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The preparation method of sapo-34 molecular sieve

A technology of SAPO-34 and molecular sieves, which is applied in the field of preparation of SAPO-34 molecular sieves, and can solve the problems of low ethylene selectivity and large molecular sieve grains

Active Publication Date: 2017-11-21
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 that the SAPO-34 molecular sieve crystal grain synthesized by the prior art is relatively large, and there is a problem of low selectivity of ethylene and propylene in the process of producing light olefins from methanol. The present invention provides a new SAPO-34 molecular sieve. 34 molecular sieve preparation method

Method used

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  • The preparation method of sapo-34 molecular sieve
  • The preparation method of sapo-34 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Prepare the initial crystallization solution in the same way as Comparative Example 1, put it in a kettle after aging; raise the temperature to 200°C at a rate of 8°C / min, stop heating after 4 hours of crystallization, and cool to room temperature with water; again at a rate of 5°C / min Raise the temperature to 200°C, continue crystallization for 2 hours, stop heating, and cool to room temperature; heat up to 200°C again at a rate of 2°C / min, and continue crystallization for 24 hours. The obtained product is washed, centrifuged, and dried at 110°C to obtain a solid sample. XRD results showed that the obtained product was SAPO-34 molecular sieve with an average grain size of 0.5 μm. The catalytic evaluation results of the MTO reaction show that the diene (ethylene+propylene) selectivity reached a high point of 83.6% when the reaction was carried out for 45 minutes.

Embodiment 2

[0025] Prepare the initial crystallization solution in the same way as in Comparative Example 1, put it in a kettle after aging; raise the temperature to 210°C at a rate of 8°C / min, stop heating after crystallization for 3 hours, and cool to room temperature with water; again at a rate of 5°C / min Raise the temperature to 210°C, continue crystallization for 1 hour, stop heating, and cool to room temperature; heat up to 200°C again at a rate of 2°C / min, and continue crystallization for 24 hours. The obtained product is washed, centrifuged, and dried at 110°C to obtain a solid sample. XRD results showed that the obtained product was SAPO-34 molecular sieve with an average grain size of 0.5 μm. The catalytic evaluation results of the MTO reaction show that the diene (ethylene+propylene) selectivity reached a high point of 83.4% when the reaction was carried out for 45 minutes.

Embodiment 3～8

[0027] Prepare the initial crystallization solution in the same way as Comparative Example 1, put it in a kettle after aging; raise the temperature to 200°C at a rate of 8°C / min, stop heating after crystallization for n hours, and cool it to room temperature with water; again at a rate of 5°C / min Raise the temperature to 200°C, continue to crystallize mh, stop heating, and cool to room temperature; raise the temperature to 200°C again at a rate of 2°C / min, and continue to crystallize for 24 hours. The obtained product is washed, centrifuged, and dried at 110°C to obtain a solid sample. The average particle size and MTO catalytic results are shown in Table 1.

[0028] Table 1

[0029]

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Abstract

The present invention relates to a preparation method of SAPO‑34 molecular sieve, which mainly solves the problem of low selectivity of ethylene and propylene in the process of using the molecular sieve prepared in the prior art in the process of producing light olefins from methanol. The present invention comprises the following steps by adopting: a ) Prepare phosphorus source, aluminum source, silicon source, templating agent, HF and water to make crystallization solution, and put it into crystallization tank after aging at T1 temperature ≤ 100°C for 1-24h; b) at ≥5°C / min The temperature is raised to T2 at a temperature of 180-230°C for 1-12 hours of hydrothermal crystallization; c) water cooling to T3 temperature ≤ 100°C; d) repeat step b); e) repeat step c); f) at ≤ 5°C The technical solution for obtaining molecular sieve products is obtained by hydrothermal crystallization at T4 temperature of 180-230°C for 2-36 hours at a rate of 1 / min, which solves this problem well and can be used in the industrial production of SAPO‑34 molecular sieves.

Description

technical field [0001] The invention relates to a preparation method of SAPO-34 molecular sieve. Background technique [0002] Ethylene and propylene are important basic organic chemical raw materials in the chemical industry, and play a pivotal role in the modern petroleum and chemical industries. In recent years, with the increasing shortage of global oil resources and the rising price of crude oil, the contradiction between supply and demand caused by the production of ethylene and propylene by traditional oil routes has become tense, and all countries are committed to developing new non-petroleum production of olefins. route. Among them, coal or natural gas passes through synthesis gas (CO+H 2 ) The process of producing light olefins via methanol is currently recognized as the most promising technical route. my country's energy structure, which is rich in coal resources and relatively scarce in petroleum resources, also determines that once the process route of coal-t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 管洪波刘红星钱坤张玉贤
Owner CHINA PETROLEUM & CHEM CORP