Method for synthesizing core-shell type zeolite molecular sieve

A technology of zeolite molecular sieve and synthesis method, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve the problems of expensive raw materials, large environmental pollution of template agents, and difficulty in industrial scale-up production, and reduce side effects. Reaction, improved selectivity and stability, effect of high reactivity

Active Publication Date: 2010-06-09
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0009] The technical problem to be solved by the present invention is that the shell phase of the core-shell molecular sieve reported in the prior art is mostly an all-silicon type core-shell molecular sieve. Ammonium bromide is used as a template, which has the problems of expensive raw materials, high environmental pollution of the template, and difficulty in industrial scale-up production. A new method for synthesizing core-shell zeolite molecular sieves is provided.

Method used

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  • Method for synthesizing core-shell type zeolite molecular sieve
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  • Method for synthesizing core-shell type zeolite molecular sieve

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Embodiment 1

[0027] 15 milliliters of ethylamine, 210 grams of water glass (containing SiO 2 25.8 wt%, Na 2 O 7.3% by weight), 9.7 g of aluminum sulfate and 650 g of water were mixed, stirred for 1 hour, and then 25 g of SiO 2 / Al 2 o 3 25 ZSM-5 nuclear phase molecular sieve, the pH of the synthesis solution is 9.2, vigorously stirred for 3 hours, put into a 1000 ml stainless steel crystallization kettle, sealed, heated to 150°C, and crystallized at constant temperature for 3 days. At the end of the crystallization, quench the solid product, filter, wash, and dry overnight at 110°C to obtain the core-shell molecular sieve CS2, and the shell SiO 2 / Al 2 o 3 After analysis, it is found that it is 80, and the core-shell ratio is 95 / 5. The XRD analysis results are consistent with the literature data.

[0028] After ion-exchanging the core-shell molecular sieve CS2 according to the method described in Comparative Example 1, the core-shell molecular sieve CS2 and SiO 2 Binder mixed, stirr...

Embodiment 2～10

[0030] Examples 2-10 are based on the synthesis ratio and synthesis conditions in Table 1, and the core-shell molecular sieves CS3-12# are synthesized according to the similar method and steps of Embodiment 1, and the core crystal catalyst Cat.0 is prepared according to the similar method of Example 1. and core-shell molecular sieve catalysts CS-Cat1~4#, see Table 2 for details.

[0031] Table 1 Preparation conditions of core-shell molecular sieves

[0032]

[0033] Table 2 Core-shell catalyst preparation conditions

[0034]

Embodiment 11

[0036] Use 2 grams of catalyst to evaluate toluene methanol selective alkylation reaction performance on a fixed bed continuous micro-reactor: the reaction raw material is a toluene methanol mixed solution (toluene methanol molar ratio is 2), and under the condition of hydrogen in the gas phase, the reaction pressure is 0.5 MPa, reaction temperature 420°C, feed liquid volume space velocity 4 hours -1 1. Under the condition that the hydrogen-to-hydrocarbon ratio is 3, the toluene conversion rate and p-xylene selectivity were measured by sampling and analysis in the process, as shown in Table 3. Listed in the table is that the reaction data of the catalyst that the ZSM-5 nuclei crystal of 25 is made is as comparative example in the table, and the result shows, compared with ZSM-5 nuclei crystal catalyst and all-silicon-shell phase catalyst (comparative example 1) , the core-shell molecular sieve catalyst has a high p-xylene selectivity, the deactivation speed of the catalyst is ...

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Abstract

The invention relates to a method for synthesizing ZSM-5/ZSM-5 core-shell type zeolite molecular sieve, mainly solving the technical problems of expensive used raw materials, great environment pollution of template agent, high difficulty of industrial amplification and synthesis, difficult industrial production and the like of the core-shell type zeolite molecular sieve in the prior art. The invention adopts the following technical scheme: the core-shell zeolite molecular sieve is prepared by adopting ZSM-5 core phase molecular sieve with a relatively low silica alumina ratio as a seed crystal, using at least one of soluble glass, silica solution, sodium silicate, white carbon black or atlapulgite which are cheap and easily obtained as a silicon source, and taking at least one organic amine from ethylamine, ethanediamine, propylamine and butylamine or the mixture of the organic amine and inorganic amine as a template agent so as to better solve the above technical problems. The invention can be used in industrialized synthetic production of core-shell type molecular sieve.

Description

technical field [0001] The invention relates to a method for synthesizing a ZSM-5 / ZSM-5 core-shell type zeolite molecular sieve. Background technique [0002] Zeolite molecular sieve is a kind of microporous crystal material with skeleton structure. It has specific size and shape of pore structure, large specific surface area and strong adjustable acidity. It is widely used in the process of petroleum refining and processing. Such as catalytic cracking, alkane isomerization, catalytic reforming and toluene disproportionation and other catalytic reactions. [0003] With the development of the petrochemical industry, people have carried out more and more researches on how to increase the yield of the target product, suppress side reactions, and improve the selectivity of the reaction. Generally speaking, while improving the selectivity of the catalyst in the reaction process, it often results in a significant decline in the activity of the catalyst. Therefore, in order to im...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B01J29/40
Inventor 孔德金邹薇
Owner CHINA PETROLEUM & CHEM CORP
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