SAPO-11 molecular sieve and synthesis method thereof

A technology of SAPO-11, synthesis method, applied in molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate and other directions, can solve problems such as easy transformation of crystal structure, and achieve improved crystal morphology, simple synthesis process, and crystallite size. The effect of increasing the size

Active Publication Date: 2022-04-22
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has simple operation steps, is not affected by gelation temperature, etc., does not require post-processing steps, and can effectively increase the yield of SAPO-11 molecular sieve, and is easy to carry out industrial production; effectively solves the problem of easy production of SAPO-11 molecular sieves in the prior art Miscellaneous crystals, the crystal structure is easily transformed into Pna2 after calcination to remove the template agent 1 space group problem

Method used

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  • SAPO-11 molecular sieve and synthesis method thereof
  • SAPO-11 molecular sieve and synthesis method thereof
  • SAPO-11 molecular sieve and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of the first step reaction mixture

[0035] 10.9 grams of pseudoboehmite (containing 75% Al 2 o 3 ) and 63.6 grams of deionized water were stirred evenly, and 18.5 grams of phosphoric acid (containing 85% H 3 PO 4 ), mixed and stirred for 2 hours; then 9.7 grams of di-n-propylamine (chemically pure) was added thereto, and continued to stir for 2 hours; next, 8 grams of silica sol (containing 30% SiO 2 ), fully stirred for 2 hours to form an initial reaction gel; finally, 1 gram of SAPO-11 molecular sieve powder was added to the initial reaction gel, and stirred evenly to form a reaction mixture.

[0036] The second step hydrothermal crystallization treatment

[0037] The reaction mixture was put into a stainless steel autoclave, and the temperature was kept at 110°C for 1 hour, at 120°C for 1 hour, at 130°C for 1 hour, and at 200°C for 24 hours to carry out the hydrothermal crystallization reaction. After the crystallized product was filtered and washed...

Embodiment 2

[0041] 10.9 grams of pseudoboehmite (containing 75% Al 2 o 3 ) and 63.6 grams of deionized water were stirred evenly, and 18.5 grams of phosphoric acid (containing 85% H 3 PO 4 ), mixed and stirred for 2 hours; then 5 grams of di-n-propylamine (chemically pure) was mixed with 4.7 grams of diisopropylamine (chemically pure) and added thereto, and continued to stir for 2 hours; then add 8 grams of silica sol (containing 30% SiO 2 ), fully stirred for 2 hours to form an initial reaction gel; finally, 1 gram of SAPO-11 molecular sieve powder was added to the initial reaction gel, and stirred evenly to form a reaction mixture.

[0042] The reaction mixture was put into a stainless steel autoclave, and the temperature was kept at 110°C for 2 hours, at 120°C for 2 hours, at 130°C for 2 hours, and at 160°C for 24 hours to carry out the hydrothermal crystallization reaction. After the crystallized product was filtered and washed, it was dried at 120° C. and weighed to obtain 19.2 gr...

Embodiment 3

[0059] The calcined SAPO-11 molecular sieve obtained in Example 1-2 and Comparative Example 1-2 was loaded with 0.5% Pt to prepare a catalyst, which was pressed into tablets and sieved into 40-60 mesh samples. The catalyst numbers were catalyst 1 and catalyst 2 respectively. , Catalyst 3, and Catalyst 4, to investigate their catalytic effects in the isomerization reaction process of n-dodecane. Evaluation conditions are reaction pressure 2MPa, space velocity 1.0h -1 , the molar ratio of hydrogen to hydrocarbon is 12:1, and the reaction results are shown in Table 1.

[0060] Table 1

[0061]

[0062]

[0063] It can be seen from Table 1 that compared with the traditional three-stage hydrothermal synthesis method, the SAPO-11 molecular sieve prepared by the four-stage crystallization method showed higher reactivity in the hydroisomerization reaction of n-dodecane And isomer selectivity, the yield of dodecane isomers reaches more than 80%, and has more excellent isomeriza...

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Abstract

The invention provides an SAPO-11 molecular sieve and a synthesis method thereof. The synthesis method comprises the following steps: (1) stirring an aluminum source, a phosphorus source, a silicon source, a template agent, water and the SAPO-11 molecular sieve to form initial gel; (2) the molar ratio of Al2O3 in the aluminum source to P2O5 in the phosphorus source to SiO2 in the silicon source to the template agent to the water is 1: (0.8-1.2): (0.05-1.0): (0.4-2.0): (40-60); the mass ratio of Al2O3 to the SAPO-11 molecular sieve in the aluminum source is 1: (0.01-0.5); and (3) carrying out segmented crystallization on the prepared reaction mixture in a high-pressure reaction kettle, and recovering the product. According to the method, the problems that mixed crystals are easily generated when the SAPO-11 molecular sieve is synthesized in the prior art, and the crystal structure of the SAPO-11 molecular sieve is easily converted into a Pna21 space group after a template agent is removed through roasting are effectively solved, and meanwhile, the yield of the SAPO-11 molecular sieve can be effectively improved; the synthesis method is simple to operate and easy for industrial production.

Description

technical field [0001] The invention belongs to the technical field of petroleum refining, relates to a SAPO-11 molecular sieve and a synthesis method thereof, in particular to a high-yield synthesis method of the SAPO-11 molecular sieve with a stable 1cm2 space group crystal structure. Background technique [0002] In 1984, B.M.Lok, a scientist of Union Carbide Corporation, publicly published a patent for the synthesis of a series of silicoaluminophosphate molecular sieves (SAPO-n) US 4,440,871, which opened a new era for the application of SAPO molecular sieves. There are many types of SAPO-n series molecular sieves, which can be divided according to the pore size: micro-pore structure (such as SAPO-20, 25, 28), small-pore structure (such as SAPO-17, 18, 26), medium-pore structure (such as SAPO-11, 31, 41) and large pore structure (such as SAPO-5, 36, 40) four types. As a member of the family, SAPO-11 molecular sieve has a pore size of 0.39nm×0.64nm, has a one-dimensional...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
CPCC01B37/08C01B39/54C01P2002/72C01P2004/03Y02P30/40
Inventor 王新苗陆雪峰杨晓东刘彦峰高善彬谭明伟靳丽丽孟祥彬董春明张国甲倪术荣马东海徐伟池方磊郭金涛王刚丛丽茹李淑杰孙生波
Owner PETROCHINA CO LTD
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