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SAPO-34/ZSM-5 composite molecular sieve and synthesis method of composite molecular sieve

A composite molecular sieve, ZSM-5 technology, applied in the direction of molecular sieve and alkali exchange phosphate, etc., can solve the problems of low reactivity, weak acidity, single pore size of porous materials, etc., and achieve high reactivity, good technical effect, wide acid distribution Effect

Inactive Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] One of the technical problems to be solved by the present invention is that the porous material synthesized in the prior art has a single pore size, weak acidity and low reactivity. A new composite molecular sieve is provided. The molecular sieve has multi-stage channels, wide acid distribution, Advantages of high reactivity

Method used

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  • SAPO-34/ZSM-5 composite molecular sieve and synthesis method of composite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Weigh 14.7g of pseudo-boehmite and mix it with 78g of water, add 18.5g of orthophosphoric acid (85%) under stirring conditions, continue stirring evenly, add 9g of silica sol (40%), 10g of triethylamine and 10g of Tetraethylammonium hydroxide, stir evenly;

[0031] (2) Weigh 15g of H-type ZSM-5 molecular sieve, add it to the mixture obtained in step (1), and stir evenly;

[0032] (3) Transfer the mixed solution obtained in step (2) to a closed high-pressure crystallization kettle, and crystallize at 180°C for 48 hours;

[0033] (4) The product was taken out, washed with water, dried, and calcined at 550°C for 4 hours to remove the template agent to obtain SAPO-34 / ZSM-5 composite molecular sieve, which was quantified by XRD diffraction. The weight content of SAPO-34 molecular sieve in the product was 60%, ZSM The weight content of -5 molecular sieve is 40%, and the XRD diffraction pattern of composite molecular sieve is as follows figure 1 shown.

[0034]

Embodiment 2

[0036](1) Weigh 14.7g of pseudo-boehmite and mix it with 100g of water, add 23g of orthophosphoric acid (85%) under stirring conditions, continue stirring evenly, add 12g of silica sol (40%), 25g of tetraethylammonium hydroxide , stir evenly;

[0037] (2) Weigh 10g of Na-type ZSM-5 molecular sieve, add it to the mixture obtained in step (1), and stir evenly;

[0038] (3) Transfer the mixed solution obtained in step (2) to a closed high-pressure crystallization kettle, and crystallize at 160°C for 60 hours;

[0039] (4) The product was taken out, washed with water, dried, and roasted at 540°C for 5 hours to remove the template agent to obtain a SAPO-34 / ZSM-5 composite molecular sieve, which was quantified by XRD diffraction. The weight content of SAPO-34 molecular sieve in the product was 70%, ZSM The weight content of -5 molecular sieve is 30%.

[0040]

Embodiment 3

[0042] (1) Mix 38g of aluminum isopropoxide with 100g of water, add 25g of orthophosphoric acid (85%), 5g of aluminum dihydrogen phosphate under stirring conditions, continue stirring evenly, add 22g of silica sol (40%), 20g of morpholine And 30g tetraethylammonium hydroxide, stir;

[0043] (2) Weigh 40g of ZSM-5 molecular sieve with Zn ion exchange, add it to the mixed solution obtained in step (1), and stir evenly;

[0044] (3) Transfer the mixed solution obtained in step (2) to a closed high-pressure crystallization kettle, and crystallize at 200°C for 50 hours;

[0045] (4) The product was taken out, washed with water, dried, and roasted at 550°C for 6 hours to remove the template agent to obtain a SAPO-34 / ZSM-5 composite molecular sieve, which was quantified by XRD diffraction. The weight content of SAPO-34 molecular sieve in the product was 40%, ZSM The weight content of -5 molecular sieve is 60%.

[0046] Press and crush the composite molecular sieve, take 9g of 10-20...

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Abstract

The invention relates to an SAPO-34 / ZSM-5 composite molecular sieve and a synthesis method of the composite molecular sieve, solving the problems of single pore diameter, low acidity and low reaction activity of the porous materials which are synthesized by the prior art. The synthesis method of the composite molecular sieve comprises the following steps: firstly mixing a silicon source, an aluminum source, a phosphorus source and an organic template agent according to a certain ratio, then adding a certain quantity of ZSM-5 molecular sieves, uniformly mixing and carrying out hydrothermal crystallization, and synthesizing the SAPO-34 / ZSM-5 composite molecular sieve by controlling nucleation and crystal growth conditions, wherein the composite molecular size is adjustable in ratio of two phases; an XRD diffraction spectrum of the composite molecular size has a maximum d interval at the positions of 7.92+ / -0.1, 8.79+ / -0.1, 9.52+ / -0.1, 12.85+ / -0.1, 16.00+ / -0.1, 20.56+ / -0.1, 23.01+ / -0.05, 23.24+ / -0.05, 23.86+ / -0.05, 25.83+ / -0.1, 30.55+ / -0.1 and 31.32+ / -0.1. The composite molecular sieve can be applied to industrial production for preparing aromatic hydrocarbon by reacting methyl alcohol / dimethyl ether.

Description

technical field [0001] The invention relates to a SAPO-34 / ZSM-5 composite molecular sieve and a synthesis method thereof. [0002] Background technique [0003] ZSM-5 molecular sieve is a microporous silica-alumina zeolite molecular sieve with a ten-membered ring channel structure. It has a large specific surface area, good channel shape selectivity, high thermal stability and hydrothermal stability. Wide range of applications. The ZSM-5 molecular sieve has a pore size range of 0.52~0.56nm, which is suitable for the aromatization, isomerization, catalytic oxidation, catalytic cracking and methanol catalytic hydrocarbon production of alkanes. By controlling the synthesis conditions, the molecular sieve framework can be adjusted. According to the distribution and ratio of silicon and aluminum, ZSM-5 molecular sieves with different acid amounts and strengths can be obtained. SAPO-34 molecular sieve is a kind of silicoaluminophosphate (SAPO) molecular sieve, which was first s...

Claims

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Application Information

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IPC IPC(8): C01B39/54
Inventor 陈希强汪哲明周伟
Owner CHINA PETROLEUM & CHEM CORP
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