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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 problem of low crystallinity of molecular sieve, no silicon source utilization, and molecular sieve grain shape. problems such as irregular appearance, to achieve the effects of complete grains, low water-to-silicon ratio, and high yield per kettle

Active Publication Date: 2016-06-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, from the results of the electron microscope in the examples, the molecular sieve crystal grains are irregular in shape and do not have the typical morphology characteristics of ZSM-5 molecular sieve, indicating that the crystallinity of the molecular sieve is low
In addition, the invention does not involve the problem of silicon source utilization

Method used

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  • Preparation method of ZSM-5 molecular sieve

Examples

Experimental program
Comparison scheme
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preparation example Construction

[0013] The preparation method of ZSM-5 molecular sieve provided by the present invention is characterized in that the first mixture obtained by uniformly mixing silicon source, alkali, seed crystal and water is treated at a constant temperature at 150-200°C in a closed reaction kettle for no more than After 10 hours, the temperature was lowered to zero, and then the second mixture obtained by uniformly mixing the aluminum source, alkali and water was added, and the third mixture obtained was hydrothermally crystallized at 140-180°C in a closed reaction kettle for 5- 20 hours and reclaim product, wherein, the molar composition of described first mixture is: M 2 O / SiO 2 =0.03-0.07, H 2 O / SiO 2 =5-10, the amount of the seed crystal added is 1-10% by weight of the silicon source calculated as silicon dioxide, and 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.

[0014] In the present invention, the silic...

Embodiment 1

[0028] 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 11 grams of coarse-pore silica gel to obtain a molar ratio of NaOH 2 O / SiO 2 =0.03;H 2 O / SiO 2 =5.5 of the first mixture, it was placed in a closed reactor under stirring, the temperature was raised to 190° C. and kept for 2 hours, and then the temperature was lowered to zero.

[0029] 0.3 g of NaOH, 0.63 g of sodium aluminate and 5 g of water were uniformly mixed to obtain a second mixture.

[0030] The second mixture is added to the first mixture and mixed to obtain a third mixture, and the molar ratio of the third mixture is composed of: SiO 2 / Al 2 o 3=67, Na 2 O / SiO 2 =0.05,H 2 O / SiO 2 =7.

[0031] The third mixture was kept at 165° C. for 15 hours and then cooled. The product was filtered, washed and dried.

[0032] The obtained solid product was tested for crystallinity and silicon-aluminum ratio. Detected by XRD, the spectrum is s...

Embodiment 2

[0034] Dissolve 0.43 grams of NaOH in 18 grams of deionized water under stirring, then add 0.55 grams of ZSM-5 seed crystals and 11 grams of coarse-pore silica gel to obtain a molar ratio of NaOH 2 O / SiO 2 =0.03,H 2 O / SiO 2 =5.5 of the first mixture, it was placed in a closed reactor under stirring, the temperature was raised to 185° C. and kept for 4 hours, and then the temperature was lowered to zero.

[0035] 1.4 g of NaOH, 0.76 g of sodium aluminate and 5 g of water were uniformly mixed to obtain a second mixture.

[0036] The second mixture is added to the first mixture and mixed to obtain a third mixture, and the molar ratio of the third mixture is composed of: SiO 2 / Al 2 o 3 =55, Na 2 O / SiO 2 =0.13,H 2 O / SiO 2 =7.

[0037] The third mixture was kept at 165°C for 10 hours and then cooled, and the product was filtered, washed and dried.

[0038] The obtained solid product was tested for crystallinity and silicon-aluminum ratio. Detected by XRD, the spectrogra...

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Abstract

A preparation method of a ZSM-5 molecular sieve is characterized in that the method comprises the following steps: allowing a first mixture obtained by uniformly mixing a silicon source, an alkali, crystal seeds and water to stay in a closed reaction kettle at a constant temperature of 150-200DEG C for 10h or below, adding a second mixture obtained by uniformly mixing an aluminum source, the alkali and water, carrying out hydrothermal crystallization on the above obtained third mixture in the closed reaction kettle at 140-180DEG C for 5-20h, and recovering the finally obtained product, wherein a molar ratio of M2O / SiO2 of the first mixture is 0.03-0.07, a molar ratio of H2O / SiO2 of the first mixture is 5-10, the addition amount of the crystal seeds is 1-10% of the weight of the silicon source calculated by silica, a molar ratio of SiO2 / Al2O3 of the first mixture is 20-100, a molar ratio of M2O / SiO2 of the third mixture is 0.03-0.15, and a molar ratio of H2O / SiO2 of the third mixture is 5-15. The method has the advantages of no use of a template, high yield of a single kettle, and high silicon utilization rate.

Description

technical field [0001] The invention relates to a preparation method of ZSM-5 molecular sieve, more specifically, relates to a method for preparing ZSM-5 molecular sieve 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] At present, the synthesis of ZSM-5 molecular sieves can be divided into template method and non-template method. The so-called template method generally refers to the use of organic amines, ammonia water, and alcohols as templates for synthesis, and the non-template method refers to the reaction system without the above-mentioned tem...

Claims

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Application Information

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