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Synthesis method of SSZ-13 molecular sieve

A synthesis method and molecular sieve technology are applied in the field of synthesis of SSZ-13 molecular sieves, which can solve the problems of increased synthesis cost and obstacles to the industrialized production of SSZ-13 molecular sieves, and achieve the advantages of shortened induction period, good hydrothermal stability, and easy industrialized production. Effect

Active Publication Date: 2017-05-10
SHANGHAI NOVEL CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method uses choline chloride as a template, replacing the previous use of N,N,N-trimethyl-1-adamantylamine (TMAA+) cations and benzyltrimethylammonium cations as templates, and synthesizes SSZ-13 molecular sieve was produced. Although this scheme uses a relatively cheap template agent, the synthesis time is at least 4 days, which leads to an increase in synthesis cost and has brought considerable obstacles to the industrial production of SSZ-13 molecular sieve.

Method used

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  • Synthesis method of SSZ-13 molecular sieve
  • Synthesis method of SSZ-13 molecular sieve
  • Synthesis method of SSZ-13 molecular sieve

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Embodiment 1

[0039] The synthesis of embodiment 1, SSZ-13 molecular sieve

[0040] (1) Mix 10g of USY molecular sieve (silicon to aluminum ratio 50) with 100g of 20% N,N,N-trimethyl-1-adamantyl ammonium hydroxide solution, stir at 60°C for 6h, and then filter , to obtain USY molecular sieves adsorbed with N,N,N-trimethyl-1-adamantyl ammonium hydroxide (mixture A) and filtrate L containing N,N,N-trimethyl-1-adamantyl ammonium hydroxide 95.7g.

[0041](2) Dissolve 10.09g potassium hydroxide in 48g deionized water, stir to obtain potassium hydroxide solution, then add 3.33g aluminum sulfate octadecahydrate to the above potassium hydroxide solution, stir to make aluminum sulfate octadecadenate completely Dissolve, then add 60g 30% silica sol dropwise, after the silica sol is added completely, continue to stir for 2h, then add 0.12g SAPO-34 molecular sieve (silicon content is 4%) and 0.24g SSZ-13 molecular sieve (silicon-aluminum ratio 40) mixed seeds, to obtain the mixture B.

[0042] (3) T...

Embodiment 2

[0046] The synthesis of embodiment 2, SSZ-13 molecular sieve

[0047] (1) Mix 10g of Beta (silicon to aluminum ratio 70) molecular sieve with 300g of N,N,N-trimethyl-1-adamantyl ammonium hydroxide solution with a mass concentration of 60%, stir at 20°C for 10h, and then filter, Obtain the Beta molecular sieve (mixture A) that adsorbs N,N,N-trimethyl-1-adamantyl ammonium hydroxide and filtrate L 280g containing N,N,N-trimethyl-1-adamantyl ammonium hydroxide .

[0048] (2) Dissolve 10.09g of potassium hydroxide in 66.4g of deionized water, then add 2.85g of aluminum sulfate octadecahydrate to the above potassium hydroxide solution, stir to dissolve it completely, then add 60g of 30% Silica sol, after the silica sol is completely added, continue to stir for 2h, then add 0.12g SAPO-34 molecular sieve (silicon content 12%) and 0.24g SSZ-13 molecular sieve (silicon-aluminum ratio is 40) mixed seed crystals to obtain the mixture b.

[0049] (3) Take 1.8g of mixture A and add it to...

Embodiment 3

[0053] The synthesis of embodiment 3, SSZ-13 molecular sieve

[0054] (1) Mix 10g of Beta (silicon to aluminum ratio 15) molecular sieve with 100g of 40% N,N,N-trimethyl-1-adamantyl ammonium hydroxide solution, stir at 40°C for 8h, and then filter out Adsorbed Beta molecular sieve (mixture A) with N,N,N-trimethyl-1-adamantyl ammonium hydroxide and filtrate L 93.6g containing N,N,N-trimethyl-1-adamantyl ammonium hydroxide .

[0055] (2) Dissolve 7.2g of sodium hydroxide in 42g of deionized water, then add 3.42g of aluminum sulfate octadecahydrate to the above sodium hydroxide solution, stir to dissolve it completely, and then add 62g of orthosilicon drop by drop After the ethyl orthosilicate is completely added, continue to stir for 2 h, and then add a mixed seed crystal of 0.12 g SAPO-34 molecular sieve (silicon content 8%) and 0.24 g SSZ-13 molecular sieve (silicon-aluminum ratio is 3.5) , to obtain mixture B.

[0056] (3) Take 1.8g of mixture A and add it to mixture B, st...

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Abstract

The invention provides a synthesis method of an SSZ-13 molecular sieve. A USY molecular sieve or Beta molecular sieve with adsorbed N,N,N-trimethyl-1-adamantanamine cations is used as a structure guide agent to synthesize the SSZ-13 molecular sieve together with an aluminum source, a silicon source, an alkali source, water and mixed seeds, thereby greatly reducing the consumption of the expensive template N,N,N-trimethyl-1-adamantanamine cations in the traditional method, and obviously lowering the cost for synthesizing the SSZ-13 molecular sieve. The method can enhance the crystallization rate of the SSZ-13 molecular sieve and shorten the required crystallization time, and thus, is more beneficial to industrial production. The SSZ-13 molecular sieve synthesized by the method has high crystallinity and favorable hydrothermal stability; and the synthesized SSZ-13 molecular sieve can be used as an MTO (Methanol To Olefins) catalyst and can also be used as an automobile tail gas treatment catalyst support.

Description

technical field [0001] The invention belongs to the field of inorganic synthesis and catalyst preparation, and in particular relates to a synthesis method of SSZ-13 molecular sieve. Background technique [0002] SSZ-13 molecular sieve has good thermal stability and can be used as a carrier for adsorbents or catalysts, such as air purifiers, automobile exhaust catalysts, etc. At the same time, SSZ-13 molecular sieve also has cation exchange and acidity adjustability, so it has good catalytic performance for various reaction processes such as catalytic cracking and hydrocracking of hydrocarbons, and olefin and aromatic hydrocarbon construction reactions. [0003] US Patent No. 4544538 discloses a synthesis method of SSZ-13 molecular sieve for the first time. In this method, N,N,N-trimethyl-1-adamantanamine (TMAA+) organic cation was used as template to synthesize SSZ-13 molecular sieve. However, N,N,N-trimethyl-1-adamantanamine is expensive, resulting in high cost of synthes...

Claims

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Application Information

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IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72
Inventor 薛招腾李改夏建超文怀有谈赟
Owner SHANGHAI NOVEL CHEM TECH
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