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Method for in situ synthesis of sapo-11@γ-al2o3 composite carrier material using hydrated modified alumina as matrix

A technology of SAPO-11 and composite carrier, applied in chemical instruments and methods, molecular sieve catalysts, chemical/physical processes, etc., can solve the problems of less research on in-situ synthesis technology, increase effective specific surface area, improve utilization rate, The effect of simplifying the preparation process

Active Publication Date: 2019-08-09
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] At present, most of the researches on the synthesis of SAPO-11 molecular sieves are devoted to improving the acidity and pore structure of SAPO-11 molecular sieves, but there are few studies on its in situ synthesis technology.

Method used

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  • Method for in situ synthesis of sapo-11@γ-al2o3 composite carrier material using hydrated modified alumina as matrix
  • Method for in situ synthesis of sapo-11@γ-al2o3 composite carrier material using hydrated modified alumina as matrix
  • Method for in situ synthesis of sapo-11@γ-al2o3 composite carrier material using hydrated modified alumina as matrix

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Modification of alumina matrix: 60g of deionized water and 10g of alumina balls were mixed and transferred to a crystallization kettle lined with polytetrafluoroethylene, hydrated and modified at 150°C for 24h, and the product was filtered, After washing and drying at 120°C for 4 hours, a hydrated modified alumina matrix was obtained.

[0062] (2) Preparation of SAPO-11 molecular sieve nanocrystal precursor solution: Add 8g of aluminum isopropoxide to 60g of deionized water at 80°C and stir for 2h; add 7g of phosphoric acid dropwise and stir for 2h; add 4.95g of diisopropoxide dropwise Propylamine, stirring for 2h; adding 1g of tetrapropoxysilane, stirring for 2h, placing the mixture in a polytetrafluoroethylene-lined crystallization kettle, and pre-crystallizing at 160°C for 12h to obtain the SAPO-11 nanocrystalline precursor solution.

[0063] (3) Preparation of gel mixture: Dissolve 0.2g CTABr in 20g deionized water, stir for 2h; add the precursor solution obtai...

Embodiment 2

[0067] Prepare SAPO-11@γ-Al according to the preparation method of Example 1 2 o 3 Composite material B. The difference from Example 1 is the feeding sequence of the precursor solution preparation process.

[0068] (1) Modification of alumina matrix: same as embodiment 1.

[0069] (2) Preparation of SAPO-11 molecular sieve nanocrystal precursor solution: add 70 g of phosphoric acid to 100 g of deionized water, stir at 80°C for 2 h; add 8 g of aluminum isopropoxide, and stir for 4 h; add 4.95 g of diisopropylamine dropwise, Stir for 2h; add 1g of tetrapropoxysilane, stir for 4h, place the mixture in a crystallization kettle lined with polytetrafluoroethylene, precrystallize at 160°C for 12h, and obtain SAPO-11 nanocrystal precursor solution .

[0070] (3) Preparation of gel mixture: with embodiment 1.

[0071] (4) Preparation of composite carrier material: same as Example 1.

[0072] The relative crystallinity of SAPO-11 molecular sieve in the product is 28%. Its XRD spe...

Embodiment 3

[0074] Prepare SAPO-11@γ-Al according to the preparation method of Example 1 2 o 3 Composite material C. The difference from Example 1 is that a different silicon source is used.

[0075] (1) Modification of alumina matrix: same as embodiment 1.

[0076] (2) Preparation of SAPO-11 molecular sieve nanocrystal precursor solution: add 8g aluminum isopropoxide to 60g deionized water at 80°C, stir for 6h; add 7g phosphoric acid dropwise, stir for 2h; add 4.95g diisopropoxide dropwise Propylamine; add 0.79g tetraethyl orthosilicate, stir for 6h, place the mixture in a crystallization kettle lined with polytetrafluoroethylene, precrystallize at 160°C for 12h, and obtain SAPO-11 nanocrystalline precursor solution .

[0077] (3) Preparation of gel mixture: with embodiment 1.

[0078] (4) Preparation of composite carrier material: same as Example 1.

[0079] The relative crystallinity of SAPO-11 molecular sieve in the product is 28%. Its XRD spectrum is shown in Figure 10 .

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Abstract

The invention provides an in-situ synthesis method for synthesizing composite material SAPO-11@gamma-Al2O3 by using hydrous modified alumina as substrate. The method comprises the steps of using water for hydrothermal modification of alumina substrate to acquire a alumina substrate, mixing aluminum source, phosphoric acid, organic template, silicon source and water, conducting pre-crystallization, adding the product in a surface activating agent solution while stirring the product, conducting aging treatment to acquire a gel mixture, mixing the modified alumina substrate and the gel mixture, conducting crystallization, and conducting processing and calcination to acquire the composite material SAPO-11@gamma-Al2O3. The method integrally combines nanocrystal assembly, in-situ synthesis and catalyst preparation together, avoids that the alumina substrate dissolves in the synthetic system, simplifies the preparation process of catalyst carrier, hugely increases the effective specific surface area of molecular sieves, thus upgrading the utilization rate of the molecular sieves.

Description

technical field [0001] The present invention relates to the field of petrochemical technology, specifically, the present invention relates to a kind of in-situ synthesis of SAPO-11@γ-Al with hydrated modified alumina as the matrix 2 o 3 Composite carrier material method. Background technique [0002] SAPO-11 is a silicoaluminophosphate molecular sieve first developed by UOP in 1984 (US4440871). Because of its unique pore structure and suitable acidity, it is widely used in isomerization, alkylation, adsorption separation and natural gas conversion. has broad application prospects. The synthesis of SAPO-11 molecular sieve usually uses pseudoboehmite or aluminum isopropoxide as the aluminum source, phosphoric acid as the phosphorus source, acidic silica sol or tetraethyl silicate as the silicon source, under hydrothermal or solvothermal conditions, to Di-n-propylamine, diisopropylamine, etc. are synthesized as templates. The SAPO-11 molecular sieve thus obtained has only a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/85B01J35/10C10G45/12
CPCB01J29/85B01J35/1004B01J2229/18C10G45/12C10G2300/202
Inventor 刘海燕张萍鲍晓军
Owner CHINA UNIV OF PETROLEUM (BEIJING)