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Synthetic method of SAPO (Silicoaluminophosphate)-11 molecular sieve

A SAPO-11, synthesis method technology, applied in molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate and other directions, can solve the problems of large molecular sieve crystal grain, low crystallinity, high synthesis cost, and achieve uniform particle size, The effect of high relative crystallinity and low cost

Active Publication Date: 2012-03-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the high synthesis cost of SAPO-11 molecular sieves in the previous literature, the synthetic molecular sieves have larger crystal grains and lower crystallinity, and provide a compound compounded with diethylamine and fluoride The method that template agent synthesizes SAPO-11 molecular sieve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Preparation of SAPO-11 molecular sieve (addition of fluoride)

[0016] After mixing 16.4g of raw phosphoric acid (85% aqueous solution) and 77.1g deionized water, stir evenly, add pseudo-boehmite 10.2g under stirring, add silica sol (containing SiO 2 25%) 5.1 g, after stirring and reacting to form a gel, finally, 5.2 g of diethylamine solution and 1.8 g of hydrofluoric acid solution were slowly added to the above-mentioned gel, and the stirring was continued to form a gel reaction mixture. Put the above reaction mixture into a crystallization kettle with a polytetrafluoroethylene liner, crystallize at 180°C under autogenous pressure for 24 hours, and finally wash the crystallized product with deionized water, filter, and dry in air at 100°C Dry, the obtained product is analyzed by XRD diffraction to be SAPO-11 molecular sieve, the relative crystallinity is 100%, and the crystal particle size is 2.2 μm.

Embodiment 2

[0018] The operation steps and experimental conditions are the same as in Example 1, except that the addition of hydrofluoric acid is changed to 3.6g, and the resulting product is analyzed by XRD diffraction to be SAPO-11 molecular sieve, with a relative crystallinity of 100% and a crystal particle size of 1.8 μm.

Embodiment 3

[0020] The operation steps and experimental conditions are the same as in Example 1, except that the crystallization temperature is changed to 160° C., and the crystallization time is 48 hours. The resulting product is analyzed by XRD diffraction to be SAPO-11 molecular sieve, with a relative crystallinity of 98%, and a crystal particle size of 2.5 μm.

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Abstract

The invention relates to a synthetic method of an SAPO (Silicoaluminophosphate)-11 molecular sieve and mainly aims at solving the problems of relatively-low crystallinity, larger molecular sieve crystal grains and higher synthetic cost of the SAPO-11 molecular sieve in the prior art. The technical scheme that the SAPO-11 molecular sieve is produced by adding a low-price composite template agent of diethylamine and fluoride is adopted in the invention, so that the problem can be better solved; and the invention can be used for alkanes isomerization industrial production.

Description

technical field [0001] The invention relates to a synthesis method of silicon phosphorus aluminum molecular sieve, in particular to a preparation method of using diethylamine and hydrofluoric acid as a mixed template to synthesize small grain SAPO-11 molecular sieve with AEL structure. Background technique [0002] Silicoaluminophosphate (SAPO) molecular sieve is a new type of non-zeolite molecular sieve launched by Union Carbide Corporation in 1984. SAPO-n is replaced by Si atoms for AlPO 4 After the P or Al atoms in the framework are formed by AlO 4 、PO 4 and SiO 4 The non-neutral molecular sieve framework composed of tetrahedrons has exchangeable cations and has proton acidity; at the same time, the pore size of SAPO-n molecular sieves is 0.3-0.8nm, almost including the entire pore size range of zeolite molecular sieves; the SAPO-n molecular sieves Pore ​​volume (H 2 O) is 0.18~0.48cm 3 / g. As a new generation of molecular sieves, SAPO-n molecular sieves have been ...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 赵昱刘红星陆贤张玉贤
Owner CHINA PETROLEUM & CHEM CORP