with deionized water until the pH value of the filtrate was 6.5, and then the filter residue was vacuum-dried to constant weight;

[0038] (2) Methyl orthosilicate, tin sulfate, tetraethylammonium hydroxide, sodium sulfate and water are mixed in proportion to obtain a molar ratio of SiO 2 : Sn: Tetraethylammonium hydroxide: Sodium sulfate: H 2 O=1:0.1:4.7:1.5:100 reaction mixture, then add sodium hydroxide solution to the reaction mixture to adjust the pH value to 11.5, and then carry out the initial crystallization of the reaction mixture, keep the temperature of the reaction mixture at 150°C, crystallize The reaction time was 3 days, and the primary crystallization product was obtained;

[0039]...

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Abstract

The invention relates to the technical field of chemical engineering, and in particular relates to a preparation method of a molecular sieve for cyclohexane catalytic oxidation. The preparation methodcomprises the following steps: (1) pretreating petroleum coke; (2) mixing a silicon source, a tin source, a structure guiding agent, a mineralizer and water according to a ratio, adding an alkaline substance, and conducting primary crystallization; (3) dispersing the silicon source into water, dropwise adding a precipitant to form amorphous sol, and carrying out secondary crystallization; (4) adding a binding agent, a binding assistant and water into the filter residue and the secondary crystallization product for kneading and forming, roasting the formed object, and then conducting crushingand sieving to obtain the molecular sieve. The composite molecular sieve is formed by the silicon-tin and petroleum coke carbonization, and the silicon in the silicon source is reduced by the carbon rich in the petroleum coke, and a pore structure is filled with silicon carbide with high hardness, meanwhile gas is released, and the pore structure is prevented from being reduced, so that the obtained molecular sieve has a relatively large specific surface area and the catalytic activity is improved.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a method for preparing molecular sieves used for catalytic oxidation of cyclohexane. Background technique [0002] Cyclohexane, also known as hexahydrobenzene, has always been a very important process product in petrochemical and fine chemical industries, and the selective oxidation of cyclohexane is of great significance in chemical production. Under the oxidation reaction with oxygen, the main products are cyclohexanol and cyclohexanone. Because cyclohexanol and cyclohexanone are easier to oxidize than cyclohexane, not only adipic acid, but also ε-caprolactone, 6-hydroxy By-products such as hexanoic acid are formed. In order to improve the selectivity and yield of products and reduce the formation of by-products, it is necessary to try to control the conversion rate of cyclohexane. At present, cobalt salts are mainly used as catalysts or no catalysts are used in ...

Claims

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Application Information

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IPC IPC(8): B01J29/00C07C51/285C07C55/14
CPCB01J29/005B01J2229/183C07C51/285C07C55/14
Inventor 黄帮义
Owner ANHUI HAIDE PETROCHEM
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