Preparation method of high-crystallinity hierarchical pore molecular sieve

A high crystallinity, molecular sieve technology, used in molecular sieve catalysts, molecular sieves and alkali exchange compounds, carbon monoxide or formate reaction preparation, etc., to improve thermal stability, crystallinity and acid strength, improve heat and mass transfer. The effect of efficiency

Inactive Publication Date: 2019-02-22
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, there is no report in the literature on the use of hierarchically porous molecular sieves op

Method used

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  • Preparation method of high-crystallinity hierarchical pore molecular sieve
  • Preparation method of high-crystallinity hierarchical pore molecular sieve
  • Preparation method of high-crystallinity hierarchical pore molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] At 100 °C, 5 g HY was soaked in 0.1 mol L-1 H4EDTA solution (100 mL), stirred and refluxed for 6 h, and then dried and roasted to obtain HY-DAl0.10. 3g of HY-DAl0.10 was treated in a mixed solution of 0.1 mol L-1 tetrapropylammonium bromide (TPABr) and 0.1 mol L-1 NH4OH for 1 h, washed with water until neutral, and dried at 120 °C for 8 h. Calcined at 550°C for 6 h to remove the template agent to obtain HY-DAl0.10-DSiNH4OH0.10+TPABr0.10.

[0027] In the fixed-bed reactor, 1.0 g of the catalysts prepared above were charged respectively, and the pressure in the reaction tube was 5 MPa. CO (99.9999%) with a flow rate of 50mL / min is mixed into the reaction tube through a stainless steel reaction tank filled with methylal (DMM) (98wt%) at room temperature (25°C), and the saturated vapor of DMM is mixed into the reaction tube by adjusting the back pressure valve To keep the reaction tube pressure constant. The reaction temperature was 90-120°C, and the reaction product was ...

Embodiment 2

[0032]At 100°C, 5 g HY was soaked in 0.1 mol L-1 H4EDTA solution (100 mL), stirred and refluxed for 6 h, and then dried and roasted to obtain HY-DAl0.10. 3g of HY-DAl0.10 was treated in a mixed solution of 0.1 mol L-1PDA (TMAOH, TEAOH, TPAOH, TBAOH) and 0.1 mol L-1 NH4OH for 1 h, washed with water until neutral, and dried at 120 °C for 8 h. Calcined at 550°C for 6 h to remove the template to obtain HY-DAl0.10-DSiNH4OH0.10+PDA0.10.

[0033] In the fixed-bed reactor, 1.0 g of the catalysts prepared above were charged respectively, and the pressure in the reaction tube was 5.0 MPa. CO (99.9999%) with a flow rate of 50mL / min is mixed into the reaction tube through a stainless steel reaction tank filled with methylal (DMM) (98wt%) at room temperature (25°C), and the saturated vapor of DMM is mixed into the reaction tube by adjusting the back pressure valve To keep the reaction tube pressure constant. The reaction temperature was 100 °C, and the reaction products were analyzed onl...

Embodiment 3

[0038] At 100°C, 5 g HY was soaked in 0.1 mol L-1 H4EDTA solution (100 mL), stirred and refluxed for 6 h, and then dried and roasted to obtain HY-DAl0.10. Take 3g of HY-DAl0.10 and treat it in the mixed solutions with concentrations of 0.01, 0.02, 0.05, 0.1, 0.2 mol L-1TPAOH and 0.1 mol L-1 NH4OH for 1 h, wash with water until neutral, and dry at 120°C for 8 h, calcination at 550°C for 6 h to remove the template agent to obtain HY-DAl0.10-DSiNH4OH0.10+PDAy.

[0039] In the fixed-bed reactor, 1.0 g of the catalysts prepared above were charged respectively, and the pressure in the reaction tube was 5.0 MPa. CO (99.9999%) with a flow rate of 50mL / min is mixed into the reaction tube with saturated steam of DMM through a stainless steel reaction tank filled with methylal (DMM) (98wt%) at room temperature (25°C), and adjusted by adjusting the back pressure valve To keep the reaction tube pressure constant. The reaction temperature was 100 °C, and the reaction products were analyze...

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Abstract

The invention discloses a preparation method of a high-crystallinity hierarchical pore molecular sieve and relates to a preparation method of a molecular sieve catalyst. According to the preparation method disclosed by the invention, an organic guide agent is added in the conventional acid and base desilicication and dealumination process and achieves the effects of molecular sieve pore channel supporting and porous structure optimizing, and acid strength and acid distribution in the molecular sieve pore channel are effectively optimized. The crystallinity and acid strength of the modified molecular sieve are obviously improved, and the molecular sieve has large pore diameter and mesoporous-microporous composite structure, and the structure obviously promotes the mass transfer efficiency of the heavy component product. The prepared high-crystallinity large-pore diameter hierarchical pore HY molecular sieve is used for methylal carbonylation reaction for preparing high-value-added methyl methoxyacetate, and when the reaction pressure is 5.0 MPa and the reaction temperature is 100 DEG C, the methylal conversion rate is close to 100%, the methyl methoxyacetate selectivity is higher than 95%, and the catalyst does not have obvious inactivation during stability evaluation of 1000 hours.

Description

technical field [0001] The invention relates to a method for preparing a molecular sieve catalyst, in particular to a method for preparing a molecular sieve with high crystallinity and hierarchical pores. Background technique [0002] Methyl methoxyacetate (MMAc) is an important organic chemical raw material, which can be used for the kinetic resolution of chiral amine compounds, the synthesis of vitamin B6 and sulfa-5-pyrimidine, etc., as a catalyst for polymerization reactions; at the same time, MMAc It is the upstream product of non-petroleum route (use cheap and easy-to-obtain methylal as the reaction raw material, and synthesize high value-added MMAc through carbonylation reaction) to produce bulk chemical raw material ethylene glycol (generate ethylene glycol monomethyl ether through hydrogenation reaction, Then through hydrolysis reaction to generate ethylene glycol), ethylene glycol is mainly used in the production of polyester fiber, antifreeze, unsaturated polyeste...

Claims

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Application Information

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IPC IPC(8): C01B39/00C01B39/24C01B39/38B01J29/08C07C67/37C07C69/708
CPCC01B39/026B01J29/084B01J37/0018C01B39/24C01B39/38C07C67/37C07C69/708
Inventor 石磊张冬喜王岩李新钰
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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