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Synthesis method of M (at) SSZ-13 (at) NanoBeta with core-shell structure

A core-shell structure, in-situ synthesis technology, applied in chemical instruments and methods, carbon compound catalysts, catalysts including molecular sieves, etc., can solve problems such as inability to prevent precious metals

Pending Publication Date: 2022-04-19
TAIYUAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Sulfide reacts to form H in the hydrogenation reaction 2 S (molecular size 0.36nm), the pore size of the small-pore SSZ-13 zeolite (0.38nm), cannot prevent noble metals from being 2 S poisoning
In addition, the transmission distance of active hydrogen migrating to the acidic carrier is an important factor affecting the hydrogen overflow effect. Only the small-pore zeolite encapsulated with noble metals is simply physically mixed with the acidic material, and the transmission distance of the active hydrogen on the acidic carrier has certain limitations. sex

Method used

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  • Synthesis method of M (at) SSZ-13 (at) NanoBeta with core-shell structure
  • Synthesis method of M (at) SSZ-13 (at) NanoBeta with core-shell structure
  • Synthesis method of M (at) SSZ-13 (at) NanoBeta with core-shell structure

Examples

Experimental program
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Effect test

Embodiment 1

[0049] A preparation method of Pt@SSZ-13@NanoBeta core-shell structure, the specific operation is as follows: Weigh 0.66g sodium hydroxide (NaOH), dissolve it in 7mL distilled water, add dropwise 660µl 0.02g / mL chloroplatinic acid solution (H2PtCl6 •6H2O (Pt≥37.5%)), add 75µl 3-mercaptopropyltrimethoxysilane (TMSH) dropwise, stir for 0.5h, add 6.5g N,N,N-trimethyl-1-adamantyl hydrogen dropwise Ammonium oxide ((TMAdaOH≥25%), stir evenly, add 0.62g sodium aluminate (NaAlO2), stir for 0.5h, then add dropwise 7.5g silica sol (SiO2=40%), stir for 2h, form initial gel, mol The proportioning ratio is SiO2:Al2O3:Pt:TMSH:TMAdaOH:Na2O:H2O=20:1:0.01:0.15:3:4.7:364.

[0050] The above initial gel was put into a hydrothermal reaction kettle, heated to 160°C for hydrothermal crystallization reaction for 96 hours, the product was filtered, washed, dried, and calcined at 550°C for 6 hours to obtain the product Pt@SSZ-13 molecular sieve.

[0051] Weigh 0.26g of sodium hydroxide, dissolve it i...

Embodiment 2

[0058] A preparation method of Pt@SSZ-13@NanoBeta core-shell structure, the specific operation is as follows: Weigh 0.8g sodium hydroxide, dissolve it in 7mL distilled water, add dropwise 1255µl 0.02g / mLH2PtCl6•6H2O (Pt≥37.5%), Add 141µl 3-mercaptopropyltrimethoxysilane dropwise, stir for 0.5h, add dropwise 5g N,N,N-trimethyl-1-adamantyl ammonium hydroxide ((TMAdaOH≥25%), stir well, add 0.3 g sodium aluminate, stirred for 0.5h, then added dropwise 7.5g of 40% silica sol, stirred for 2h to form an initial gel, and the molar ratio was SiO2: Al2O3: Pt: TMSH: TMAdaOH: Na2O: H2O=40:1: 0.04: 0.6: 5: 10: 706. Put the above initial gel into a hydrothermal reaction kettle, heat up to 160°C for hydrothermal crystallization reaction for 96 hours, filter the product, wash, dry, and roast at 550°C for 6 hours to obtain the product Pt@ SSZ-13 molecular sieve. Figure 21 is the EDSmapping layered diagram of Pt@SSZ-13 molecular sieve, Figure 22 It is the EDS mapping Pt distribution diagram...

Embodiment 3

[0063] A preparation method of Pd@SSZ-13@NanoBeta core-shell structure, the specific operation is as follows: Weigh 0.66g sodium hydroxide, dissolve it in 12mL distilled water, add 21 µl 0.1g / mL PdCl2 (Pd≥59%) dropwise, Add 40µl 3-mercaptopropyltrimethoxysilane dropwise, stir for 0.5h, add dropwise 6.5g N,N,N-trimethyl-1-adamantyl ammonium hydroxide ((TMAdaOH≥25%), stir evenly, Add 0.6g of sodium aluminate, stir for 0.5h, then add 7.5g of 40% silica sol dropwise, stir for 2h to form an initial gel. The molar ratio is SiO2: Al2O3: Pd: TMSH: TMAdaOH: Na2O: H2O=20: 1: 0.004: 0.08: 3: 4.7: 364. Put the above initial gel into a hydrothermal reaction kettle, heat up to 160°C for hydrothermal crystallization reaction for 96 hours, filter, wash and dry the product, and roast at 550°C for 6 hours to obtain the product Pd@SSZ-13 molecular sieve.

[0064] Weigh 0.26g of sodium hydroxide, dissolve it in 4.3mL of distilled water, add dropwise 25.8g of tetraethylammonium hydroxide, stir ev...

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Abstract

The invention relates to a preparation method of M (at) SSZ-13 (at) NanoBeta with a core-shell structure, which specifically comprises the following steps: encapsulating noble metal in core layer SSZ-13 zeolite in situ to form a core layer M (at) SSZ-13, taking a part of the core layer sample, putting the core layer sample into Beta synthetic gel, crystallizing to form the core-shell type M (at) SSZ-13 (at) NanoBeta, and performing orifice modification on the SSZ-13 zeolite through the growth of the shell layer NanoBeta zeolite to limit the contact between sulfide and noble metal, so as to obtain the core-shell type M (at) SSZ-13 (at) NanoBeta. The sulfur resistance of the catalyst is improved, the active hydrogen component in the hydrogen overflow effect can perform hydrogenation on the polycyclic aromatic hydrocarbon adsorbed on the acid site of the shell layer, and then the hydrogenation product is further cracked on the NanoBeta zeolite, so that the selective hydrocracking of the polycyclic aromatic hydrocarbon is realized. The core-shell hydrogenation catalyst prepared by the invention has high catalytic activity and good sulfur resistance.

Description

technical field [0001] The invention relates to a catalyst with a core-shell structure, in particular to a method for synthesizing M@SSZ-13@NanoBeta with a core-shell structure. Background technique [0002] With the intensification of heavy and inferior crude oil in the world, LCO (lightcycle oil, accounting for about 20-30wt% of FCC product composition) produced after catalytic cracking is rich in a large amount (50-70%) such as naphthalene, The high-value utilization of polycyclic aromatic hydrocarbons of anthracene, phenanthrene and their derivatives is an important problem to be solved in the oil refining industry. The hydrocracking of polycyclic aromatic hydrocarbons into light aromatics such as benzene, toluene, xylene and ethylbenzene (BTX), which are important raw materials in the petrochemical industry, is a conversion route with low hydrogen consumption and high added value. At the same time, the characteristics of LCO rich in aromatics can be used to meet the ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/80C07C4/06C07C15/04C07C15/06C07C15/08
CPCB01J29/80C07C4/06B01J29/7415B01J29/743B01J29/7007B01J2229/186B01J2229/20C07C2529/80C07C15/04C07C15/06C07C15/08Y02P20/52
Inventor 范彬彬董奇张传浩于峰史秀峰李瑞丰
Owner TAIYUAN UNIV OF TECH
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