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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 potassium hydroxide inorganic alkali synthesis system, and improves the specific surface area and crystallinity of the high-silicon-alumina bichabazite molecular sieve.

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

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Experimental program
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Effect test

Embodiment 1

[0058] Embodiment 1: adopt composite inorganic base to synthesize high silicon aluminum zeolite (ratio of material is SiO 2 :0.005Al 2 o 3 : 0.05K 2 O: 0.02Na 2 O:0.1 Templating agent: 5H 2 O (water in the system after stopping the distillation))

[0059] Gel preparation: 36g silica mass concentration is 50% alkaline silica sol (silicon dioxide mass concentration is 50%, Na 2 (2 mass content 0.4%) join in the polytetrafluoroethylene reactor, 50 ℃ of water baths are stirred, then add the aqueous solution of the templating agent hydroxide-N, N, N-trimethyladamantane ammonium that 15.825g mass concentration is 40% , stir evenly, slowly add 1.68g potassium hydroxide, then add 0.48g sodium hydroxide, stir evenly, then slowly add an aqueous solution made of 0.9996g aluminum sulfate octadecahydrate and 5.8g deionized water, stir and distill at 50°C, 1 After one hour, about 6.637g of water evaporated, the distillation was stopped, and the mixture was sealed and kept stirring at ...

Embodiment 2

[0064] Embodiment 2: adopt composite inorganic base to synthesize high silicon aluminum ratio chabazite (ratio of material is SiO 2 :0.001Al 2 o 3 : 0.12K 2 O: 0.30Na 2 O: 0.08 Templating agent: 8H 2 O (water in the system after adding aluminum sulfate))

[0065] Gel preparation: 36g silica mass concentration is 40% alkaline silica sol (silicon dioxide mass concentration is 40%, Na 2 (2 mass content 0.3%) join in the polytetrafluoroethylene reactor, 20 ℃ of water baths are stirred, then add the aqueous solution of the templating agent hydroxide-N, N, N-trimethyladamantane ammonium that 16.88g mass concentration is 30% , stir evenly, slowly add 4.032g potassium hydroxide, then add 7.2g sodium hydroxide, stir evenly, then slowly add an aqueous solution made of 0.2g aluminum sulfate octadecahydrate and 9.794g deionized water, seal and keep stirring at 20°C for 6 Hour. Then the gel was stirred on a homogenizer at 20,000 rpm for 10 minutes to obtain a uniform gel.

[0066] ...

Embodiment 3

[0070] Embodiment 3: adopt composite inorganic base to synthesize high silicon aluminum zeolite (ratio of material is SiO 2 :0.008Al 2 o 3 : 0.15K 2 O: 0.15Na 2 O:0.06 Templating agent: 6H 2 O (water in the system after stopping the distillation))

[0071] Gel preparation: 60g silica mass concentration is 30% alkaline silica sol (silicon dioxide mass concentration is 30%, Na 2 (0.2% by mass content) joins in the polytetrafluoroethylene reactor, stirs in 60 ℃ of water baths, then adds 10.38g mass concentration and is the templating agent hydroxide-N, N-dimethyl-N-ethylcyclohexane of 30% Alkane ammonium aqueous solution, stir well, slowly add 5.04g potassium hydroxide, then add 3.6g sodium hydroxide, stir well, then slowly add 1.8g aluminum nitrate nonahydrate and 5.4g deionized water solution, distill at 60°C After 2.5 hours, 22.924 g of water evaporated, the distillation was stopped, and the mixture was stirred at 60° C. for 2 hours. Then the gel was stirred on a homoge...

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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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