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Preparation process for aluminosilicophosphate molecular sieve

A technology of aluminosilicate and molecular sieve, which is applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali-exchanged phosphate, etc., can solve the problems of SAPO molecular sieve performance regulation and the understanding of natural layered aluminosilicate still needs to be improved And other issues

Active Publication Date: 2012-04-25
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0017] Although the above-mentioned patent documents also involve some technical characteristics of using kaolin to synthesize SAPO-34, SAPO-5 and SAPO-20 molecular sieves, various SAPO molecular sieves based on natural layered aluminosilicates such as kaolinite and montmorillonite There are still large technical bottlenecks in the preparation method of the prepared SAPO molecular sieve and the performance regulation of the obtained SAPO molecular sieve, and the understanding of the change process of the natural layered aluminosilicate in the hydrothermal treatment needs to be improved.

Method used

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  • Preparation process for aluminosilicophosphate molecular sieve
  • Preparation process for aluminosilicophosphate molecular sieve
  • Preparation process for aluminosilicophosphate molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Inner Mongolia Hohhot coal series kaolin, kaolinite content is 92.5%.

[0059] Grind to an average particle size of less than 10 μm to obtain a ground activated powder.

[0060] Get 30.0g of grinding activation powder body, join in 200.0g deionized water, add pseudo-boehmite 16.4g (aluminum oxide content 78.0%) respectively afterwards, add 85.0% concentrated phosphoric acid 52.0g, morpholine 60.0g, get Mix slurry.

[0061] Transfer the above slurry to a 500ml resin ball mill jar, add 200g of zirconia balls with a diameter of 3mm, and mill for 8 hours in a planetary ball mill at a speed of 400r / min to obtain the initial slurry.

[0062] The above initial slurry was aged at room temperature for 24 h.

[0063] After aging, the initial slurry was transferred to a 500ml reactor lined with polytetrafluoroethylene, and crystallized at 240°C for 60h.

[0064] Suction filter the slurry after the crystallization reaction, and recover the filtrate for use. The solid filter res...

Embodiment 2

[0068] Coal-measure kaolin in Hohhot, Inner Mongolia, with a kaolinite content of 92.5%.

[0069] Grind to an average particle size of less than 50 μm, place it in a muffle furnace, and roast at 800°C for 2 hours to obtain a crushed and roasted activated powder.

[0070] Take 25.4 g of ground activated powder and add it to 200.0 g of deionized water, then add 13.0 g of activated alumina, 52.0 g of 85.0% concentrated phosphoric acid, and 60.0 g of morpholine to obtain a mixed slurry.

[0071] Transfer the above slurry to a 500ml resin ball mill jar, add 200g of zirconia balls with a diameter of 3mm, and mill in a planetary ball mill for 2 hours at a speed of 600r / min to obtain the initial slurry.

[0072] The above initial slurry was aged at room temperature for 24 h.

[0073] After aging, the initial slurry was transferred to a 500ml reactor lined with polytetrafluoroethylene, and crystallized at 200°C for 20h.

[0074] Suction filter the slurry after the crystallization rea...

Embodiment 3

[0078] Suzhou natural kaolin, kaolinite content is 90.6%.

[0079] Grind by wet ball milling until the average particle size is less than 50 μm, place it in a muffle furnace, and roast at 800°C for 2 hours to obtain crushed roasted activated powder.

[0080] Take 50.0 g of ground activated powder and place it in 300.0 g of deionized water, add 30.0 g of pseudoboehmite (78.0% alumina content), 100.0 g of 85.0% concentrated phosphoric acid, and 120.0 g of morpholine to obtain a mixed slurry material.

[0081] Transfer the above slurry to two 500ml resin ball milling tanks, add 200g of zirconia balls with a diameter of 3mm to the tanks respectively, and mill in a planetary ball mill for 20 hours at a speed of 400r / min to obtain the initial slurry.

[0082] The initial slurry was transferred to a PTFE-lined 1L reactor and crystallized at 200°C for 20h.

[0083] Suction filter the slurry after the crystallization reaction, and recover the filtrate for use. The solid filter resid...

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Abstract

The invention discloses a universal preparation process for aluminosilicophosphate (SAPO) molecular sieve materials from natural lamellar aluminosilicate minerals. According to the invention, on the basis of the cheap natural lamellar aluminosilicate minerals, the SAPO molecular sieve materials are prepared by carrying out activation, slurrying of ingredients, hydrothermal crystallization and removal of structure directing agents; the natural lamellar aluminosilicate minerals can be fully used as a composite silicon aluminum source, are enabled to completely dissolve by utilizing the reaction activity of an alumina layer with phosphorous species and structure directing agent species under a hydrothermal condition and utilizing dissolving and coordination capacity of a silica layer in a medium, and can assemble anew to form a variety of SAPO molecular sieve materials under the action of the structure directing agents. The process provided in the invention substantially reduces synthesis cost for SAPO molecular sieves; the prepared molecular sieves have variable structure and composition, controllable silicon content and silicon distribution and adjustable acidic site intensity and acidic site distribution; the prepared SAPO molecular sieve materials have a wide application prospect in the fields of catalysis, adsorption, ion exchange, functional materials, etc.

Description

technical field [0001] The invention relates to a method for preparing silicoaluminophosphate (SAPO) molecular sieves. Specifically, the present invention relates to a preparation method of a SAPO molecular sieve which has broad application prospects in the fields of catalysis, adsorption, ion exchange and functional materials, especially a kind of natural layered aluminosilicate mineral through activation-ingredient- A method for preparing SAPO molecular sieves by hydrothermal crystallization-destructure directing agent. Background technique [0002] Natural layered aluminosilicate minerals are used in ceramics, refractory materials, papermaking, plastics, rubber, petrochemicals, petroleum processing, coatings, paints, adhesives, optical glass, pesticides, fertilizers, medicine, glass fiber, textiles and daily cosmetics And other industries are widely used. Layered aluminosilicate is composed of silicon-oxygen tetrahedron and aluminum-oxygen (hydroxyl) octahedron, in whic...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 王体壮卢旭晨闫岩
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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