Method for synthesizing boron-silicon and iron-silicon MTT zeolite in absence of organic structure directing agent

A technology of organic structure and directing agent, applied in the direction of crystalline aluminosilicate zeolite, iron silicate, inorganic chemistry, etc., can solve the problems of increased cost, waste liquid, exhaust gas emission, etc. The effect of purity, good reactivity

Active Publication Date: 2020-04-07
JIAXING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This not only increases the cost of synthesis, but also leads to the discharge of a large amount of waste liquid and waste gas.

Method used

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  • Method for synthesizing boron-silicon and iron-silicon MTT zeolite in absence of organic structure directing agent
  • Method for synthesizing boron-silicon and iron-silicon MTT zeolite in absence of organic structure directing agent
  • Method for synthesizing boron-silicon and iron-silicon MTT zeolite in absence of organic structure directing agent

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Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1: Preparation of solid ferrosilicon precursor

[0028] First, dissolve 0.2 g NaOH in 3 g H 2 O, then this solution was added dropwise to 30 g of aqueous silica sol with a mass fraction of 40% under stirring conditions. Then, ferric nitrate solution (dissolving a certain amount of ferric nitrate nonahydrate in 10gH 2 O) was added dropwise to the above solution. Then, the solution was stirred for another 2 h, and placed in an oven at 150° C. for 12 h to evaporate the water in the solution. In this way, solid ferrosilicon precursors can be obtained. In this solution, the masses of ferric nitrate nonahydrate added were 0.4g, 0.8g, and 8g respectively. Therefore, the Si / Fe molar ratios of the obtained solid ferrosilicon precursors are 200, 100, and 10, respectively.

Embodiment 2

[0029] Embodiment 2: Preparation of solid silicon boron precursor

[0030] First, dissolve 0.2 g NaOH in 3 g H 2 O, then this solution was added dropwise to 20 g of aqueous silica sol with a mass fraction of 40% under stirring conditions. Next, with sodium metaborate solution (a certain amount of sodium metaborate tetrahydrate is dissolved in 10g H 2 O) was added dropwise to the above solution. Then, the solution was stirred for another 2 h, and placed in an oven at 150° C. for 12 h to evaporate the water in the solution. In this way, a solid silicon-boron precursor can be obtained. In this solution, the masses of sodium metaborate tetrahydrate added were 0.09g, 0.61g, and 1.8g, respectively. Therefore, the Si / B molar ratios of the obtained solid silicon-boron precursors were 200, 30, and 10, respectively.

Embodiment 3

[0031] Embodiment 3: No organic structure directing agent method synthesis Fe-MTT zeolite

[0032] 1.56g solid ferrosilicon precursor (Si / Fe=100), 0.3g Na 2 SiO 3 9H 2 O, 1.9g ethanol and 0.16g all-silicon MTT (accounting for 10% of the mass ratio of solid precursor) seed crystals were placed in the grinding mill, and then crystallized at 140°C for 4 days to complete crystallization, and the product was suction filtered and dried get the product. The reaction raw material ratio is as follows:

[0033] SiO 2 :Fe:Na 2 O: ethanol = 1:0.01:0.04:1.5

[0034] Through XRD analysis, its structure is MTT zeolite ( figure 1 ), and the Fe-MTT zeolite obtained by this method can be seen that its iron has entered the zeolite framework ( figure 2 ).

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Abstract

The invention relates to a preparation method of a molecular sieve, and aims to provide a method for synthesizing boron-silicon and iron-silicon MTT zeolite in the absence of an organic structure directing agent. The method comprises the following steps: putting a solid silicon iron or silicon boron precursor, an alkali source, a seed crystal and ethanol into a mortar, and grinding; transferring an obtained mixture into a reaction kettle, and reacting for 15-6d at the temperature of 120-180 DEG C; and carrying out suction filtration on an obtained product, and drying to obtain the iron-siliconzeolite molecular sieve or boron-silicon zeolite molecular sieve. The product prepared by the method provided by the invention maintains good crystallinity and purity, and has good reaction activity.According to the present invention, environment-friendly ethanol is adopted as a zeolite pore channel filler, and only a small amount of the seed crystal is added as the guiding agent of the target product, such that the solid phase state is always maintained during the whole synthesis process, and the unnecessary waste gas and waste liquid discharge and loss during the production process are reduced. The adopted inorganic raw materials are environment-friendly and relatively low in price, so that the method has important significance in the field of actual chemical production.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for synthesizing borosilicate and iron-silicon MTT zeolites in the presence of no organic structure-directing agent. Background technique [0002] As a typical porous material, zeolite molecular sieve is widely used in the fields of catalysis, adsorption, separation and ion exchange. Zeolite molecular sieves currently widely used in industry mainly include FAU, MFI, Beta, MOR, MTT, etc. Among them, MTT, as a zeolite with a one-dimensional ten-membered ring channel structure, has been widely used in the process of hydroisomerization reaction. It is worth pointing out that the zeolites used in these applications are all in the form of aluminosilicates. Although great progress has been made in the green synthetic route of silica-alumina zeolites in recent years, for example, the synthesis method without organic structure directing agent is widely used in the synt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
CPCC01B39/087C01B39/12C01B39/08C01P2002/72C01P2002/84C01P2002/80
Inventor 朱龙凤曹雪波朱杰朱连文金银樱
Owner JIAXING UNIV
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