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A kind of synthetic method of the hzsm-5 molecular sieve that adopts double template

A synthesis method and molecular sieve technology are applied in the synthesis field of HZSM-5 molecular sieve, can solve problems such as the harm of the second template agent, achieve good crystallization effect, facilitate rapid synthesis, and save the washing step.

Active Publication Date: 2021-03-30
CHNA ENERGY INVESTMENT CORP LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the ion exchange step is omitted, the second template is harmful to the human body

Method used

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  • A kind of synthetic method of the hzsm-5 molecular sieve that adopts double template

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] According to the synthetic ratio of SiO 2 :Al 2 o 3 :NH 4 OH:C 2 h 5 OH:H 2 O=100:2:350:360:5500, 1.5005g aluminum nitrate, 8.1g deionized water, 49.2g ammonia water and 16.6g C 2 h 5 Mix OH, stir well, add 74.4g ethyl orthosilicate dropwise, stir for 1h, finally add 0.88g seed crystal, continue stirring for 2h. The obtained gel was dried at 100° C. for 12 h, and ground in a mortar for 20 min to obtain a dry powder. Weigh 1g of dry gel powder, put it into a crucible, place the crucible in a crystallization reactor containing 3g of water at the bottom, crystallize at 210°C for 6h, cool down to room temperature, dry at 120°C for 12h, and roast at 550°C for 6h to obtain the product , its XRD spectrum is as figure 1 As shown (test conditions: carried out on a Rikagu X-ray diffractometer (XRD), tube voltage 40kV, tube current 30mA, scanning range 3°~80°, scanning speed 8° / min, step size 0.02, after the test with the seed crystal Comparison of XRD spectra shows that...

Embodiment 2

[0032] According to the synthetic ratio of SiO 2 :Al2 o 3 :NH 4 OH:C 2 h 5 OH:H 2 O=100:1:350:380:5500, 0.7503g aluminum nitrate, 8.4g deionized water, 49.2g ammonia water and 17.5g C 2 h 5 OH mixed, stirred evenly, added 74.4g of ethyl orthosilicate dropwise, stirred for 1h, finally added 0.86g of seed crystals, and continued to stir for 2h. The obtained gel was dried at 100° C. for 12 h, and ground in a mortar for 20 min to obtain a dry powder. Weigh 1g of dry gel powder, put it into a crucible, place the crucible in a crystallization reactor containing 3g of water at the bottom, crystallize at 210°C for 6h, cool down to room temperature, dry at 120°C for 12h, and roast at 550°C for 6h to obtain the product , as detected by XRD, it also belongs to HZSM-5 molecular sieve; at the same time, the relative crystallinity of the HZSM-5 molecular sieve is 99.02%.

Embodiment 3

[0034] According to the synthetic ratio of SiO 2 :Al 2 o 3 :NH 4 OH:C 2 h 5 OH:H 2 O=100:0.5:350:380:5500, 0.3751g aluminum nitrate, 8.5g deionized water, 49.2g ammonia water and 17.5g C 2 h 5 OH mixed, stirred evenly, added 74.4g ethyl orthosilicate dropwise, stirred for 1h, finally added 0.83g seed crystal, continued to stir for 2h. The obtained gel was dried at 100° C. for 12 h, and ground in a mortar for 20 min to obtain a dry powder. Weigh 1g of dry gel powder, put it into a crucible, place the crucible in a crystallization reactor containing 3g of water at the bottom, crystallize at 190°C for 12h, cool down to room temperature, dry at 120°C for 12h, and roast at 550°C for 6h to obtain the product , as detected by XRD, it also belongs to HZSM-5 molecular sieve; at the same time, the relative crystallinity of the HZSM-5 molecular sieve is 98.96%.

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Abstract

The invention discloses a synthesis method of an HZSM-5 molecular sieve adopting a dual template agent. The synthesis method comprises the steps that a silicon source, an aluminum source, a template agent, seed crystal and water are mixed in proportion and uniformly stirred to form gel; the gel is dried and ground into powder; the powder is crystallized in a reaction kettle containing water at the bottom; and a crystallized product is dried and calcined to obtain the product. The method does not use a raw material containing sodium ions, saves traditional ammonium exchange, washing and calcination processes, avoids separation of the product and mother liquid in the traditional crystallization technology, does not use expensive organic amine as the template agent, and has the characteristics of low cost, small waste liquid quantity, high yield and the like.

Description

technical field [0001] The invention belongs to the field of preparation of ZSM-5 molecular sieve catalysts, in particular to a method for synthesizing HZSM-5 molecular sieves using double templates. Background technique [0002] HZSM-5 molecular sieve has a unique pore structure and adjustable acidity, and can be used as a catalyst or adsorption separation material. The traditional method is to exchange NaZSM-5 with ammonium, and then roast to obtain HZSM-5. Therefore, it can be understood that if HZSM-5 is directly synthesized without introducing alkali metal ions in the preparation process, the ion exchange step can be omitted, thereby simplifying making process. Bibby was first published in literature (D.M.Bibby, N.B.Milestone, L.P.Aldridge.NH 4 + -tetraalkyllammonium systems in the synthesis of zeolites.Nature.1980,285:30-31) reported that using silicic acid, aluminum hydroxide, tetrapropylammonium hydroxide (TPAOH), and ammonia water as raw materials, hydrothermal c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72
Inventor 江永军雍晓静罗春桃
Owner CHNA ENERGY INVESTMENT CORP LTD
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