Preparation method and application of SSZ-13 molecular sieve

A molecular sieve and crystallization reaction technology, applied in the field of molecular sieves, can solve the problems of destroying the crystal skeleton structure, reducing the crystallinity of SSZ-13 molecular sieve, and complicated synthesis steps, achieving high and low carbon olefin selectivity, shortening time and cost, and low product. Effect of carbon rate

Pending Publication Date: 2019-08-23
EAST CHINA UNIV OF SCI & TECH
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  • Summary
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  • Description
  • Claims
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Problems solved by technology

For example, the methods disclosed in patent application CN104709917A, patent application CN105197955A and patent application CN105692647A are all secondary synthesis methods, and the synthesis steps are tedious, and the grinding process will destroy the original skeleton structure of the crystal and reduce the crystallization of SSZ-13 molecular sieve Spend

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  • Preparation method and application of SSZ-13 molecular sieve
  • Preparation method and application of SSZ-13 molecular sieve
  • Preparation method and application of SSZ-13 molecular sieve

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preparation example Construction

[0020] The invention provides a kind of preparation method of SSZ-13 molecular sieve, it comprises the steps:

[0021] Step (a), dissolving sodium hydroxide, aluminum source, silicon source and template in water to obtain mixture 1, in said mixture 1, the moles of said water, sodium hydroxide, aluminum source, silicon source and template The ratio is (30~50):(0.1~0.3):(0.02~0.01):1:(0.1~0.3).

[0022] Wherein, the aluminum source is selected from at least one of aluminum isopropoxide, activated alumina, aluminum isopropoxide, and pseudo-boehmite; the silicon source is selected from silica sol, tetraethyl orthosilicate, silicic acid At least one of sodium and fumed silica. The templating agent is an organic amine, for example, N,N,N-trimethyl-1-adamantyl ammonium hydroxide. Specifically, weigh a predetermined amount of water, aluminum source, silicon source, sodium hydroxide and template agent, add water, aluminum source, silicon source, sodium hydroxide and template agent in...

Embodiment 1

[0038] N,N,N-trimethyl-1-adamantyl ammonium hydroxide, sodium hydroxide, aluminum isopropoxide, fumed silica, water according to the molar ratio TMAdaOH:Na 2 O: Al 2 o 3 :SiO2 2 :H 2 Mix O=0.2:0.1:0.04:1:44, stir at 30°C for 2 hours to form mixture 1, add 1g of anionic polyacrylamide with a molecular weight of 2 million to every 100g of mixture 1 to form mixture 2, and age at room temperature 24h, put it into a stainless steel autoclave with polytetrafluoroethylene, crystallize at 175°C for 120h, wash, dry at 110°C, and roast at 550°C to obtain SSZ-13 molecular sieve (sample number S-1). Its XRD pattern is shown in figure 1 , SEM image see figure 2 . Depend on figure 2It can be seen from the SEM image that the SSZ-13 molecular sieve obtained in this embodiment is cubic and uniform in size, about 100 nm.

Embodiment 2

[0044] N,N,N-trimethyl-1-adamantyl ammonium hydroxide, sodium hydroxide, aluminum isopropoxide, fumed silica, water according to the molar ratio TMAdaOH:Na 2 O: Al 2 o 3 :SiO2 2 :H 2 Mix O=0.2:0.1:0.04:1:44, stir at 30°C for 2 hours to form mixture 1, add 1g of anionic polyacrylamide with a molecular weight of 2 million to every 100g of mixture 1 to form mixture 2, and age at room temperature 24h, put it into a stainless steel autoclave with polytetrafluoroethylene, then crystallize in a conventional reactor at 150°C for 120h, wash, dry at 110°C, and roast at 550°C to obtain SSZ-13 molecular sieve (sample number S -4). Its XRD pattern is shown in figure 1 , SEM image see Figure 5 . Depend on Figure 5 It can be seen from the SEM image that the SSZ-13 molecular sieve obtained in this example is ellipsoidal in shape and uniform in size, about 390 nm.

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Abstract

The invention provides a preparation method and application of an SSZ-13 molecular sieve. The preparation method comprises the following steps: (1) dissolving sodium hydroxide, an aluminum source, a silicon source and a template in water so as to obtain a mixture 1, wherein in the mixture 1, the molar ratio of water, an alkali source, the aluminum source, the silicon source and the template is (30-50):(0.1-0.3):(0.02-0.01):1:(0.1-0.3), and the template is organic amine; (2) adding polyacrylamide to the mixture 1 so as to obtain a mixture 2; (3) performing a crystallization reaction on the mixture 2 so as to obtain an initial product; (4) performing acquisition of SSZ-13 molecular sieve raw powder; and (5) performing baking for a certain period of time so as to obtain the SSZ-13 molecular sieve. The preparation method has the advantages that polyacrylamide is introduced, the growth rate of SSZ-13 molecular sieve grains is inhibited, and the small-grain SSZ-13 molecular sieve has higherselectivity to low-carbon olefin, a lower carbon deposition rate and a longer single-pass reaction life.

Description

technical field [0001] The invention relates to the field of molecular sieves, in particular to a preparation method of SSZ-13 molecular sieves and applications of SSZ-13 molecular sieves. Background technique [0002] SSZ-13 molecular sieve has excellent selective catalytic performance in chemical fields such as tail gas catalysis and methanol to olefins. The traditional method of synthesizing SSZ-13 molecular sieve is hydrothermal synthesis method. The SSZ-13 molecular sieve synthesized by this method is prone to carbon deposition, which leads to the short lifetime of the catalyst with SSZ-13 as the active component in the methanol-to-olefins reaction. [0003] By reducing the grain size of the SSZ-13 molecular sieve to reach the nanometer level, the diffusion problem of the molecular sieve catalyst can be well solved, so as to reduce the carbon deposition of the SSZ-13 molecular sieve and achieve the purpose of prolonging the single-pass life of the catalyst. [0004] At...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48B01J29/04C07C1/20C07C11/04B82Y40/00
CPCC01B39/48B01J29/041C07C1/20B82Y40/00C01P2002/72C01P2004/03C01P2004/64Y02P20/52Y02P30/20Y02P30/40
Inventor 应卫勇马宏方徐志强钱炜鑫张海涛吕志新
Owner EAST CHINA UNIV OF SCI & TECH
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