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Method capable of reducing crystal grain size of aluminum phosphate molecular sieve

A kind of technology of phosphorus-aluminum molecular sieve and molecular sieve, which is applied in the direction of molecular sieve catalyst, molecular sieve characteristic aluminum phosphate, molecular sieve and alkali exchange phosphate, etc. It can solve the problems of unfavorable product actual production and application, complex synthesis process and high cost of raw materials, so as to improve the comprehensive utilization The effect of low rate, type and particle size, simple and practical synthesis method

Inactive Publication Date: 2019-08-30
陕西煤化工技术工程中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In the preparation of the above-mentioned small-grain aluminum phosphate molecular sieve, there are problems such as high raw material cost, complex synthesis process, and low yield, which are not conducive to the actual production and application of the product. Therefore, a simple, efficient, and low-cost method is sought. , and a new method for preparing aluminum phosphate molecular sieves that can improve catalytic performance is of great significance

Method used

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  • Method capable of reducing crystal grain size of aluminum phosphate molecular sieve
  • Method capable of reducing crystal grain size of aluminum phosphate molecular sieve
  • Method capable of reducing crystal grain size of aluminum phosphate molecular sieve

Examples

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Embodiment 1

[0034] Example 1: Source or preparation of aluminum phosphate molecular sieve samples (a) to (l) used as seed crystals.

[0035] The sample (a) is the flaky SAPO-34 molecular sieve prepared in Example 6 of patent CN106477595A, with a crystal size of about 1.5 μm and a thickness of 50-200 nm.

[0036] Sample (b) is a SAPO-11 molecular sieve purchased from Shanghai Shentan Environmental Protection New Material Co., Ltd., with a crystal particle size of 1-5 μm.

[0037] sample (c)

[0038] Add 12.3g pseudo-boehmite, 18.5g phosphoric acid, 7.4g silica sol, 26.8g triethylamine and 75g water into the beaker, mix and stir evenly, then transfer to a 200ml hydrothermal synthesis kettle, and heat up to 200°C under stirring Crystallized for 30h. After the crystallization, the solid product was cooled and centrifuged. The solid product was washed with deionized water until neutral, dried at 120°C, and then baked in a muffle furnace at 600°C for 4 hours to obtain a SAPO molecular sieve ...

Embodiment 2~15

[0057] Embodiment 2~15: the preparation of small particle size aluminum phosphate molecular sieve

[0058] When using silicon source, aluminum source, phosphorus source, aluminum phosphorus molecular sieves (a)~(l) that can be used as seeds, metal salt solution, organic amine template agent R and water or the above preparation (a)~(l) samples The collected mother liquor is mixed with silicon source, aluminum source, phosphorus source, phosphorus-aluminum molecular sieves (a)~(l) that can be used as crystal seeds, metal salt solution, and organic amine template agent R in a certain proportion to prepare crystallization liquid , secondary crystallization at a certain temperature for a period of time; the aluminum phosphate molecular sieve with small particle size is prepared by separation. Among them, the source of the seed crystal used as the raw material and the template used for the secondary crystallization of the traditional / seed crystal method, each raw material, the ratio...

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Abstract

The invention discloses a method capable of reducing a crystal grain size of an aluminum phosphate molecular sieve. The method comprises the steps of adding a seed crystal into a crystallization liquid and performing secondary hydrothermal crystallization. Specifically, the method comprises the following steps: uniformly mixing a silicon source, an aluminum source, a phosphorus source, a phosphorus-aluminum molecular sieve capable of being used as a seed crystal, a metal salt solution, and water or a crystallization mother liquid obtained after a seed crystal is prepared, and mixing the mixedsolution and an organic amine templating agent R to prepare an initial gel crystallization solution; and putting the crystallization solution into a hydrothermal synthesis kettle, performing crystallization, and performing separation to obtain a small-particle-size molecular sieve. The method provided by the invention is simple and high-efficiency, and can prepare the small-particle-size molecularsieve with a crystal grain size reduced by at least 50% or more in at least one dimension without using an expensive tetraethylammonium hydroxide organic amine templating agent, and has universality.

Description

technical field [0001] The invention relates to the field of preparation methods of molecular sieve materials, in particular to a preparation method for reducing the grain size of aluminum phosphate molecular sieves. Background technique [0002] In 1982, United Carbide Corporation (UCC) successfully developed a series of aluminum phosphate molecular sieves, known as the third generation molecular sieves. This type of molecular sieve has a regular pore structure and good thermal and hydrothermal stability. At the same time, by introducing heteroatoms into the framework of the molecular sieve to replace Al or P atoms, the acidity modulation of the molecular sieve can be realized, thereby broadening its range. Application in petrochemical, coal chemical and other processes. At present, this type of molecular sieve has been widely used as catalyst, adsorbent and catalyst carrier, and has been highly valued by the field of material science research and industry at home and abro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/04C01B37/08C01B39/54B01J29/83B01J29/85B01J35/02B01J35/00
CPCC01B37/04C01B37/08C01B39/54B01J29/83B01J29/85C01P2004/61C01P2004/62B01J35/40
Inventor 陈亚妮张世刚张鑫张小虎张随平张军民刘建斌
Owner 陕西煤化工技术工程中心有限公司
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