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Method for synthesizing molecular sieve under solvent-free condition through grinding solid phase raw materials

A solvent-free and raw material-free technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of narrow synthesis range, limited application, increased production cost, etc., and achieve high yield and Increased single-pot utilization rate, huge industrial application prospects, and simplified synthesis steps

Active Publication Date: 2012-08-08
淮安六元环新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the types of molecular sieves synthesized by this method are limited, and it is only suitable for the synthesis of phosphorus-aluminum framework molecular sieves at present.
Moreover, the high price of ionic liquids greatly limits its application in industrial fields.
[0003] At present, the synthetic route that can be applied to industrial production on a large scale is still the hydrothermal route, because other synthetic routes involve the use of organic solvents, which increases the production cost, and the applicable synthetic range is narrow

Method used

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  • Method for synthesizing molecular sieve under solvent-free condition through grinding solid phase raw materials
  • Method for synthesizing molecular sieve under solvent-free condition through grinding solid phase raw materials
  • Method for synthesizing molecular sieve under solvent-free condition through grinding solid phase raw materials

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Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1: the preparation of pure silicon ZSM-5 sample

[0031] First, weigh the solid raw materials: 0.285 grams of amorphous silicon dioxide, 0.5276 grams of sodium silicate nonahydrate, 0.24 grams of tetrapropylammonium bromide and 0.46 grams of ammonium chloride and pour them into a mortar, then grind and mix them for 15 minutes. Minutes later, the reaction mixture was put into a polytetrafluoroethylene-lined steel reactor, reacted at 180°C for 1 day, the reaction product was fully washed with deionized water, and dried at 80°C for more than 12 hours to obtain Final product. The chemical ratio of the system is as follows: Na 2 O:Al 2 o 3 : SiO 2 :H 2 O:R is 0.2:0:1:3:0.1.

[0032] attached figure 1 According to the XRD characterization results of the product, it can be seen that the product has a typical MFI structure and has a high degree of crystallinity.

[0033] attached figure 2 It is a scanning electron microscope photo of the product, and the el...

Embodiment 2

[0034] Embodiment 2: the preparation of ZSM-5 sample containing aluminum

[0035] First solid raw materials: 0.285 gram of amorphous silicon dioxide, 1.319 gram of sodium silicate nonahydrate, 0.72 gram of tetrapropylammonium bromide, 0.013 gram of boehmite and 0.69 gram of ammonium nitrate are weighed and poured into a mortar, and then Grinding and mixing, after grinding for 15 minutes, put the reaction mixture into a polytetrafluoroethylene-lined steel reaction kettle, react at 180°C for 2 days, fully wash the reaction product with deionized water, and put it at 80°C Dry for more than 12 hours to get the final product. The chemical ratio of the system is as follows: Na 2 O:Al 2 o 3 : SiO 2 :H 2 O:R is 0.5:0.0125:1:4.5:0.3.

[0036] attached image 3 It is the XRD characterization result of the product, and it can be known that the product is MFI pure phase from the XRD characteristic peak.

[0037] attached Figure 4 It is a scanning electron microscope photo of the...

Embodiment 3

[0038] Embodiment 3: the preparation of ZSM-5 sample containing gallium

[0039] First, weigh the solid raw materials: 0.285 grams of amorphous silicon dioxide, 1.0552 grams of sodium silicate nonahydrate, 0.48 grams of tetrapropylammonium bromide, 0.084 grams of gallium oxide and 0.825 grams of ammonium carbonate, pour them into the mortar, and then grind After mixing and grinding for 15 minutes, the reaction mixture was put into a polytetrafluoroethylene-lined steel reactor and reacted at 180°C for 1 day. The reaction product was fully washed with deionized water and dried at 80°C for 12 hours or more to obtain the final product. The chemical ratio of the system is as follows: Na 2 O: Ga 2 o 3 : SiO 2 :H 2O:R is 0.4:0.05:1:4.5:0.2.

[0040] attached Figure 5 It is the XRD characterization result of the product, and it can be known that the product is MFI pure phase from the XRD characteristic peak.

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Abstract

The invention relates to a method for preparing a molecular sieve, aiming to provide a method for synthesizing a molecular sieve under a solvent-free condition through grinding solid phase raw materials. The method comprises the following steps of: grinding and mixing the pre-weighed solid raw materials which include silicon sources, metal atom sources, an organic template agent, and an alkalinity regulator, putting the grinded material into a reactor, and performing a crystallization reaction for 1-8 days at a temperature ranged from 80 DEG C to 180 DEG C; and drying for over 12 hours at a temperature of 80 DEG C after washing the reaction product thoroughly by using deionized water to obtain a final product. A ZSM-5 molecular sieve, a Beta molecular sieve, a ZSM-39 molecular sieve, and a SOD molecular sieve, which have a good crystallinity and a controllable silicon-aluminum ratio, can be prepared through the method provided by the invention. The synthetic route only involves a mixture of the raw materials without a use of any solvents, which simplifies the synthetic process compared to the traditional method, improves the yield rate and the single reactor utilization rate greatly, reduces the production cost greatly, saves energy and reduces emission, and has a wide industrial application prospect.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for synthesizing molecular sieves directly by grinding solid-phase raw materials under solvent-free conditions. Background technique [0002] Molecular sieves, especially silica-alumina molecular sieves, are widely used in various catalysis due to their unique pore characteristics, good adsorption performance and shape selectivity, high specific surface area, good thermal stability and hydrothermal stability. Reacting. Molecular sieve research is closely related to industry, and the exploration of new molecular sieve synthesis routes has become a hot spot for researchers. The earliest synthesis route of molecular sieves is hydrothermal synthesis, which is characterized by using a large amount of water as a solvent for synthesis. Later, the route of solvothermal method was discovered, which is characterized in that organic solvents such as alcohols replaced wat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/40
Inventor 肖丰收任利敏吴勤明孟祥举杨承广朱龙凤
Owner 淮安六元环新材料有限公司
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