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Synthetic method of SAPO-44 molecular sieve modified by rare earth metals

A SAPO-44, rare earth metal technology, applied in the synthesis field of SAPO-44 molecular sieve, can solve the problems of low catalytic activity, low selectivity of ethylene and propylene, etc.

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

[0007] The technical problem to be solved by the present invention is that the SAPO-44 molecular sieve prepared in the prior art has the problems of low catalytic activity and low selectivity of ethylene and propylene in the process of methanol to light olefins, and a rare earth metal modified SAPO is provided. The synthetic method of -44 molecular sieve

Method used

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  • Synthetic method of SAPO-44 molecular sieve modified by rare earth metals

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] According to Equation 1.6C 6 h 13 N:0.5SiO2 2 : 1.0Al 2 o 3 : 1.0P 2 o 5 : 70H 2 O:0.03Ce(NO 3 ) 3 Weigh out ingredients.

[0022] A certain amount of sodium aluminate solution with a concentration of 35wt% and phosphoric acid aqueous solution were fully stirred and mixed to form a uniform jelly, and cerium nitrate aqueous solution and orthosilicate were added sequentially under stirring, and finally a certain amount of template agent cyclohexylamine was slowly added. Add it to the above gel, mix well, put the above reaction mixture into a crystallization kettle with a polytetrafluoroethylene liner, crystallize at 190°C under autogenous pressure for 48 hours, and finally use the crystallized product Washed with ion water, filtered, and dried in air at 100°C, the obtained product was analyzed by XRD diffraction to be SAPO-44 molecular sieve, indicating that rare earth metal ions evenly entered the framework of the molecular sieve.

Embodiment 2

[0024] The original powders obtained in Comparative Example 1 and Example 2 were calcined at 600°C for 4.0 hours to remove the template agent, respectively pressed into tablets and crushed, and then sieved to take out the particle size parts of 20 to 40 mesh. The numbers were respectively S44-1, S44-2 Catalyst, pending evaluation.

Embodiment 3

[0026] Using a fixed-bed catalytic reaction device, the S44-1 and S44-2 catalysts obtained in Comparative Example 1 and Example 1 were respectively subjected to catalyst evaluation experiments. Experimental conditions: the catalyst loading is 2.0 grams, the reaction temperature is 460°C, the reaction pressure is normal pressure, and the gravimetric space velocity of methanol is 6.0 hours -1 . The results are shown in Table 1.

[0027] Table 1

[0028]

[0029] As can be seen from Table 1, compared with the SAPO-44 molecular sieve without adding metal, the SAPO-44 molecular sieve sample containing metal cerium can improve the selectivity of low-carbon olefins, especially (ethylene+propylene).

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Abstract

The invention relates to a synthesis method of an SAPO-44 molecular sieve modified by rare earth metals. The method is mainly used for solving the problems of low catalytic activity and low ethylene and propylene selectivity during the process of preparing low-carbon alkene from methanol by utilizing the SAPO-44 molecular sieve manufactured in the prior art. The technical scheme adopted by the invention is as follows: according to the method, a reaction gel is formed by uniformly mixing a phosphorus source, an aluminum source, a silicon source, a metal salt, a template agent and water and comprises the following molar compositions: Al2O3, P2O5, SiO2, R, M and H2O at a ratio of 1.0:(0.8-1.2):(0.2-0.8):(1.3-2.5):(0.02-1.2):(30-70); the reaction gel is crystallized for 16-72 hours at the temperature of 160-210 DEG C; M is a rare earth metal ion, R is a composite template agent consisting of at least one of a cyclohexylamine single template agent or cyclohexylamine and diethylamine, triethylamine, di-n-propylamine, diisopropylamine and tetraethyl ammonium hydroxide, so that the problems in the prior art are well solved, and the method provided by the invention can be applied to the process of preparing an alkene catalyst by utilizing an oxygen-containing compound.

Description

technical field [0001] The invention relates to a method for synthesizing a metal-modified SAPO-44 molecular sieve, in particular to a method for synthesizing a rare-earth metal-modified SAPO-44 molecular sieve. 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. Sialuminophosphate molecular sieve (SAPO-n) is made of SiO 2 , AlO 2 and PO 2 + A microporous crystal composed of three tetrahedral units, w...

Claims

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Application Information

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IPC IPC(8): C01B39/54
Inventor 赵昱刘红星陆贤方敬东
Owner CHINA PETROLEUM & CHEM CORP
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