Method for synthesizing SAPO-11 molecular sieve by using long chain alkyl silane as silicon source

A SAPO-11, 1. SAPO-11 technology, applied in the field of preparation of SAPO-11 molecular sieve, can solve the problems of small external surface area, small number of pores, difficult and multi-branched isomerization reaction, etc., and achieve high isomerization performance, The effect of slowing down the rapid polycondensation and promoting the crystallization process

Active Publication Date: 2012-04-04
CHINA UNIV OF PETROLEUM (BEIJING) +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although the SAPO-11 molecular sieve-based catalyst obtained by the technical scheme disclosed in the above-mentioned patent can improve the selectivity of hydrocarbon multi-branched isomerization to a certain extent, the SAPO-11 molecular sieve particles synthesized by it are all composed of crystal particles of 700-1000nm. Particle composition, so that the synthetic product has the disadvantages of fewer pores and a smaller external area
Since the multi-branched isomerization reaction is mainly carried out on the pores and the outer surface, it is difficult for the SAPO-11 molecular sieve synthesized by the prior art to efficiently promote the multi-branched isomerization reaction of hydrocarbons

Method used

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  • Method for synthesizing SAPO-11 molecular sieve by using long chain alkyl silane as silicon source
  • Method for synthesizing SAPO-11 molecular sieve by using long chain alkyl silane as silicon source
  • Method for synthesizing SAPO-11 molecular sieve by using long chain alkyl silane as silicon source

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 Synthesis of SAPO-11 molecular sieve with n-hexadecyltrimethoxysilane as silicon source

[0029]Mix 13.6g of phosphoric acid (AR, 85%) and 45g of deionized water uniformly in a 35°C water bath, add 9g of pseudoboehmite, and magnetically stir in a 35°C water bath for 2 hours to obtain an aluminum phosphate sol; Hexaalkyltrimethoxysilane [C 12 h 25 Si(CH 3 O) 3 ] (97%) was pre-hydrolyzed in 10 g of water for 1 h, then added to the aluminum phosphate sol (the molar ratio of the amount of n-hexadecyltrimethoxysilane added to the aluminum source was 0.3:1), and continued to stir in a water bath at 35 ° C After 2h, slowly add 7.9g di-n-propylamine (AR, 99%) again, continue stirring 2h to form homogeneous sol (mixed solution), the mol ratio of reaction system material is Al 2 o 3 :P 2 o 5 : SiO 2 :DPA:H 2 O=1:0.95:0.3:1.2:50;

[0030] Put the sol into a polytetrafluoroethylene autoclave, crystallize at 185°C for 48h, then centrifuge, wash the solid product ...

Embodiment 2

[0039] Example 2 Synthesis of SAPO-11 molecular sieve with n-octyltriethoxysilane as silicon source

[0040] The 6.5g of n-hexadecyltrimethoxysilane in Example 1 was changed to 5.2g of n-octyltriethoxysilane, and the composition and operating conditions of the rest of the reactants were the same as in Example 1.

[0041] The XRD characterization results of the obtained SAPO-11 molecular sieve are shown in figure 1 In the curve D, the pore structure data are shown in Table 1.

Embodiment 3

[0042] Example 3 Synthesis of SAPO-11 molecular sieve with dimethyl n-octadecyl[3-trimethoxysilylpropyl]ammonium chloride and ethyl orthosilicate as silicon source

[0043] Change the 6.5g n-hexadecyltrimethoxysilane in embodiment 1 into 2g ethyl orthosilicate and 4.6g dimethyl n-octadecyl [3-trimethoxysilyl propyl] ammonium chloride ( BC, biochemical reagent), the molar ratio of ethyl orthosilicate and dimethyl n-octadecyl [3-trimethoxysilylpropyl] ammonium chloride is 1: 1, and the composition of the remaining reactants and operating conditions and implementation Example 1 is the same.

[0044] The XRD characterization results of the obtained SAPO-11 molecular sieve are shown in figure 1 In curve C, the pore structure data are shown in Table 1.

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Abstract

The invention relates to a method for synthesizing an SAPO-11 molecular sieve by using long chain alkyl silane as a silicon source, which comprises the following steps: adding the mixture of long chain alkyl silane or long chain alkyl silane quaternary ammonium salt and tetraethoxysilane or acid silicasol into deionized water for prehydrolysis to obtain pre-hydrolyzed solution; uniformly mixing deionized water with phosphoric acid and a aluminum source, and adding the pre-hydrolyzed solution and a template agent to obtain mixed solution; subjecting the mixed solution to crystallization, separating a solid product, washing the solid product and drying the solid product to obtain SAPO-11 molecular sieve raw powder; and roasting the SAPO-11 molecular sieve raw powder to obtain the SAPO-11 molecular sieve. In the synthesis method provided by the invention, the long chain alkyl silane or long chain alkyl silane quaternary ammonium salt is used as the silicon source of the SAPO-11 molecularsieve, the synthesized SAPO-11 molecular sieve is formed by aggregation of small crystalline grains, and the SAPO-11 molecular sieve has a large outside surface and a large medium-pore pore volume.

Description

technical field [0001] The invention relates to a preparation method of SAPO-11 molecular sieve, in particular to a method for synthesizing SAPO-11 molecular sieve by using long-chain alkylsilane as a silicon source. Background technique [0002] Because microporous molecular sieves have regularly arranged micropore channels, highly crystalline pore walls and a large number of uniformly distributed active sites, they are widely used in petroleum refining and petrochemical fields. Traditionally defined, the crystal structure of silica-alumina molecular sieves is composed of SiO 4 and AlO 4 Composition of tetrahedrons. In 1982, the United States Union Carbide successfully synthesized aluminum phosphate molecular sieve AlPO 4 -n, which consists of AlO 4 and PO 4 The tetrahedrons are alternately composed, there is no exchangeable charge, and thus no acidic. Si atoms are introduced into the framework of aluminum phosphate molecular sieves to form silicoaluminophosphate mo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85
Inventor 范煜肖寒袁景利程驰刘燕来鲍晓军石冈刘海燕
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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