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Preparation method of multistage pore canal SAPO-11 (silicoaluminophosphate-11) molecular sieve and application thereof in gasoline modification

A technology of SAPO-11 and molecular sieve, which is applied in the direction of molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate, refined hydrocarbon oil, etc., can solve the problem of less SAPO-n molecular sieve, and achieve improved selectivity and effective removal , the effect of high multi-branched isomer selectivity

Active Publication Date: 2010-12-15
CHINA UNIV OF PETROLEUM (BEIJING) +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the synthesis of SAPO-n molecular sieves with hierarchical pore structure.

Method used

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  • Preparation method of multistage pore canal SAPO-11 (silicoaluminophosphate-11) molecular sieve and application thereof in gasoline modification
  • Preparation method of multistage pore canal SAPO-11 (silicoaluminophosphate-11) molecular sieve and application thereof in gasoline modification
  • Preparation method of multistage pore canal SAPO-11 (silicoaluminophosphate-11) molecular sieve and application thereof in gasoline modification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1 Synthesis of SAPO-11 by adding TDPA

[0027] Stir 0.34 n-tetradecyl organophosphoric acid (TDPA) and 30 g deionized water uniformly in a water bath at 35°C for 0.5 h, then add 4.40 g of phosphoric acid (AR, 85%), stir for 0.5 h, then add 9 g of pseudoboehmite After continuing to stir in a water bath at 35°C for 4h, slowly add 7.9g of di-n-propylamine (abbreviated as DPA, AR, 99%), and after continuing to stir for 2h, add 1.3g of ethyl orthosilicate (AR, 99%), Continue stirring for 2h to obtain the reaction sol (mixed solution), the mol ratio of the material contained in the reaction sol system is Al 2 o 3 :P 2 o 5 : SiO 2 :DPA:H 2 O:TDPA=1:0.92:0.3:1.2:80:0.06;

[0028] The reaction sol was put into a polytetrafluoroethylene high-pressure reactor, and after crystallization at 185°C for 48 hours, the solid product was separated by centrifugation, washed with deionized water to pH = 7-8, and dried at 120°C for 6 hours to obtain SAPO- 11 molecular sieve ra...

Embodiment 2

[0034] Example 2 Synthesis of SAPO-11 by adding n-DPA

[0035] 0.34g TDPA among the embodiment 1 is changed into 0.27g n-decyl organic phosphoric acid (being called for short n-DPA), and the mol ratio of the material contained in the reaction sol system is Al 2 o 3 :P 2 o 5 : SiO 2 :DPA:H 2 O: n-DPA = 1: 0.92: 0.3: 1.2: 80: 0.06, the crystallization time was 48 h, and the rest of the operating conditions were the same as in Example 1 to obtain SAPO-11 molecular sieve.

[0036] The X-ray diffraction spectrum figure of the obtained SAPO-11 molecular sieve is shown in figure 1 In the curve C, the pore structure data are shown in Table 1, and the nitrogen adsorption and desorption are as follows: figure 2 Shown in curve D.

Embodiment 3

[0037] Example 3 Synthesis of SAPO-11 by adding ODPA

[0038] 0.34g TDPA in embodiment 1 is changed into 0.41g ODPA, and the mol ratio of the material contained in the reaction sol system is Al 2 o 3 :P 2 o 5 : SiO 2 :DPA:H 2 O: ODPA = 1: 0.92: 0.3: 1.2: 60: 0.06, the crystallization time was 48 h, and the rest of the operating conditions were the same as in Example 1 to obtain SAPO-11 molecular sieve.

[0039] The X-ray diffraction spectrum figure of the obtained SAPO-11 molecular sieve is shown in figure 1 In the curve C, the pore structure data are shown in Table 1, and the nitrogen adsorption and desorption are as follows: figure 2 Shown in curve D.

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Abstract

The invention relates to a preparation method of a multistage pore canal SAPO-11 (silicoaluminophosphate-11) molecular sieve and application thereof in gasoline modification. The preparation method comprises the following steps of: uniformly mixing alkylated organic phosphonic acid and deionized water, and sequentially adding phosphoric acid, an aluminum source, a template agent and a silicon source to obtain a mixed solution; carrying out crystallization, separating, washing and drying a solid product to obtain raw multistage pore canal SAPO-11 molecular sieve powder; and sintering to obtain the multistage pore canal SAPO-11 molecular sieve. In the invention, by introducing the amphiphilic alkylated organic phosphonic acid into a conventional SAPO-11 molecular sieve synthesis system and adjusting the chain length and the addition quantity of the alkylated organic phosphonic acid, the pore diameter of the molecular sieve is adjusted. The surfaces of an SAPO-11 molecular sieve product prepared with the preparation method is formed by small crystal grains, contains rich mesopore canals and has larger specific surface area and pore volume.

Description

technical field [0001] The present invention relates to a preparation method of a silicoaluminophosphate molecular sieve and its application in gasoline upgrading, in particular to a preparation method of a multi-stage pore SAPO-12 molecular sieve and its application in gasoline upgrading, which belongs to the preparation of molecular sieves technology field. Background technique [0002] Microporous molecular sieves are widely used in petroleum refining and petrochemical fields due to their regularly arranged micropore channels, highly crystalline pore walls, and a large number of evenly distributed active sites. 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, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08C10G45/12C10G45/64
Inventor 范煜肖寒程驰袁景利刘燕来鲍晓军石冈刘海燕
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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