Composite inorganic base method synthesizing chabazite-type molecular sieve with high silica-alumina ratio and application thereof

A technology of high silicon-aluminum ratio and chabazite, which is applied in the field of preparation of zeolite molecular sieves, can solve the problems of low crystallinity and low specific surface area of ​​products, and achieve low acid center density, improved specific surface area, and large specific surface area.

Active Publication Date: 2014-11-05
天津众智科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

By introducing a certain amount of sodium hydroxide, it overcomes the problems of low specific surface area and low crystallinity of the product in the single pota

Method used

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  • Composite inorganic base method synthesizing chabazite-type molecular sieve with high silica-alumina ratio and application thereof
  • Composite inorganic base method synthesizing chabazite-type molecular sieve with high silica-alumina ratio and application thereof
  • Composite inorganic base method synthesizing chabazite-type molecular sieve with high silica-alumina ratio and application thereof

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0058] Example 1: Synthesis of high silica alumina ratio chabazite (material ratio is SiO 2 :0.005Al 2 O 3 : 0.05K 2 O: 0.02Na 2 O:0.1 Template: 5H 2 O (water in the system after stopping distillation))

[0059] Gel preparation: 36g of alkaline silica sol with a silica mass concentration of 50% (the silica mass concentration is 50%, Na 2 O mass content 0.4%) was added to the polytetrafluoroethylene reactor, stirred in a water bath at 50°C, and then 15.825g aqueous solution of the template agent-N, N, N-trimethyladamantane ammonium hydroxide with a mass concentration of 40% was added , Stir evenly, slowly add 1.68g potassium hydroxide, then 0.48g sodium hydroxide, stir evenly, then slowly add 0.9996g aluminum sulfate octahydrate and 5.8g deionized water solution, stir and distill at 50℃, 1 After hours, about 6.637g of water was volatilized, the distillation was stopped, and the mixture was sealed and kept at 50°C for 4 hours. Then, the gel was stirred on a homogenizer at 10,000 rp...

Example Embodiment

[0064] Example 2: Synthesis of high silica alumina ratio chabazite (material ratio is SiO 2 :0.001Al 2 O 3 : 0.12K 2 O: 0.30Na 2 O:0.08 template agent: 8H 2 O (water in the system after adding aluminum sulfate))

[0065] Gel preparation: 36g of alkaline silica sol with a silica mass concentration of 40% (the silica mass concentration is 40%, Na 2 O mass content 0.3%) was added to the polytetrafluoroethylene reactor, stirred in a water bath at 20°C, and then added 16.88g of a 30% mass concentration template agent-N, N, N-trimethyladamantane ammonium aqueous solution , Stir evenly, slowly add 4.032g potassium hydroxide, then 7.2g sodium hydroxide, stir evenly, then slowly add 0.2g aluminum sulfate octahydrate and 9.794g deionized water solution, 20 ℃ sealed heat preservation and stir 6 hour. Then, the gel was stirred on a homogenizer at 20,000 rpm for 10 minutes to obtain a uniform gel.

[0066] Crystallization: Transfer the prepared gel to a 100ml hydrothermal reactor and staticall...

Example Embodiment

[0070] Example 3: Synthesis of high silica alumina ratio chabazite using composite inorganic base (material ratio is SiO 2 :0.008Al 2 O 3 : 0.15K 2 O: 0.15Na 2 O:0.06 template agent: 6H 2 O (water in the system after stopping distillation))

[0071] Gel preparation: 60g of alkaline silica sol with a silica mass concentration of 30% (the silica mass concentration is 30%, Na 2 O mass content 0.2%) was added to the polytetrafluoroethylene reactor, stirred in a water bath at 60°C, and then 10.38g of the template hydrogen hydroxide-N, N-dimethyl-N-ethylcyclohexane with a mass concentration of 30% was added. The aqueous solution of alkane ammonium, stir well, slowly add 5.04g potassium hydroxide, then 3.6g sodium hydroxide, stir well, then slowly add 1.8g nonahydrate aluminum nitrate and 5.4g deionized water solution, distill at 60℃ After 2.5 hours, 22.924g of water was evaporated, the distillation was stopped, and the mixture was airtightly stirred at 60°C for 2 hours. Then, the gel w...

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Abstract

A composite inorganic base method synthesizing a chabazite-type molecular sieve with high silica-alumina ratio is as below: evenly mixing an alkaline silica sol and a template; slowly adding potassium hydroxide; adding sodium hydroxide; continuing to stir; then slowly adding an aqueous solution of aluminum sulfate; distilling to remove excessive water; sealing, insulating and stirring; conducting high speed shearing to obtain a uniform gel; and conducting crystallization, roasting and ammonium exchange to obtain a product. The invention has the advantages of high silica-alumina ratio, high specific surface area, high MTO diolefin selectivity and pollution-free preparation process.

Description

technical field [0001] The invention belongs to a method for preparing zeolite-type molecular sieves, and in particular relates to a synthesis method of high-silicon-aluminum hechabazite-type molecular sieves and the application of high-silicon-alumina healhazite-type molecular sieves as methanol-to-olefin (MTO) catalysts. Background technique [0002] Since methanol to olefins (MTO) has the potential to replace steam cracking technology, it has good economic and social value. Currently, SAPO-34 molecular sieve is the most common active component of MTO catalysts on the market. At the same time, people have never stopped studying the MTO properties of silica-alumina zeolite molecular sieves with the same CHA structure as SAPO-34 molecular sieves. [0003] The SSZ-13 molecular sieve invented by Chevron Petroleum Company of the United States has a CHA crystal structure, which is disclosed in the patent US4544538. However, the synthetic method of this patent has a high amount...

Claims

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Application Information

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IPC IPC(8): C01B39/04B01J29/06C07C11/12C07C1/20
CPCY02P20/52
Inventor 常云峰黄小东
Owner 天津众智科技有限公司
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