Preparation method for nanoscale composite structure molecular sieve

A composite structure and molecular sieve technology, applied in molecular sieves and base exchange compounds, nanotechnology, nanotechnology, etc., can solve the problems of molecular sieve catalytic performance degradation, achieve high activity and anti-carbon deposition ability, simplify synthesis process, and widely distribute acidity Effect

Inactive Publication Date: 2019-04-12
江苏黄马化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If it is applied in the cyclohexene hydration reaction, the cyclohexanol obtained from the reaction will react further and generate by-products such as dicyclohexyl ether, which will be adsorbed in the pores of the molecular sieve, and the catalytic performance of the molecular sieve will be reduced. A sharp decline

Method used

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  • Preparation method for nanoscale composite structure molecular sieve
  • Preparation method for nanoscale composite structure molecular sieve
  • Preparation method for nanoscale composite structure molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of molecular sieve with nanoscale composite structure, comprising the following steps:

[0028] (1) Add 1391g deionized water into the beaker, start stirring, add 60.9g sodium hydroxide, stir to dissolve, add 65.28g aluminum sol (AL2O3 content 25%), after stirring for 25min, slowly add 600g silica sol (SiO2 content 40%) %), the mixture sol was obtained after stirring for 2h;

[0029] (2) Transfer the mixture sol obtained in step (1) into a high-pressure crystallization kettle. The crystallization adopts a temperature program, and the temperature is raised to 168°C in 8 hours. After 24 hours at a constant temperature, the temperature is lowered and cooled. The value is 9;

[0030] (3) Mix the pre-configured 1800ml, 0.5mol / L sulfuric acid aqueous solution with the washed solid product, heat to 80°C, keep the temperature for 2h, filter and wash until the pH value is 4, stop at 120°C The molecular sieve with nanoscale composite structure is obtained b...

Embodiment 2

[0032] A preparation method of molecular sieve with nanoscale composite structure, comprising the following steps:

[0033] (1) Add 1756.3g deionized water into the beaker, start stirring, add 51.7g potassium hydroxide, stir to dissolve, add 58.29g aluminum sol (AL2O3 content 25%), stir for 30min, slowly add 600g silica sol (SiO2 content 40%), the mixture sol was obtained after stirring for 2 hours;

[0034] (2) Transfer the mixture sol obtained in step (1) into a high-pressure crystallization kettle. The crystallization adopts a temperature program, and the temperature is raised to 172°C in 8 hours. After 24 hours at a constant temperature, the temperature is lowered and cooled. value is 8;

[0035] (3) Mix the pre-configured 1800ml, 0.5mol / L sulfuric acid aqueous solution with the washed solid product, heat to 80°C, keep the temperature for 2h, filter and wash until the pH value is 5, stop it at 125°C The molecular sieve with nanoscale composite structure is obtained by dr...

Embodiment 3

[0037] A preparation method of molecular sieve with nanoscale composite structure, comprising the following steps:

[0038] (1) Add 1610.67g deionized water into the beaker, start stirring, add 57.35g sodium hydroxide, stir to dissolve, add 60.44g aluminum sol (AL2O3 content 25%), stir for 35min, slowly add 600g silica sol (SiO2 content 40%), the mixture sol was obtained after stirring for 2 hours;

[0039] (2) Transfer the mixture sol obtained in step (1) into a high-pressure crystallization kettle. The crystallization adopts a temperature program, and the temperature is raised to 166°C in 8 hours. After 24 hours at a constant temperature, the temperature is lowered and cooled. The value is 9;

[0040] (3) Mix the pre-configured 1800ml, 0.5mol / L sulfuric acid aqueous solution with the washed solid product, heat to 80°C, keep the temperature for 2h, filter and wash until the pH value is 4, stop it at 130°C The molecular sieve with nanoscale composite structure is obtained by...

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Abstract

The invention discloses a preparation method for a nanoscale composite structure molecular sieve. The preparation method includes the following steps that 1, an alkali source, a silicon source, an aluminum source and deionized water are uniformly mixed according to a certain mole ratio, so that mixture sol is obtained; 2, the mixture sol is transferred into a high-pressure crystallizing kettle, increased in temperature according to a program, then kept constant in temperature and cooled, a reactant is filtered to obtain a solid product, and washing is conducted until the pH value is smaller than or equal to 9; 3, after washing, the solid product is subjected to ion exchange treatment, after a reaction is ended, a solid product is obtained through filtering, washing is conducted until the pH value of the solid product is larger than or equal to 4, and through drying, the nanoscale composite structure molecular sieve is obtained. By adjusting the optimal mole ratio of the alkali source to the silicon source to the aluminum source to the deionized water, the nanoscale composite type zeolite molecular sieve with MOR and MFI topology structures can be obtained, and the composite structure molecular sieve is high in conversion rate of a catalytic reaction, has higher anti-carbon deposition capacity, and will not have remarkably-reduced activity after being used ten times constantly through recycling.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and in particular relates to a method for preparing molecular sieves with a nanoscale composite structure of MOR and MFI topology. Background technique [0002] As a widely used industrial raw material, cyclohexanol can be used as a stabilizer for water-soluble latex, and can also be used as a synthetic raw material for the production of adipic acid and caprolactam, monomers for polymerization, plasticizers, PVC and other resin stabilizers , but also a synthetic raw material for pesticides and herbicides. [0003] At present, the source of cyclohexanol is mostly obtained through cyclohexene hydration catalysis, and the cyclohexene hydration catalyst commonly used in industry is a molecular sieve with a composite structure. The technical process for preparing cyclohexanol as a catalyst, the small-grain ZSM-5 molecular sieve is prepared by using tetrapropylammonium bromide, ethyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/46B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B39/46C01P2004/80
Inventor 陶德志梁飞王晓鹏卢磊于新功李鹏博陈丹丹
Owner 江苏黄马化工有限公司
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