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A kind of microporous composite silica-alumina molecular sieve and preparation method thereof

A silicon-alumina molecular sieve and microporous technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of uneven composition distribution, inability to give full play to the composite catalytic performance of molecular sieves, and uneven compounding of pore structure, so as to increase crystal nuclei Quantity effect

Active Publication Date: 2016-01-20
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The composite molecular sieve product obtained by this method has the disadvantages of uneven distribution of composition and uneven compounding of pore structure, which cannot fully exert the catalytic performance of molecular sieve composite.

Method used

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  • A kind of microporous composite silica-alumina molecular sieve and preparation method thereof
  • A kind of microporous composite silica-alumina molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 15.7g of potassium hydroxide to deionized water, stir and dissolve, add 1.72g of sodium metaaluminate and 30.3g of triethylamine to make working solution A; mix 120g of silica sol (SiO 2 The content is 30%) into the working solution A, and vigorously stirred to obtain the initial silicon-aluminum sol B, and its molar composition is: SiO 2 / Al 2 o 3 =60, R / SiO 2 =0.5, (M 1 +M 2 ) / SiO 2 =0.5, M 1 / M 2 =14,OH - / SiO 2 =0.5, H 2 O / SiO 2 =50, M 1 for K + ,M 2 for Na + , R is triethylamine.

[0028] Adjust the pH value of the initial silica-alumina sol B to 12.0 with 98% sulfuric acid to obtain silica-alumina sol C; age the silica-alumina sol C at room temperature for 24 hours to obtain silica-alumina sol D; heat silica-alumina sol D to a temperature of 175°C , constant temperature crystallization 90h.

[0029] The crystallized product was filtered and washed until the pH value of the filtrate = 8. The filter cake was dried at 120°C for 2 hours, and then ...

Embodiment 2

[0032] Add 67.2g of potassium hydroxide into deionized water, stir and dissolve, add 1.72g of sodium metaaluminate and 121.2g of triethylamine to make working solution A; mix 240g of silica sol (SiO 2 The content is 30%) into the working solution A, and vigorously stirred to obtain the initial silicon-aluminum sol B, and its molar composition is: SiO 2 / Al 2 o 3 =120, R / SiO 2 =1, (M 1 +M 2 ) / SiO 2 =1, M 1 / M 2 =60,OH - / SiO 2 =1,H 2 O / SiO 2 =50, M 1 for K + ,M 2 for Na + , R is triethylamine.

[0033] Adjust the pH value of the initial silica-alumina sol B to 13.0 with 98% sulfuric acid to obtain silica-alumina sol C; age silica-alumina sol C at room temperature for 24 hours to obtain silica-alumina sol D; heat silica-alumina sol D to a temperature of 170°C , constant temperature crystallization 75h.

[0034] The crystallized product was filtered and washed until the pH value of the filtrate = 8, and the filter cake was dried at 120°C for 2 hours, and then cal...

Embodiment 3

[0036] Add 16.8g of potassium hydroxide and 12.0g of sodium hydroxide into deionized water, stir and dissolve, add 2.3g of aluminum sulfate and 121.2g of triethylamine to make working solution A; mix 240g of silica sol (SiO 2 The content is 30%) into the working solution A, and vigorously stirred to obtain the initial silicon-aluminum sol B, and its molar composition is: SiO 2 / Al 2 o3 =60, R / SiO 2 =0.5, (M 1 +M 2 ) / SiO 2 =0.5, M 1 / M 2 =1,OH - / SiO 2 =0.5,H 2 O / SiO 2 =50, M 1 for K + ,M 2 for Na + , R is triethylamine.

[0037] Adjust the pH value of the initial silica-alumina sol B to 11.0 with 98% sulfuric acid to obtain silica-alumina sol C; age silica-alumina sol C at room temperature for 12 hours to obtain silica-alumina sol D; heat silica-alumina sol D to a temperature of 170°C , constant temperature crystallization 60h.

[0038] The crystallized product was filtered and washed until the pH value of the filtrate was 8. The filter cake was dried at 120°C ...

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Abstract

The invention relates to a microporous composite silicon aluminum molecular sieve and a preparation method thereof. The method is as below: adding an inorganic alkali source into deionized water, stirring for dissolving, adding an aluminum source and a template agent to prepare an operating fluid A; adding a silicon source into the operating fluid A to obtain a silicon aluminum initial sol B, adjusting the pH value to 9-13, aging at the room temperature for 4-36h, and crystallizing at 130-180 DEG C for 40-120 h; and filtering the crystallization products, washing until the pH value filtrate reaching 7-9, drying the filter cake at 80-140 DEG C for 1-4 h, and calcining at 450-700 DEG C for 2-6 h. The molecular sieve has TON / MTT micro composite topology structure, and can be used for processing processes including isomerization-visbreaking, hydrocracking and catalytic cracking of petroleum fractions.

Description

technical field [0001] The invention relates to a microporous composite silicon-aluminum molecular sieve and a preparation method thereof, in particular to a silicon-aluminum molecular sieve with a microporous composite structure. Background technique [0002] Molecular sieve is one of the most important components of inorganic microporous crystal materials. It has uniform composition, regular structure, adjustable surface acidity and molecular pore size, and has special shape-selective catalytic properties. It is used as a catalytic material. , gas separation and adsorbents, ion exchangers, etc. have been widely used in the fields of oil and gas processing, fine chemicals, environmental protection and nuclear waste treatment. Therefore, the design and synthesis of zeolite molecular sieves has become a hot spot in the development of new catalytic materials. [0003] ZSM-22 and ZSM-23 molecular sieves are representatives of the technical field of molecular sieve shape-select...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 秦丽红李海岩田然王东青吕倩王亮谢彬赵野李洪刚肖勇孙宏磊王福宝艾连锋李实钟立平董志强刘振宇杜立岩林哲张国静
Owner PETROCHINA CO LTD