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Method for synthesizing chabazite-type molecular sieve with high silica-alumina ratio by using seed crystal and composite inorganic base and application thereof

A high silicon-aluminum ratio, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, molecular sieve catalyst, chemical instrument and method, etc., can solve the problem of CHA zeolite without high specific surface area, high MTO diolefin selectivity, template Eliminate the problems of large dosage of agent, achieve superior MTO reaction performance, shorten crystallization time, and lower production cost

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

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Problems solved by technology

However, this method consumes a large amount of water and does not belong to a high-solid synthesis system. 2 O / SiO 2 = 10-50, resulting in a large difference in the ratio of silicon to aluminum of the synthesized product and the ratio of silicon to aluminum of the synthetic material; the method adopts a single inorganic alkali source, the amount of seed crystals is large, and the amount of template agent is large. Template agent R / SiO 2 =0.15-0.25
There is no report in this patent that the crystal seed has an impact on the specific surface area of ​​the chabazite product, MTO reactivity, etc., and the CHA zeolite disclosed in the patent has no report of a high specific surface area, nor does it have a high MTO diene selectivity report

Method used

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  • Method for synthesizing chabazite-type molecular sieve with high silica-alumina ratio by using seed crystal and composite inorganic base and application thereof
  • Method for synthesizing chabazite-type molecular sieve with high silica-alumina ratio by using seed crystal and composite inorganic base and application thereof
  • Method for synthesizing chabazite-type molecular sieve with high silica-alumina ratio by using seed crystal and composite inorganic base and application thereof

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preparation example Construction

[0042] Preparation of SSZ-13 molecular sieve seed crystals: 14.4g alkaline silica sol (SiO 2 The mass concentration is 30%, Na 2 (0.2% by mass content, the rest being water) was added to the reactor, stirred in a water bath at 30° C., and 17.89 g of a mass concentration of 25% was added to the aqueous solution of N, N, N-trimethyladamantane ammonium hydroxide, stirred evenly, Then add 2.69g of sodium hydroxide, continue to stir evenly, and then slowly add an aqueous solution made of 1.3328g of aluminum sulfate octadecahydrate and 17.355g of distilled water. Stir at 30°C for 4 hours. The above mixture was transferred to a 100ml hydrothermal reaction kettle and subjected to static crystallization at 160°C for 144 hours. After the crystallization is complete, carry out suction filtration, wash with deionized water to pH = 7.0, and dry at 100°C to obtain 2.5 grams of SSZ-13 molecular sieve samples, labeled as Seed-1, which are used as Comparative Example 2, Example 1, Example 2 ...

Embodiment 1

[0056] Embodiment 1: Utilize crystal seed and composite inorganic base to synthesize high silicon aluminum ratio chabazite type molecular sieve (molar material ratio is SiO 2 :0.005Al 2 o 3 : 0.02K 2 O: 0.10Na 2 O: 0.07 Templating agent: 5H 2 O (water in the system after adding aluminum sulfate). SSZ-13 molecular sieve marked as Seed-1 was added with 1% of the mass of silica as a seed crystal).

[0057] Gel preparation: 36g of alkaline silica sol (SiO 2 The mass content is 50%, Na 2 (2 mass content 0.4%) joins in the reactor, 20 ℃ of water baths are stirred, then add 10.128g templating agent mass concentration and be the aqueous solution of the hydroxide-N, N, N-trimethyladamantane ammonium of 43.75%, stir evenly, Slowly add 0.672g of potassium hydroxide, then add 2.4g of sodium hydroxide, continue to stir evenly, then slowly add an aqueous solution made of 0.9996g of aluminum sulfate octadecahydrate and 2.961g of distilled water, and add 0.18g of SSZ-13 molecular sieve...

Embodiment 2

[0062] Embodiment 2: Utilize crystal seed and composite inorganic base to synthesize high silicon aluminum ratio chabazite type molecular sieve (molar material ratio is SiO 2 :0.008Al 2 o 3 : 0.05K 2 O: 0.02Na 2 O:0.05 Template agent: 6H 2 O (the water in the system after adding the aluminum source), add SSZ-13 molecular sieve marked as Seed-1 with 0.1% of the mass of silicon dioxide as the seed crystal. )

[0063] Gel preparation: 36g of alkaline silica sol (SiO 2 The mass content is 50%, Na 2 (2 mass content 0.4%) join in the reactor, 30 ℃ of water baths are stirred, then add 7.91g templating agent mass concentration and be the aqueous solution of the hydroxide-N, N, N-trimethyladamantane ammonium of 40%, stir evenly, Slowly add 1.68g of potassium hydroxide, then add 0.48g of sodium hydroxide, continue to stir evenly, then slowly add an aqueous solution made of 1.8g of aluminum nitrate nonahydrate and 9.02g of distilled water, add 0.018g of SSZ-13 molecular sieve as a...

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Abstract

A method synthesizing a chabazite-type molecular sieve with high silica-alumina ratio by using seed crystal and composite inorganic base 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; adding a chabazite crystal phase molecular sieve as the seed crystal; 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 new method for synthesizing high-silicon-aluminum hechabazite-type molecular sieves and the application of high-silicon-aluminum healhazite-type molecular sieves as methanol-to-olefins (MTO) catalysts. Background technique [0002] As basic organic chemical raw materials, low-carbon olefins, especially ethylene and propylene, play a pivotal role in petrochemical and other industries. Since methanol-to-olefins (MTO) has the potential to replace steam cracking technology, it has good economic value and social value. 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 Chev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01J29/06C07C11/02C07C1/20
CPCY02P20/52
Inventor 常云峰黄小东
Owner 天津众智科技有限公司
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