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Zn-SAPO-17/SAPO-44 composite molecular sieve as well as preparation method and application thereof

A technology of SAPO-44 and SAPO-17, applied in the field of composite molecular sieve and its preparation, to achieve the effect of good catalytic performance

Active Publication Date: 2021-03-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Up to now, the literature about Zn-SAPO-17 / SAPO-44 composite structure molecular sieve and its synthesis method has not been reported yet.

Method used

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  • Zn-SAPO-17/SAPO-44 composite molecular sieve as well as preparation method and application thereof
  • Zn-SAPO-17/SAPO-44 composite molecular sieve as well as preparation method and application thereof
  • Zn-SAPO-17/SAPO-44 composite molecular sieve as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Synthesis of Zn-SAPO-17 / SAPO-44 Composite Molecular Sieves

[0048] Take by weighing 102.98g of aluminum nitrate [Al(NO 3 ) 3 9H 2 O, purity ≥ 98wt.%, 0.27mol] and 26.36g of zinc acetate [Zn(OAc) 2 2H 2 O, 0.12mol] was dissolved in 562.95mL of deionized water, stirred evenly to form solution C 0 , after which 25.53g of phosphoric acid [H 3 PO 4 , purity ≥ 85wt.%, 0.14mol], 858.46g of tetraethylammonium hydroxide [TEAOH, 25wt.% aqueous solution, 1.46mol] into C 0 solution, after fully stirring for 0.5h, solution C was obtained 1 , after which 3.24g of acidic silica sol [SiO 2 , 40wt.%, 0.13mol] and 721.45g of cyclohexylamine [HCHA, 99wt.%, 7.28mol] into C 1 In the solution, fully stirred for 0.5h and placed at 60°C for 12h to obtain a crystallized mixture, then placed at 170°C for 3.5d, the product was filtered and washed, then dried at 80°C for 12h, then heated to 450°C, and roasted at a constant temperature The product was obtained after 12h, which was design...

Embodiment 2

[0051] Synthesis of Zn-SAPO-17 / SAPO-44 Composite Molecular Sieves

[0052] Weigh 22220.34g of aluminum isopropoxide [Al(iPr) 3 , purity ≥99wt.%, 108.79mol] and 13180.86g of zinc nitrate [Zn(NO 3 ) 2 ·6H 2 O, 44.31mol] was dissolved in 177077.94mL of deionized water, stirred evenly to form solution C 0 , after which 9532.56g of phosphoric acid [H 3 PO 4 , purity ≥ 85wt.%, 82.68mol] and 428566.40g of tetraethylammonium hydroxide [TEAOH, 50wt.% aqueous solution, 1454.74mol] into the C solution, continue to stir for 5h to obtain solution C 1 , after which 326.22g of white carbon black [SiO 2 , 99wt.%, 5.44mol], 396860.31g of cyclohexylamine [HCHA, 4008.69mol into C 1 In the solution, stirred for 5 hours and placed at 120°C for 1 hour to obtain a crystallized mixture, then placed at 180°C for 2.5 days of crystallization, the product was filtered and washed, then dried at 120°C for 6 hours, then heated to 600°C, and roasted at a constant temperature for 4 hours. The product ...

Embodiment 3

[0054] Synthesis of Zn-SAPO-17 / SAPO-44 Composite Molecular Sieves

[0055] Weigh 1092.92g of aluminum sulfate [Al 2 (SO 4 )3 18H 2 O, purity ≥98wt.%, 1.64mol] and 188.63g of zinc sulfate [ZnSO 4 ·7H 2 O, 0.66mol] was dissolved in 5371.02mL of deionized water, stirred evenly to form solution C 0 , after which 187.19g of phosphoric acid [H 3 PO 4 , 85%wt., 1.62mol], 14770.04g of tetraethylammonium bromide [TEABr, 70.28mol] were put into solution C, and stirring was continued for 1.5h to obtain solution C 1 , after which 5.82g of silica [SiO 2 , 99wt.%, 0.10mol], 3968.19g of cyclohexylamine [HCHA, 40.01mol] into C 1 In the solution, stirred for 2.5h and placed at 100°C for 3h to obtain a crystallized mixture, then placed at 175°C for 3d, the product was filtered and washed, then dried at 110°C for 8h, then heated to 500°C, and roasted at a constant temperature for 8h to obtain The product is denoted as ZSS-3, and the reactant stoichiometric ratio (molar ratio) of this sy...

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Abstract

The invention discloses a ZnSAPO17 / SAPO44 composite molecular sieve as well as a preparation method and application thereof. The Zn-SAPO-17 / SAPO-44 composite molecular sieve has two phases of an SAPO-17 molecular sieve and an SAPO-44 molecular sieve, zinc element introduced in situ is taken as framework atoms to be distributed in the composite molecular sieve, and based on the weight percentage ofthe Zn-SAPO-17 / SAPO-44 composite molecular sieve,the weight percentage of the SAPO-17 molecular sieve is 1-98.9%, the weight percentage of the SAPO-44 molecular sieve is 1-98.9%, and the weight percentage of the Zn element is 0.1-5%. The composite molecular sieve provided by the invention is a novel composite structure molecular sieve, and has the advantages of complex pore structure distribution, large total amount of acid centers and high catalytic activity.

Description

technical field [0001] The invention relates to a composite molecular sieve and its preparation method and application, in particular to a Zn-SAPO-17 / SAPO-44 composite molecular sieve and its preparation method and application. Background technique [0002] Porous material is a kind of solid compound with regular pore structure. The pore diameter of zeolite molecular sieve is generally below 2nm, so it is classified as microporous material. It is characterized by selective adsorption. Its unique pore system makes it have different sieving properties. The ability to size molecules, which is why this type of material is called a "molecular sieve". Moreover, this type of material has a wide range of internal pore size distribution and rich and diverse topological structures, and is widely used in the fields of adsorption, heterogeneous catalysis, carriers of various guest molecules, and ion exchange. [0003] Zeolite molecular sieve is a crystalline silicate material, generall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B01J29/85C07C1/20C07C11/02
CPCC01B37/08C01B39/54B01J29/85C07C1/20C01P2002/72C01P2004/03C07C11/02Y02P30/40
Inventor 乔健袁志庆陶伟川王振东滕加伟
Owner CHINA PETROLEUM & CHEM CORP
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