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Seeding method for synthesizing chabasite type molecular sieve with high silica/alumina ratio and application of the molecular sieve

A technology of high silicon-aluminum ratio and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, molecular sieve catalyst, chemical instruments and methods, etc., can solve the problem of high specific surface area and high MTO diene selectivity, which is not high solid content Problems such as synthesis system and large amount of seed crystals are used to achieve superior MTO reaction performance, increase the selectivity of MTO diolefins, and reduce the amount of use

Active Publication Date: 2014-11-26
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

And this method consumes a lot of water, H 2 O / SiO 2 =10-50, does not belong to the high solid content synthetic system
This method introduces the CHA crystal phase product as crystal seed, but the method seed crystal consumption is bigger, and the seed crystal consumption is SiO 2 2-3% of the mass, and there is no report on the impact of crystal seeds on properties such as high silicachabazite specific surface area and crystallinity in this patent, and the CHA zeolite disclosed in this patent does not have reports on high specific surface area and high MTO diene selectivity

Method used

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  • Seeding method for synthesizing chabasite type molecular sieve with high silica/alumina ratio and application of the molecular sieve
  • Seeding method for synthesizing chabasite type molecular sieve with high silica/alumina ratio and application of the molecular sieve
  • Seeding method for synthesizing chabasite type molecular sieve with high silica/alumina ratio and application of the molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1: take SAPO-34 molecular sieve as crystal seed crystal synthesis high silicon aluminum hapiazite type molecular sieve (molar material ratio is SiO 2 :0.005Al 2 o 3 : 0.06K 2 O: 0.08Na 2 O: 0.03 Templating agent: 4H 2 O (water in the system after stopping distillation). Add the SAPO-34 molecular sieve marked as Seed-1 with 1% of the mass of silica as the seed crystal)

[0050] Preparation of SAPO-34 molecular sieve seed crystals: Add 10.2g of aluminum isopropoxide to a 100ml beaker, stir at 20°C, add 4.9g of orthophosphoric acid with a mass concentration of 85%, add 13.827g of distilled water, stir well, add 3g of neutral Silica sol (silica mass content is 30%, Na 2 (0.1% by mass content), stirred for 30 minutes, added 36.75g of 40% aqueous solution of tetraethylammonium hydroxide by mass, and stirred for 5 hours. The above mixture was transferred to a 100ml hydrothermal reaction kettle and subjected to static crystallization at 200°C for 120 hours. A...

Embodiment 2

[0056] Embodiment 2: use low-silicon-aluminum ratio chabazite molecular sieve as crystal seed to synthesize high-silicon-aluminum ratio chabazite type molecular sieve (molar material ratio is SiO 2 :0.008Al 2 o 3 : 0.02K 2 O: 0.02Na 2 O: 0.05 Templating agent: 5H 2 O (water in the system after stopping distillation). Add SSZ-13 molecular sieve marked as Seed-2 with 0.1% of the mass of silica as a seed crystal. )

[0057] The preparation of SSZ-13 molecular sieve seed crystal: with 10g alkaline silica sol (silica mass concentration is 30%, Na 2 (0.2% by mass content) was added to the reactor, stirred in a water bath at 30° C., and 17.89 g of the templating agent mass concentration was added to the aqueous solution of N, N, N-trimethyladamantane ammonium hydroxide, stirred evenly, and then added 1.92g sodium hydroxide, continue to stir evenly, then slowly add the aqueous solution made of 1.3328g aluminum sulfate octadecahydrate and 11.355g distilled water. Stir at 30°C f...

Embodiment 3

[0063] Embodiment 3: use low-silicon-aluminum type chabazite as crystal seed crystal to synthesize high-silicon-aluminum ratio chabazite (molar material ratio is SiO 2 :0.006Al 2 o 3 : 0.05K 2 O: 0.05Na 2 O:0.01 template agent: 3H 2 O (water in the system after stopping distillation). Add SSZ-13 molecular sieve marked as Seed-3 with 0.5% silica mass as seed crystal)

[0064] SSZ-13 molecular sieve seed crystal preparation: 14.4g alkaline silica sol (silica mass concentration is 30%, Na 2 (0.2% by mass content) into the reactor, stirred in a water bath at 30° C., added 17.89 g of a mass concentration of 25% aqueous solution of N, N, N-trimethyladamantane ammonium hydroxide, stirred evenly, and then added 2.69 g potassium hydroxide, continue to stir evenly, then slowly add the aqueous solution made of 1.3328g aluminum sulfate octadecahydrate and 17.355g distilled water. Stir at 30°C for 4 hours. The above mixture was transferred to a 100ml hydrothermal reaction kettle an...

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Abstract

The invention discloses a seeding method for synthesizing chabasite type molecular sieve. The seeding method comprises the following steps: evenly mixing alkaline silica sol and a template agent, slowly adding potassium hydroxide into the mixture, then adding sodium hydroxide, keeping on stirring, then slowing adding an aluminum sulphate water solution, adding a crystal seed in a chabasite crystalline phase, carrying out distillation to remove excess water, sealing, maintaining the temperature, stirring, shearing in a high speed so as to obtain uniform gel; and finally subjecting the gel to steps of crystallization, burning, and ammonium-exchange so as to obtain the finished product. The molecular sieve has the advantages of high silica / alumina ratio, high specific surface area, high MTO diolefin selectivity, and no pollution during the whole preparation process.

Description

technical field [0001] The invention relates to a method for synthesizing a high-silicon-aluminum haphazite molecular sieve by using a crystal seed and the application of the high-silicon-aluminum haphazite molecular sieve as a methanol-to-olefin (MTO) catalyst. 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, and methanol-to-olefins (MTO) has the potential to replace steam cracking technology as the main technical route for the production of ethylene and propylene. It has good economic value 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 Petr...

Claims

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Application Information

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