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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 problem of high production cost and achieve the effect of regular morphology and high crystallinity

Active Publication Date: 2017-02-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN102432032 invented a method for preparing nano-silicon molecular sieves (ZSM-5), in which 0.5-5% of the mass of silicon source amino acids are added, and the prepared molecular sieves have a grain size of 40-160nm. From the perspective of the patent content, The addition of amino acids results in molecular sieves with smaller grains, but it uses expensive tetrapropylammonium hydroxide as a template, which makes the production cost higher

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

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Dissolve 1.92 grams of NaOH in 28 grams of deionized water, then add 1.12 grams of lysine and 0.87 grams of sodium aluminate, raise the temperature to 60 ° C, stir at constant temperature for 3 hours, then add 1.02 grams of n-butylamine, and then add 11.5 grams of silica gel, The molar ratio of the obtained reaction mixture is: SiO 2 / Al 2 o 3 =50,H 2 O / SiO 2 =7.8, Na 2 O / SiO2 =0.06, n-butylamine / SiO 2 =0.07, lysine / SiO 2 =0.04. The mixture was placed in a sealed stainless steel reaction vessel and crystallized at 160°C for 24 hours. After cooling, the product was filtered, washed and dried.

[0039] Detected by XRD, the obtained molecular sieve has figure 1 The standard spectrum characteristic of ZSM-5, its relative crystallinity is 105%. Its grain morphology is shown by the scanning electron microscope photo, and the sample is hexagonal, such as image 3 As shown, the average grain size is about 3um.

Embodiment 2

[0041] Dissolve 0.56 g of NaOH in 17 g of deionized water, then add 0.29 g of glycine, add 0.43 g of sodium aluminate under stirring, raise the temperature to 80°C, stir at constant temperature for 4 hours, then add 1.46 g of n-butylamine and 11.5 g of silica gel, The molar ratio of the obtained reaction mixture is: SiO 2 / Al 2 o 3 =100,H 2 O / SiO 2 =5, Na 2 O / SiO 2 =0.05, n-butylamine / SiO 2 =0.1, glycine / SiO 2 =0.02. The mixture was placed in a sealed stainless steel reaction vessel and crystallized at 160°C for 24 hours. After cooling, the product was filtered, washed and dried.

[0042] Detected by XRD, the obtained molecular sieve has figure 1 The standard spectrum characteristic of ZSM-5, its relative crystallinity is 110%. Its grain morphology is shown by the scanning electron microscope photo, and the sample is hexagonal, such as Figure 4 As shown, the average grain size is about 6um.

Embodiment 3

[0044] Dissolve 0.88 g of NaOH in 36 g of deionized water with stirring, add 0.27 g of lysine, 0.29 g of glycine, and 0.22 g of sodium aluminate, heat the mixture to 80°C, stir at constant temperature for 6 hours, and then add 2.19 Gram n-butylamine and 11.5 grams of silica gel, the reaction mixture molar ratio that obtains is: SiO 2 / Al 2 o 3 =200,H 2 O / SiO 2 =10, Na 2 O / SiO 2 =0.04, n-butylamine / SiO 2 =0.15, lysine / SiO 2 =0.01, glycine / SiO 2 =0.02. The mixture was placed in a sealed stainless steel reaction vessel, and crystallized at 150°C for 30 hours. After cooling, the product was filtered, washed and dried.

[0045] Detected by XRD, the obtained molecular sieve has figure 1 The standard spectrum characteristic of ZSM-5, its relative crystallinity is 110%. Its grain morphology is shown by the scanning electron microscope photo, and the sample is hexagonal, such as Figure 5 As shown, the average grain size is about 5um.

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Abstract

The invention discloses a method for preparing a ZSM-5 molecular sieve. The method comprises the following steps: crystallizing homogeneous slurry containing a silicon source, an aluminum source, an alkali source, a templating agent and water in a sealed reaction kettle under a hydrothermal condition, and recycling a product. The method is characterized in that the homogeneous slurry is prepared by the following steps: firstly mixing the aluminum source, the alkali source, water and a second templating agent evenly; heating to 50-100 DEG C, stirring for 1-10 hours, and then adding a first templating agent and the silicon source; and stirring to obtain the homogeneous slurry. According to the preparation method of the ZSM-5 molecular sieve disclosed by the invention, a large-crystal molecular sieve of which the mean grain size is greater than 2 microns can be obtained; and the molecular sieve is regular in morphology and high in degree of crystallinity.

Description

technical field [0001] The present invention relates to a method for preparing ZSM-5 molecular sieve, more specifically, relates to a method for preparing ZSM-5 molecular sieve with complete grain and high crystallinity. 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, such as alkylation, isomerization, disproportionation, catalytic cracking, catalytic dewaxing and methanol synthetic gasoline and other reaction processes middle. Among them, the silicon-aluminum ratio of ZSM-5 molecular sieve is considered more, and the crystal grains of molecular sieves are rarely involved. However, for ZSM-5 molecular sieves used in catalytic cracking catalysts, due to high temperature regeneration, Small grains are obviously not suitable, because it will affect the stability of molecular sieves; and for reactions that emphasize shape-selective catalysis, small ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40
CPCC01B39/40
Inventor 王殿中冯强罗一斌慕旭宏
Owner CHINA PETROLEUM & CHEM CORP