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Preparation method of nano-sized ael structure molecular sieve

A nano-sized, molecular sieve technology, applied in the direction of molecular sieve characteristic aluminum phosphate, molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of harsh synthesis conditions and hinder growth, and achieve the effect of high specific surface area

Active Publication Date: 2017-09-01
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Microwave synthesis can strengthen the decomposition of gel by introducing microwave heating, so that the number of crystal nuclei reaches a state close to saturation in a short period of time, and the subsequent crystallization speed is accelerated, and the particle size of the synthesized molecular sieve can also be controlled. The crystallinity is high, and the low-temperature aging procedure necessary for the conventional heating method can be omitted, but its synthesis conditions are relatively harsh, and the space-confined method confines the molecular sieve to a limited space, hindering its growth and preventing the aggregation of its grains

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The following raw materials are proportioned according to the molar ratio, pseudo-boehmite, Al 2 o 3 Calculated; heteroatom source, denoted as M, calculated as oxide; phosphoric acid, expressed as P 2 o 5 count;

[0021] Pseudoboehmite: phosphoric acid: di-n-propylamine = 1.0: 1.0: 1.0;

[0022] After mixing with deionized water and stirring for 30 minutes, adjust the pH value of the system to 5.5, then freeze-dry the obtained colloid at -80°C for 1 day to prepare dry glue; crystallize the obtained dry glue at 160°C for 54 hours in an autoclave Finally, the crystallized product was obtained; it was washed and filtered with deionized water 6 times the mass of the crystallized product, then dried at 100°C for 4 hours, and then calcined at 550°C for 4 hours to obtain the AlPO- 11 Molecular sieves with a particle size of 100nm and a specific surface area of ​​250m 2 / g.

Embodiment 2

[0024] The following raw materials are proportioned according to the molar ratio, pseudo-boehmite, Al 2 o 3 Calculated; Heteroatom source magnesium chloride, calculated as MgO; Phosphoric acid, calculated as P 2 o 5 count;

[0025] Pseudoboehmite: magnesium chloride: phosphoric acid: di-n-propylamine=0.8:0.15:1.0:1.1;

[0026] After mixing with deionized water and stirring for 20 minutes, adjust the pH value of the system to 7.0, then freeze-dry the obtained colloid at -70°C for 2 days to prepare dry glue; crystallize the obtained dry glue at 160°C in an autoclave for 72 hours Finally, the crystallized product was obtained; it was washed and filtered with deionized water 7 times the mass of the crystallized product, then dried at 80°C for 6 hours, and then roasted at 600°C for 3 hours to obtain the MgAPO- 11 Molecular sieves with a particle size of 200nm and a specific surface area of ​​230m 2 / g.

Embodiment 3

[0028] The following raw materials are proportioned according to the molar ratio, pseudo-boehmite, Al 2 o 3 Calculated; Heteroatom source cobaltous chloride, calculated as CoO; Phosphoric acid, calculated as P 2 o 5 count;

[0029] Pseudoboehmite: cobaltous chloride: phosphoric acid: organic amine=0.9:0.1:1.0:0.8;

[0030] The organic amine is a mixture of di-n-propylamine and diisopropylamine with a mass ratio of 1:1;

[0031] After mixing with deionized water and stirring for 40 minutes, adjust the pH value of the system to 6.0, and then freeze-dry the obtained colloid at -60°C for 2.5 days to prepare dry gel; crystallize the obtained dry gel at 170°C in an autoclave for 36 hours Finally, the crystallized product was obtained; it was washed and filtered with deionized water 8 times the mass of the crystallized product, then dried at 60°C for 12 hours, and then roasted at 650°C for 2 hours to obtain the CoAPO- 11 Molecular sieves with a particle size of 300nm and a speci...

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PUM

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Abstract

The invention relates to a preparation method for a nano-sized AEL-structure molecular sieve and belongs to the new catalytic material synthesis field and the energy and chemical industry field. Pseudo-boehmite, a heteroatom source, phosphoric acid and organic amine are used as raw materials, the raw materials are mixed, frozen and dried so that dry gel can be obtained, and then crystallization is performed on the dry gel, so that the AEL-structure molecular sieve is obtained. According to the preparation method for the nano-sized AEL-structure molecular sieve, at first, the gel is frozen and dried through a freeze drying technology to become dry gel, and then crystallization is performed on the dry gel. The AEL-structure molecular sieve prepared through the method has the advantages of achieving nanometer sizes and being high in specific area.

Description

technical field [0001] The invention relates to a preparation method of a molecular sieve with a nanometer size AEL structure, and belongs to the fields of catalytic new material synthesis, energy and chemical industry. Background technique [0002] The introduction of heteroatoms into the framework through isomorphic substitution endows phosphorus-aluminum molecular sieves with acid catalytic activity. Among them, MeAPO-11 molecular sieves have been used in the field of direct alkane isomerization and other fields because of their suitable one-dimensional ten-membered ring structure and mild acidic properties. Has been widely used. Isomerization reaction belongs to orifice catalysis reaction. Higher orifice exposure rate can improve the selectivity of isomerized hydrocarbons and reduce the particle size of molecular sieves. Preparation of nanoscale molecular sieves is an effective means to achieve this goal. The smaller molecular sieve particle size can effectively increas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/04C01B37/06C01B37/08B82Y40/00
Inventor 许本静刘欣梅刘毓翔许露吕玉超阎子峰
Owner BC P INC CHINA NAT PETROLEUM CORP