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Method for preparing molecular sieve in reaction vessel

A technology of molecular sieves and reactors, which is applied in the direction of molecular sieve compounds, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve the problems of easy loss of molecular sieves, performance degradation of molecular sieves, and influence on the physical structure of molecular sieves, and achieve uniform distribution of reaction temperature, Moderate particle size to improve the effect of the reaction process

Inactive Publication Date: 2010-09-01
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reduction of molecular sieve particle size not only makes it difficult to separate from the synthesis system by filtration, but also makes molecular sieves easy to lose during use, and also affects the physical structure of molecular sieves, resulting in a decline in the performance of molecular sieves

Method used

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  • Method for preparing molecular sieve in reaction vessel
  • Method for preparing molecular sieve in reaction vessel
  • Method for preparing molecular sieve in reaction vessel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1 Preparation of TS-2 molecular sieve by hydrothermal method

[0044] See figure 1 , the horizontal reaction kettle is a stainless steel pressure reaction kettle, which includes: a kettle body 1, the kettle body 1 is provided with a material inlet 11 and a discharge port 12; a jacket 2, the jacket 2 is located outside the kettle body 1, and has an inlet 21 and outlet 22, used for the heat removal in the reaction kettle heating and reaction process, when heating or cooling, heating steam or cooling water enters from jacket inlet 21, comes out from jacket outlet 22; And agitator, this agitator includes A stirring motor 5 as a driving device, an axial stirring shaft 4 arranged in the kettle body 1 and driven by the stirring motor 5, and a total of 3 sets of radial stirring paddles 3 fixed on the stirring shaft 4 , each group of stirring paddles 3 has blades 31; The stirring paddle is selected from a deformed turbine paddle, and the ratio (a'b' / ab) of the axial wi...

Embodiment 2

[0049] Example 2 Preparation of TS-1 molecular sieve by hydrothermal method

[0050] The length-to-diameter ratio of the horizontal reactor is 1.8, the ratio of the diameter of the deformed turbine blade to the inner diameter of the reactor is 0.6, the number of blades of the stirring paddle is 6, and the number of layers of the stirring paddle is 3, and the remainder is the same as in Example 1.

[0051] Add 100mL of 10wt% tetrapropylammonium hydroxide (TPAOH) to the above-mentioned 500mL horizontal reactor, stir at 80rpm for 10min, add 40g of tetraethyl silicate (TEOS) into the reactor, and continue stirring for 1h. Weigh 3g of tetrabutyl titanate (TBOT) and 8g of isopropanol in a beaker, stir well and add dropwise into the reactor, and continue stirring for 5h after the dropwise addition to form TS-1 sol. The reactor was sealed and self-pressure crystallized at 170°C for 72h. After crystallization, filter the product, collect and wash the filter cake, dry the filter cake a...

Embodiment 3

[0052] Example 3 Preparation of ZSM-5 molecular sieve by hydrothermal method

[0053] In a 500mL flask, add 9.04g of sodium silicate and 0.09g of sodium metaaluminate to 300mL of water, stir until a clear solution is formed, then add 11.84g of template agent tetrapropylammonium bromide (TPABr) and continue to stir to form molar The composition is n(Si):n(Al):n(TPABr):n(H 2 (0)=1:0.01:0.4:150 stock solution. The stock solution was transferred into the above-mentioned 500mL horizontal reactor, the stirring speed was controlled at 100rpm, and crystallization was carried out at 170°C for 48h. After the crystallization, the product was filtered, the filter cake was collected and washed until pH = 7, the filter cake was dried at 110°C for 5 hours, and then calcined at 550°C for 5 hours to obtain ZSM-5 molecular sieve. The shape of the obtained molecular sieve particles is more regular than the molecular sieve prepared by the existing vertical reaction kettle, which is spherical, w...

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Abstract

The invention discloses a method for producing a molecular sieve in a horizontal reaction vessel. The horizontal reaction vessel of the invention is used for hydrothermal method or sol-gel method and method for composing the molecular sieve relating to liquid and solid mixed system which can be used for composing all microporous molecular sieves, mesopore molecular sieves and microporous-mesoporecomposite molecular sieves. The invention overcomes the defects of bad mixing effect of the liquid and the solid in compositing the molecular sieve in a vertical reaction vessel and difficulty in controlling pore canal structure, grain diameter and distribution of the product thereof.

Description

technical field [0001] The present invention relates to a method for preparing molecular sieves, in particular to synthesizing microporous molecular sieves, mesoporous molecular sieves or microporous-mesoporous molecular sieves through molecular sieve synthesis methods of liquid-solid mixed systems such as hydrothermal method and sol-gel method in a reactor Molecular sieve methods such as composite molecular sieves. Background technique [0002] Molecular sieves are a class of porous solid materials with regular pore structure and super large specific surface area, which are widely used in the fields of adsorption separation, ion exchange, catalytic reaction, biology and medicine (A.Corma.From Microporous to Mesoporous Molecular Sieve Materials and Their Use in Catalysis [J]. Chemical Reviews. 1997, 97(6): 2373-2420). Hydrothermal method and sol-gel method are the main methods (Y.Wan, D.Zhao.On the ControllableSoft-Templating Approach to Mesoporous Silicates[J].Chemical Rev...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/00C01B37/00C01B39/14C01B39/22C01B39/24C01B39/08
Inventor 曹贵平张明华张大伟白伟民
Owner EAST CHINA UNIV OF SCI & TECH
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