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A kind of synthetic method of hzsm-5 molecular sieve

A synthesis method and molecular sieve technology, which are applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of cumbersome preparation process, time-consuming and harmful, and achieve simplified preparation process, high yield and pollution. low effect

Inactive Publication Date: 2017-08-15
NINGXIA UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The second template agent is harmful to the human body
The preparation process is cumbersome and time-consuming

Method used

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  • A kind of synthetic method of hzsm-5 molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0031] According to the synthetic ratio of SiO 2 :Al 2 o 3 :TPA + :NH 3 :C 2 h 5 OH:H 2 O=100:1:40:250:300:2200, mix 13.313g TPABr, 5g deionized water, 43.75g ammonia water, stir evenly, add 17.25g C 2 h 5 OH and 0.9378g of aluminum nitrate, stirred for 2 hours, added dropwise 18.75g of silica sol, continued to stir for 2 hours, the obtained gel was dried at 80°C for 12 hours, and ground in a mortar for 10 minutes to obtain a dry powder. Weigh 3g of dry gel powder, put it into a crucible, place the crucible in a crystallization reactor containing 15g of water at the bottom, crystallize at 180°C for 72h, cool down to room temperature, filter and wash until neutral, dry at 120°C for 12h, 550°C ℃ calcination for 6 hours to obtain HZSM-5 molecular sieve powder. The synthetic yield is 90% according to the ratio of the quality of the product obtained after roasting to the theoretical yield. The XRD spectrogram of gained product sample is as figure 1 shown.

Embodiment 2

[0033] According to the synthetic ratio of SiO 2 :Al 2 o 3 :TPA + :NH 3 :C 2 h 5 OH:H 2 O=100:1:30:250:250:2200, mix 9.9848g TPABr, 5g deionized water, 43.75g ammonia water, stir evenly, add 14.375g C 2 h 5 OH and 0.9378g of aluminum nitrate, stirred for 2h, added dropwise 18.75g of silica sol, continued to stir for 2h, the obtained gel was dried at 90°C for 12h, and ground in a mortar for 10min to obtain a dry powder. Weigh 3g of dry gel powder, put it into a crucible, place the crucible in a crystallization reactor containing 15g of water at the bottom, crystallize at 180°C for 72h, cool down to room temperature, filter and wash until neutral, dry at 120°C for 12h, 550°C Calcined at ℃ for 6 hours to obtain HZSM-5 molecular sieve powder with a yield of 88%.

Embodiment 3

[0035] According to the synthetic ratio of SiO 2 :Al 2 o 3 :TPA + :NH 3 :C 2 h 5 OH:H 2 O=100:1:50:250:300:2200, mix 16.6406g TPABr, 5g deionized water, 43.75g ammonia water, stir evenly, add 17.25g C 2 h 5OH and 0.9378g of aluminum nitrate, stirred for 2h, added dropwise 18.75g of silica sol, continued to stir for 3h, the obtained gel was dried at 100°C for 12h, and ground in a mortar for 10min to obtain a dry powder. Weigh 3g of dry gel powder, put it into a crucible, place the crucible in a crystallization reactor containing 15g of water at the bottom, crystallize at 180°C for 72h, cool down to room temperature, filter and wash until neutral, dry at 120°C for 12h, 550°C Calcined at ℃ for 6 hours to obtain HZSM-5 molecular sieve powder with a yield of 88%.

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Abstract

The invention relates to a synthesis method of an HZSM-5 molecular sieve, which comprises the following steps: (1) mixing an aluminum source, a silicon source, a template, ammonia water, ethanol and water, and stirring uniformly until dry glue powder forms a gel; drying the gel, and pulverizing into powder; (2) putting the dry glue powder in a water-containing reaction kettle, and crystallizing in a static state; and (3) washing the crystallization product, drying and roasting to obtain the product. The method does not use any sodium-ion-containing raw material, thereby avoiding the traditional ammonium exchange, washing and roasting process. The method avoids the separation between the product and mother solution in the traditional crystallization technique, and has the characteristics of low template consumption, low waste liquid amount, high yield, low cost, low pollution and the like.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a direct synthesis method of HZSM-5 molecular sieve. Background technique [0002] HZSM-5 molecular sieve has a unique pore structure, adjustable acidity and hydrothermal stability, and is an important catalyst or adsorption separation material. The preparation of HZSM-5 by NaZSM-5 exchange is complicated. In the 1980s, Bibby et al. used silicic acid, aluminum hydroxide, TPAOH, and ammonia water as raw materials to directly synthesize HZSM-5 with a silicon-aluminum ratio of 320 (Nature, NH 4 + -tetraalkyl ammonium systems in the synthesis of zeolites, 1980, Vol. 285, pp. 30-31). Wei et al. prepared a gel with tetraethyl orthosilicate, aluminum nitrate, and TPAOH as raw materials, and directly synthesized nanoscale HZSM-5 (Advanced Materials Research, Direct Synthesis of Nanocrystalline HZSM-5 Zeolite via Varying-Temperature Hydrothermal Synthesis, 2013, Vol. 821, pp. 1303-130...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40
Inventor 赵天生王媛范素兵张建利马清祥
Owner NINGXIA UNIVERSITY
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