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Synthesis method of silicoaluminophosphate (SAPO)-5 and SAPO-44 symbiotic molecular sieve

A technology of SAPO-44 and SAPO-5, which is applied in the synthesis field of SAPO-5 and SAPO-44 symbiotic molecular sieves, can solve the problems of low activity and single pore size of porous materials, and achieve good catalytic performance

Active Publication Date: 2013-04-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is the problem that the porous material synthesized in the prior art has a single pore size and low activity, and a method for synthesizing SAPO-5 and SAPO-44 symbiotic molecular sieves is provided

Method used

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  • Synthesis method of silicoaluminophosphate (SAPO)-5 and SAPO-44 symbiotic molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 11.5g phosphoric acid (containing H 3 PO 4 85%) mixed with 45g deionized water, 6.5g pseudo-boehmite powder under stirring, add 6.1g silica sol (containing SiO 2 30%), add 4.9g of cyclohexylamine, after fully mixing, this mixture is moved into the synthesis kettle and sealed. Crystallize at 185°C under its own pressure for 24 hours, wash the solid product with deionized water to neutrality, and dry it in air at 100°C to obtain SAPO-5 / SAPO-44 symbiotic molecular sieves. Quantification by XRD diffraction shows that the weight percentage of SAPO-5 in the intergrown molecular sieve is 28.5%, and the weight percentage of SAPO-44 is 71.5%.

Embodiment 2

[0021] 11.5g phosphoric acid (containing H 3 PO 4 85%) mixed with 63g deionized water, 20.4g aluminum isopropoxide powder under stirring, add 5.0g silica sol (containing SiO 2 30%), successively add 3.9g cyclohexylamine and 4.0g triethylamine, after fully mixing, this mixture is moved into the synthesis kettle and sealed. Crystallize at 200°C under its own pressure for 24 hours, wash the solid product with deionized water until neutral, and dry it in the air at 100°C to obtain SAPO-5 / SAPO-44 symbiotic molecular sieves. Quantification by XRD diffraction shows that the weight percentage of SAPO-5 in the intergrown molecular sieve is 32.2%, and the weight percentage of SAPO-44 is 67.8%.

Embodiment 3

[0023] 12.7g phosphoric acid (containing H 3 PO 4 85%) mixed with 34.2g deionized water, 6.5g pseudo-boehmite powder under stirring, add 1.1g silica sol (containing SiO 2 30%), add 2.5g cyclohexylamine and 14.7g tetraethylammonium hydroxide successively, after fully mixing, this mixture is moved into the synthesis kettle and sealed. Crystallize at 200°C under its own pressure for 24 hours, wash the solid product with deionized water until it is neutral, and dry it in air at 100°C to obtain SAPO-5 and SAPO-44 symbiotic molecular sieves. Quantification by XRD diffraction shows that the weight percentage of SAPO-5 in the intergrown molecular sieve is 50.5%, and the weight percentage of SAPO-44 is 49.5%.

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Abstract

The invention relates to a synthesis method of a silicoaluminophosphate (SAPO)-5 and SAPO-44 symbiotic molecular sieve, mainly aiming at solving the problems that the porous material synthesized by the prior art is single in aperture and lower in activity. The synthesis method comprises the following steps of: evenly mixing water, a phosphorus source, an aluminium source, a silicon source and template agent, wherein the prepared raw material mixture has the following molar composition: the ratio of Al2O3 to P2O5 to SiO2 to R to H2O is equal to 1.0:(0.6-1.2):(0.2-1.2):(0.8-2.5):(20-100); carrying out crystallization on the raw material mixture for 2-160h at the temperature of 150-220 DEG C; and finally, washing and drying the obtained solid to obtain the symbiotic molecular sieve, wherein R is single cyclohexylamine template agent, or the template agent formed by cyclohexylamine and any in triethylamine, diethylamine or tetraethylammonium hydroxide. The technical scheme better solves the problems, and can be used in the industrial production of low carbon olefin catalyst prepared from methanol.

Description

technical field [0001] The invention relates to a synthesis method of SAPO-5 and SAPO-44 symbiotic molecular sieves. Background technique [0002] In 1984, Lok et al first introduced Si into AlPO 4 Among the series of molecular sieves, a new class of silicoaluminophosphate (SAPO-n) molecular sieves was synthesized. This type of molecular sieves includes 13 kinds of three-dimensional microporous framework structures composed of tetrahedrons, some of which are new structures, and some are similar to conventional zeolites. It has a pore structure ranging from six-membered rings to twelve-membered rings, and the pore diameter is between 0.3 and 0.8nm, so it can meet the requirements of adsorption and diffusion of molecules of different sizes. [0003] SAPO-5 molecular sieve belongs to AFI type molecular sieve. Its skeleton is a one-dimensional linear and non-intersecting pore system of twelve-membered rings composed of two alternating four-membered rings and six-membered rings....

Claims

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Application Information

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