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Small grain SAPO-34 molecular sieve preparation method

A technology of SAPO-34 and molecular sieve, which is applied in the direction of molecular sieve characteristics such as silicoaluminophosphate, molecular sieve and alkali-exchanged phosphate, and can solve the problem of large grain size of SAPO-34 molecular sieve

Active Publication Date: 2013-12-04
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 the problem that the SAPO-34 molecular sieve crystal grains synthesized by the prior art are relatively large, and the present invention provides a new method for preparing small crystal grain SAPO-34 molecular sieves

Method used

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  • Small grain SAPO-34 molecular sieve preparation method
  • Small grain SAPO-34 molecular sieve preparation method
  • Small grain SAPO-34 molecular sieve preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Prepare the initial crystallization solution in the same way as in Comparative Example 1. After the crystallization solution is crystallized at 200 °C for 4 hours in the crystallization tank, stop heating, cool to 120 °C, and keep it for 0.5 h. The temperature was raised to 200 °C again, and the crystallization was continued for 20 h; the obtained product was 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 1.3 μm. figure 2 . The catalytic evaluation results of the MTO reaction showed that the selectivity of diene (ethylene + propylene) reached a high point of 81.9% when the reaction lasted for 45 minutes.

[0028]

Embodiment 2～5

[0030] The operation steps and experimental conditions are the same as in Example 1. In the first stage, crystallize at 200°C for 8 hours, cool to 120°C, keep for 0.5 h, then raise the temperature to 200°C at a rate of 2°C / min, and continue to crystallize for 20 h, the average particle size of the obtained samples and the MTO catalytic results are shown in Table 1.

[0031] Table 1

[0032]

Embodiment 6～8

[0034] The operation steps and experimental conditions are the same as in Example 1. In the first stage, the crystallization was performed at 200 °C for 4 hours, cooled to 150 °C, and kept for 0.5 h, then the temperature was raised to 200 °C at a rate of 2 °C / min to continue the crystallization n Hours, the average particle size of the obtained samples and the MTO catalytic results are shown in Table 2.

[0035]

[0036] Table 2

[0037]

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Abstract

The invention relates to a small grain SAPO-34 molecular sieve preparation method, wherein the problem of large SAPO-34 molecular sieve grains obtained through the existing synthesis method in the prior art is mainly solved with the present invention. According to the technical scheme, the preparation method comprises: a) preparing a phosphorus source, an aluminum source, a silicon source, a template agent and water into a crystallization solution; b) carrying out stirring aging on the crystallization solution for 1-24 h at a temperature T1 of 20-100 DEG C; c) carrying out hydrothermal crystallization on the aged crystallization solution for 1-20 h at a temperature T2 of 180-250 DEG C; d) carrying out programmed cooling until a temperature T3 is room temperature-160 DEG C, and maintaining the temperature for at least 0.1 h; and e) carrying out programmed heating until a temperature T4 is 180-250 DEG C, and carrying out hydrothermal crystallization for 2-24 h to obtain the molecular sieve product. With the technical scheme, the problem is well solved, and the preparation method can be used for industrial production of small grain SAPO-34 molecular sieve preparation.

Description

technical field [0001] The invention relates to a preparation method of small grain 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 rou...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54
Inventor 管洪波刘红星张玉贤方敬东
Owner CHINA PETROLEUM & CHEM CORP
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