SAPO-34 molecular sieve preparation method

A technology of SAPO-34 and molecular sieve, which is applied in the field of preparation of SAPO-34 molecular sieve, can solve the problems of multiple energy sources, multiple processes, and difficulty in increasing environmental protection, and achieves the effect of high crystallinity

Active Publication Date: 2012-02-01
CHNA ENERGY INVESTMENT CORP LTD +2
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  • Claims
  • Application Information

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Problems solved by technology

This method provides remedial measures after SAPO-5 or SAPO-5+SAPO-34 mixed molecular sieves appear in the synthesis results. It is an after-the-fact remedy. In fact, it belongs to the secondary crystallization synthesis, which requires two heatings and consumes more energ

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

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[0034] The invention provides a preparation method of SAPO-34 molecular sieve, especially the preparation method of SAPO-34 in the case of leakage from a crystallization reactor.

[0035] The present invention relates to the preparation method of SAPO-34 molecular sieve on the one hand, comprises the following steps:

[0036] (a) provide template agent, aluminum source, phosphorus source, silicon source water mixture;

[0037] (b) mixing each water mixture of step (a) in a mixing tank to form a slurry;

[0038] (c) transporting the slurry mixed into the glue tank to the crystallization reactor;

[0039] (d) The slurry is subjected to a crystallization reaction in a crystallization reactor;

[0040] (e) solid-liquid separation is carried out to the crystallized slurry, and the solid product is recovered;

[0041] (f) the solid product obtains molecular sieves through drying and roasting procedures;

[0042] Wherein, before the crystallization reaction, the templating agent is...

Embodiment 1

[0079] Phosphoric acid, pseudo-boehmite, 40% silica sol, triethylamine, and deionized water are mixed according to the molar ratio of 2.5Et 3 N:Al 2 o 3 : 1.1P 2 o 5 : 0.8SiO2 2 :80H 2 O and figure 1 The process shown is for preparation, wherein the aging conditions are: temperature: 25°C, time: 2 hours; the crystallization conditions are set as: temperature: 200°C, time: 48 hours, and the setting value of the safety valve of the high-pressure crystallization tank is set to When the crystallization time is 5h, the system pressure reaches 2.78MPa, the safety valve takes off, and after the pressure is relieved instantly, the safety kettle automatically resets, but the reset seal is not tight, and triethylamine still leaks during the entire crystallization process. Roasting conditions: temperature: 550°C, time: 6 hours; finally product e was obtained.

Embodiment 2

[0081] Phosphoric acid, pseudo-boehmite, 40% silica sol, triethylamine, and deionized water are mixed according to the molar ratio of 3.0Et 3 N:Al 2 o 3 : 1.1P 2 o 5 : 0.8SiO2 2 :80H 2 O and figure 1 The process shown is for preparation, wherein the aging conditions are: temperature: 25°C, time: 2 hours; the crystallization conditions are set as: temperature: 200°C, time: 48 hours, and the setting value of the safety valve of the high-pressure crystallization tank is set to When the crystallization time is 5h, the system pressure reaches 2.78MPa, the safety valve takes off, and after the pressure is relieved instantly, the safety kettle automatically resets, but the reset seal is not tight, and triethylamine still leaks during the entire crystallization process. Roasting conditions: temperature: 550°C, time: 6 hours; finally product f was obtained.

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Abstract

The invention relates to an SAPO-34 molecular sieve preparation method, which comprises the following steps of: (a) providing template, aluminium source, phosphorus source and silica source water mixtures; (b) mixing each water mixture from Step (a) in a gel preparation pot to form a slurry; (c) conveying the slurry in the gel preparation pot to a crystallization reaction vessel; (d) performing acrystallization reaction on the slurry in the crystallization reaction vessel; (e) carrying out solid-liquid separation on the crystallized slurry, and recovering a solid product; (f) carrying out drying and roasting processes on the solid product to obtain a molecular sieve. The template is superfluous relative to the aluminium source before the crystallization reaction. Based on the method provided by the invention, a pure SAPO-molecular sieve with high crystallinity can be obtained no matter whether the condition is normal or not.

Description

technical field [0001] The invention provides a preparation method of SAPO-34 molecular sieve, especially the preparation method of SAPO-34 in the case of leakage from a crystallization reactor. Background technique [0002] The new series of silicoaluminophosphate molecular sieves (US4440871, US 4499327)-SAPO-n molecular sieves researched and developed by United Carbide Corporation (UCC) in 1984 are based on organic amines as templates, hydrated alumina, phosphoric acid, silicon The sol is an aluminum source, a phosphorus source and a silicon source, and is obtained by first obtaining an organic amine / aluminum phosphate / silicon complex with a microporous phase by hydrothermal crystallization, and then removing the template (organic amine) by roasting. SAPO-34 molecular sieve is one of them, its structure is similar to chabazite, it has three-dimensional intersecting channels, the pore diameter is about 0.38nm, and it belongs to the cubic crystal system. Due to its suitable...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 朱伟平田树勋邢爱华薛云鹏岳国
Owner CHNA ENERGY INVESTMENT CORP LTD
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