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Synthetic method for small-crystal-size high-silicon Y-type molecular sieve

A synthesis method and small crystal grain technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of low external area, easy coking, unfavorable material diffusion, etc., and achieve industrial production. The effect of low synthesis cost and high catalytic activity

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the size of Y-type molecular sieves synthesized by conventional methods is generally around 1000nm or even larger, it is extremely unfavorable for the diffusion of substances in the catalytic process, and the external area is low, the conversion ability of macromolecules is weak, and it is easy to coke, etc.

Method used

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  • Synthetic method for small-crystal-size high-silicon Y-type molecular sieve
  • Synthetic method for small-crystal-size high-silicon Y-type molecular sieve
  • Synthetic method for small-crystal-size high-silicon Y-type molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) First mix 40mL of distilled water with 6g of sodium hydroxide, add 1.5g of sodium aluminate after dissolution, add 8g of white carbon black after the dissolution is complete, and then place it in a water bath at 40°C and stir for 72 hours.

[0041] (2) Slowly add 10 mL of 3.75 mol / L hydrochloric acid dropwise to the mixture obtained in step (1). During the dropwise addition, the mixture should be prevented from undergoing morphological transformation due to drastic local pH changes.

[0042] (3) Mix and add 6g of white carbon black to the mixture obtained in step (2), then stir at room temperature for 1h, then put the reaction mixture into the reactor, seal the reactor, and place the reactor in an oven at 100°C Crystallize for 50 hours, and finally dry the solid product at 120°C for 12 hours. The obtained sample number is CL1, which is a pure Y-type molecular sieve with a silicon-aluminum ratio of 5.9 and a particle size of 210nm.

Embodiment 2

[0044] (1) First mix 40mL of distilled water with 6g of sodium hydroxide, add 9g of aluminum nitrate after dissolution, add 8g of white carbon black after the dissolution is complete, then place in a 35°C water bath and stir for 72h.

[0045] (2) Slowly add 9 mL of 3.75 mol / L hydrochloric acid dropwise to the mixture obtained in step (1). During the dropwise addition, the mixture should be prevented from undergoing morphological transformation due to severe local pH changes.

[0046] (3) Mix and add 6g of white carbon black to the mixture obtained in step (2), then stir at room temperature for 1h, then put the reaction mixture into the reactor, seal the reactor, and place the reactor in an oven at 100°C The crystallization was carried out for 55 hours, and finally the solid product was dried at 120°C for 12 hours. The obtained sample number was CL2, which was a small-grain high-silicon Y-type molecular sieve.

Embodiment 3

[0048] (1) First mix 45mL of distilled water with 5.5g of sodium hydroxide, add 7g of aluminum nitrate after dissolution, add 8g of white carbon black after the dissolution is complete, then place in a 45°C water bath and stir for 60h.

[0049] (2) Slowly add 10 mL of 3.75 mol / L hydrochloric acid dropwise to the mixture obtained in step (1). During the dropwise addition, the mixture should be prevented from undergoing morphological transformation due to drastic local pH changes.

[0050] (3) Mix and add 5g of white carbon black to the mixture obtained in step (2), then stir at room temperature for 1.5h, then put the reaction mixture into the reactor, close the reactor, place the reactor in an oven at 110 It was crystallized at ℃ for 39 hours, and finally the solid product was dried at 120℃ for 12 hours. The obtained sample number is CL3, which is a small-grain high-silicon Y-type molecular sieve.

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Abstract

The invention provides a synthetic method for a small-crystal-size high-silicon Y-type molecular sieve. The method comprises the following steps: stirring water, inorganic base, an aluminum source and part of a silicon source for 2-4 days; then adjusting the basicity of the system with acid; and adding a silicon source, and finally synthesizing the Y-type molecular sieve by hydrothermal crystallization. The small-crystal high-silicon Y-type molecular sieve synthesized by the method provided by the invention has the characteristics of small crystal size and high silicon-aluminum ratio, is suitable for serving as an adsorbent for separation of a gas and liquid mixture and can also serve as a catalyst carrier or an acid catalyst component.

Description

technical field [0001] The invention belongs to the field of synthesizing molecular sieve catalytic materials, in particular to a method for synthesizing a small-grain high-silicon Y-type molecular sieve. Background technique [0002] Y-type molecular sieve is the most important catalytic material in the oil refining industry. Its invention and application replaced clay minerals and amorphous aluminosilicates, causing a technological revolution in the oil refining industry in the 1960s. So far, Y-type molecular sieve is still the main catalytic component of catalytic cracking and hydrocracking, and is the most widely used industrial molecular sieve material. [0003] At present, the silicon-aluminum ratio of Y-type molecular sieves synthesized by conventional techniques is lower than 6, usually below 5.0, and their thermal stability and hydrothermal stability are poor. Therefore, post-treatment is required in the industry to increase the silicon-aluminum ratio. However, hig...

Claims

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Application Information

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IPC IPC(8): C01B39/24
Inventor 范峰凌凤香王少军张会成陈晓刚杨春雁
Owner CHINA PETROLEUM & CHEM CORP
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