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A kind of preparation method of zsm-5 molecular sieve

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of irregular grain morphology of molecular sieve, and achieve complete grain and process. Simple, high-yield effects

Active Publication Date: 2017-08-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, according to the results of electron microscope photos, the molecular sieve crystal grains are irregular in shape and do not have the regular morphology of ZSM-5 molecular sieves.

Method used

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  • A kind of preparation method of zsm-5 molecular sieve
  • A kind of preparation method of zsm-5 molecular sieve
  • A kind of preparation method of zsm-5 molecular sieve

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preparation example Construction

[0018] The preparation method of ZSM-5 molecular sieve provided by the present invention is characterized in that the first mixture composed of the first silicon source, inorganic base, seed crystal and water is placed in a closed reaction kettle and heated to 150-200°C within 1-5 hours. The constant temperature treatment in the temperature range of ℃ is not more than 10 hours, and the second mixture formed by the second silicon source, aluminum source, inorganic alkali and water is added after cooling down to the pressure of the kettle to obtain the third mixture, and then the third mixture is heated at 140 Hydrothermal crystallization in the temperature range of -180°C for 5-20 hours and recover the product, the molar composition of the first mixture is: M 2 O / SiO 2 =0.03-0.07, H 2 O / SiO 2 =5-10, the molar composition of the third mixture is: SiO 2 / Al 2 o 3 =20-100, M 2 O / SiO 2 =0.03-0.15, H 2 O / SiO 2 =5-15, wherein M represents alkali, and the addition amount of t...

Embodiment 1

[0040] Dissolve 0.43 grams of NaOH in 18 grams of deionized water under stirring, then add 0.33 grams of ZSM-5 seed crystals and 9 grams of coarse-pore silica gel to obtain the first mixture, and its molar ratio is composed of: Na 2 O / SiO 2 =0.035,H 2 O / SiO 2 = 6.6. Put it into the autoclave, stir, heat up to 190°C for 2 hours, keep the temperature for 2 hours, cool down to zero pressure, and then add 5 grams of silica sol, 0.43 grams of NaOH, 0.83 grams of sodium aluminate and 3.7 grams of water. The second mixture, the molar ratio composition of the third mixture finally obtained is: SiO 2 / Al 2 o 3 =50, Na 2 O / SiO 2 =0.06,H 2 O / SiO 2 = 12.5, the seed crystals accounted for 3% by weight of silica.

[0041] The third mixture was then hydrothermally crystallized at a constant temperature of 170° C. for 24 hours. After cooling, the product was filtered, washed and dried.

[0042] According to XRD detection, the product is ZSM-5 molecular sieve with a relative crystal...

Embodiment 2

[0053] Dissolve 0.43 grams of NaOH in 18 grams of deionized water under stirring, then add 0.33 grams of ZSM-5 seed crystals and 9 grams of coarse-pore silica gel to obtain the first mixture, and its molar ratio is composed of: Na 2 O / SiO 2 =0.035,H 2 O / SiO 2 = 6.6. Put it into the autoclave, stir, heat up to 190°C for 2 hours, keep the temperature for 2 hours, cool down to zero pressure, and then add 5 grams of silica sol, 0.3 grams of NaOH, 0.64 grams of sodium aluminate and 2 grams of water. The second mixture, the molar ratio composition of the third mixture finally obtained is: SiO 2 / Al 2 o 3 =65, Na 2 O / SiO 2 =0.05,H 2 O / SiO 2 =7, the seed crystal accounts for 3% by weight of the silica.

[0054] The third mixture was hydrothermally crystallized at 165° C. for 15 hours, and the cooled product was filtered, washed and dried.

[0055] According to XRD detection, the product is ZSM-5 molecular sieve with a relative crystallinity of 140%.

[0056] Molecular siev...

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Abstract

A preparation method of ZSM-5 molecular sieve is characterized by comprising the following steps: carrying out hydro-thermal treatment on a first mixture composed of a first silicon source, alkali, seed crystal and water, adding the first mixture which has undergone the hydro-thermal treatment into a second mixture composed of a second silicon source, an aluminium source, alkali and water so as to obtain a third mixture, and carrying out hydrothermal crystallization on the third mixture, wherein the first silicon source is silica gel and the second silicon source is silica sol or water glass. According to the preparation method, the molecular sieve is synthesized without usage of a template and under conditions of low water-to-silicon ratio, controlled heating rate and two-stage crystallization. The preparation method has characteristics of high single-autoclave yield, simple process and high utilization rate of silicon. The prepared ZSM-5 molecular sieve has complete crystal grain, high degree of crystallization and specific hexagon morphology.

Description

technical field [0001] The invention relates to a preparation method of ZSM-5 molecular sieve, more specifically, relates to a preparation method of ZSM-5 molecular sieve with regular and specific morphology without using an organic template. Background technique [0002] Since ZSM-5 molecular sieve was synthesized by MOBIL company in 1972 (USP3702886), it has been widely used in many fields of petrochemical industry because of its high silicon-aluminum ratio, suitable acidity, good thermal and hydrothermal stability, such as alkane Alkylation, isomerization, disproportionation, catalytic cracking, catalytic dewaxing, methanol-to-gasoline, and methanol-to-olefin reactions. [0003] For different reactions, the required acidity of ZSM-5 molecular sieve is different, so more changes in the silicon-aluminum ratio of the molecular sieve are considered. When considering the diffusion factors of reactants and products, the grain size of molecular sieves will be considered, and th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38
Inventor 王殿中王萍冯强
Owner CHINA PETROLEUM & CHEM CORP
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