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Method for preparing small-grain SAPO-11 molecular sieve

A SAPO-11, molecular sieve technology, applied in the direction of molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems of increased cost and complex synthesis system, and achieves low synthesis cost and simple process steps. Effect

Active Publication Date: 2008-06-25
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] CN1356264A can obtain the SAPO-11 molecular sieve particles with a particle size of 500-1000nm by adding alcoholic organic matter (such as isopropanol) during the formation of the colloidal mixture, but this method not only makes the synthesis system more complex and increases the cost of synthesis
[0007] Previous research results show that reducing the particle size of molecular sieves is beneficial to improve the performance of molecular sieve catalysts, but the existing preparation methods cannot obtain SAPO-11 molecular sieves with a particle size of less than 1 μm in a relatively cheap way

Method used

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  • Method for preparing small-grain SAPO-11 molecular sieve
  • Method for preparing small-grain SAPO-11 molecular sieve
  • Method for preparing small-grain SAPO-11 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 0.4 moles of phosphoric acid (as H 3 PO 4meter, the same below) was added to 5.1 moles of distilled water, placed in a constant temperature water bath at 35°C and mixed evenly, and 0.2 moles of pseudo-boehmite (as Al 2 o 3 After stirring and reacting to form a gel, slowly add a mixture of 0.12 moles of di-n-propylamine and 0.08 moles of diisopropylamine to the above-mentioned gel, and then add 0.08 moles of silica sol (based on SiO 2 meter, the same below), add acid to adjust the pH value to 3.5-7.0, and continue to stir to form a gel reaction mixture.

[0036] Put the above reaction mixture into a crystallization kettle with a polytetrafluoroethylene liner, first age at 130°C under autogenous pressure for 2.5 hours, then cool to room temperature, add 50% wt of distilled water and stir evenly, and then at 190°C Crystallization under autogenous pressure for 20 hours. Finally, the crystallized product is filtered, washed, and dried at 100-110°C to obtain the molecular...

Embodiment 2

[0039] The preparation of the gel reaction mixture was the same as in Example 1. Put the reaction mixture into a crystallization kettle with a polytetrafluoroethylene liner, age at 150°C for 2 hours under autogenous pressure, then cool to room temperature, add 60% by weight of distilled water and stir evenly, and then at 190°C Crystallization under autogenous pressure for 24 hours. Finally, the crystallized product is filtered, washed, and dried at 100-110°C to obtain the molecular sieve powder.

[0040] Get part crystallization product to measure by X-ray diffraction and SEM, the result is as follows: figure 2 shown. It shows that the silicoaluminophosphate molecular sieve synthesized by this method has an AEL structure, is a SAPO-11 molecular sieve, and its grain size is 300-400 nm.

Embodiment 3

[0042] The preparation of the gel reaction mixture was the same as in Example 1. Put the reaction mixture into a crystallization kettle with a polytetrafluoroethylene liner, first age at 175°C under autogenous pressure for 1.5 hours, then partially cool to room temperature, add 40% distilled water and stir evenly, and then at 190°C Crystallization under autogenous pressure for 28 hours. Finally, the crystallized product is filtered, washed, and dried at 100-110°C to obtain the molecular sieve powder.

[0043] Get part crystallization product to measure by X-ray diffraction and SEM, the result is as follows: image 3 shown. It shows that the silicoaluminophosphate molecular sieve synthesized by this method has an AEL structure, is a SAPO-11 molecular sieve, and its grain size is 500-800nm.

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Abstract

The invention relates to a method for preparing a molecular sieve with small crystal of SAPO-11, which does not use any other organics additives except template. The method prepares the molecular sieve with small crystal of SAPO-11 which has a size ranging from 300mm to 800mm and has an AEL structure comprising water, phosphorus source, aluminum source, template, and silica source. The preparation method includes the following steps: (1) the preparation of colloid slurry: according to the total material mole ration of P2O5: (0.5 to 1.5)AL2O3: (0.4 to 2.0) R: (0 to 1.0)SiO2:(17 to 60) H2O, the water, the phosphorus source, the aluminum source, the template and the silica source are added under the condition of temperature of 5 to 80 DEG C, fast mixing and the PH value controlled between 3.5 to 7.0, wherein, R is the template; (2) the aging of slurry: the reaction mixture acquired from step (1) is gel static aged under the temperature of 80 to 190 DEG C for 0.5 to 24 hours then is cooled to the room temperature; (3) the crystallization of the slurry: under the stirring condition, 0 to 200 percent of distilled water of the total mixture is put into the aging solution, then the solution is heated up to 100 to 220 DEG C for continuous crystallization for 4 to 72 hours to get the product by filtering, washing and drying after the crystallization.

Description

technical field [0001] The invention relates to a method for synthesizing small-grain silicoaluminophosphate molecular sieves, in particular to a method for synthesizing small-grain SAPO- 11 Preparation method of molecular sieve. Background technique [0002] Silicoaluminophosphate (SAPO) molecular sieve is a new type of non-zeolitic molecular sieve introduced by Union Carbide Corporation in 1984 (USP 4440871, 1984). Among them, the SAPO-11 molecular sieve with AEL configuration has been paid attention to, and its skeleton is composed of AlO 4 、PO 4 and SiO 4 It is composed of tetrahedron and has a one-dimensional elliptical straight channel with ten-membered rings. The channel size is 0.39nm×0.63nm. At present, SAPO-11 molecular sieves have been widely studied in petrochemical fields such as catalytic cracking, hydrocracking, isomerization, alkylation of branched aromatics, isomerization dewaxing, and light olefin polymerization. Especially in the isomerization dewaxin...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 陈胜利张胜振董鹏
Owner BC P INC CHINA NAT PETROLEUM CORP
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