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Method for synthesizing mesoporous molybdenum disulphide by taking mesoporous silica molecular sieve as hard template

A mesoporous silica and molybdenum disulfide technology, applied in the direction of molybdenum sulfide, etc., can solve the problems of limited loading of active components, high price of molybdenum-based catalysts, long process flow, etc., and achieve small catalyst usage and tar recovery. High rate, promote the effect of sufficient diffusion

Inactive Publication Date: 2012-07-18
CHANGAN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The catalyst systems studied in the early stages of people mainly include catalysts such as iron series, transition metals, and molecular sieves (Li Baoqing et al., Research on Coal Hydropyrolysis in my country, Journal of Fuel Chemistry, 1995, 23 (2) 192-196; Metta Chareonpanich et al. Effect of catalysts on yields of monocyclic aromatic hydrocarbon in hydrocarcking of coal volatile matter. Fuel, 1995, 74(11): 1636-1640; Catalysis, Chinese Journal of Process Engineering, 2007, 12: 1107-1112), wherein molybdenum-based catalysts have a high tar conversion rate and are valued by people, but the price of molybdenum-based catalysts is relatively high. In order to reduce the amount of molybdenum-based catalysts, people use high The active carrier (γ-alumina, molecular sieve, etc.) loads the molybdenum catalyst, and the general loading method is the impregnation method, but the loading amount of the active component in the impregnation method is limited to a certain extent, such as MoO 3 The content usually only reaches 20% (wt), and it is very difficult to exceed 25% (wt)
At the same time, in order to load more active components, it is often necessary to impregnate, dry, and roast many times, and the process is long.

Method used

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  • Method for synthesizing mesoporous molybdenum disulphide by taking mesoporous silica molecular sieve as hard template
  • Method for synthesizing mesoporous molybdenum disulphide by taking mesoporous silica molecular sieve as hard template
  • Method for synthesizing mesoporous molybdenum disulphide by taking mesoporous silica molecular sieve as hard template

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1. Add 5 mL of ethanolamine to 20 mL of deionized water, stir evenly, and adjust the pH of the solution to 5 with hydrochloric acid having a concentration of 10% by mass to obtain a hydrochloric acid solution of ethanolamine;

[0025] Step 2: Add 2 g of ammonium tetrathiomolybdate to the hydrochloric acid solution of ethanolamine described in step 1, stir for 1 hour, and leave it to stand at room temperature for 12 hours, filter to obtain a precipitate, then wash the precipitate with water and anhydrous ethanol in turn, and finally The washed precipitate is vacuum-dried to obtain a precursor;

[0026] Step 3: Dissolve 1 g of the precursor described in Step 2 in a mixed solution of 10 mL of water and 10 mL of anhydrous methanol, add 0.5 g of mesoporous silica molecular sieve SBA-16 to the dissolved mixed solution, and stir and react for 2 hours. Ultrasonic for 2h to obtain a solid-liquid mixture;

[0027] Step 4: Filter the solid-liquid mixture described in Step 3,...

Embodiment 2

[0031] Step 1. Add 11 mL of diethanolamine to 22 mL of deionized water, stir evenly, and adjust the pH of the solution to 5 with hydrochloric acid having a concentration of 10% by mass to obtain a hydrochloric acid solution of diethanolamine;

[0032] Step 2, adding 4g of ammonium tetrathiomolybdate to the hydrochloric acid solution of diethanolamine described in step 1, stirring for 2h, then leaving it to stand at room temperature for 24h, filtering to obtain a precipitate, and then washing the precipitate with water and anhydrous ethanol in turn, Finally, the washed precipitate is vacuum-dried to obtain a precursor;

[0033] Step 3: Dissolve 2g of the precursor described in Step 2 in a mixed solution of 17mL of water and 17mL of anhydrous methanol, add 1g of mesoporous silica molecular sieve KIT-6 to the dissolved mixed solution, stir and react for 2h with Ultrasonic sonication was carried out for 3h to obtain a solid-liquid mixture;

[0034]Step 4: Filter the solid-liquid ...

Embodiment 3

[0038] Step 1. Add 8 mL of triethanolamine to 20 mL of deionized water, stir evenly, and adjust the pH of the solution to 6 with hydrochloric acid having a concentration of 10% by mass to obtain a hydrochloric acid solution of triethanolamine;

[0039] Step 2: Add 2g of ammonium tetrathiomolybdate to the hydrochloric acid solution of triethanolamine described in step 1, stir and react for 1.5h, leave it to stand at room temperature for 20h, filter to obtain a precipitate, and then wash the precipitate with water and absolute ethanol in turn , and finally the washed precipitate is vacuum-dried to obtain the precursor;

[0040] Step 3: Dissolve 1 g of the precursor described in Step 2 in a mixed solution of 10 mL of water and 10 mL of anhydrous methanol, add 0.78 g of mesoporous silica molecular sieve KIT-6 to the dissolved mixed solution, and stir for 3 hours. Ultrasonic for 2.5h to obtain a solid-liquid mixture;

[0041] Step 4: Filter the solid-liquid mixture described in St...

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Abstract

The invention discloses a method for synthesizing mesoporous molybdenum disulphide by taking a mesoporous silica molecular sieve as a hard template. The method comprises the following steps of: firstly, preparing a hydrochloric acid solution of alcohol amine; secondly, adding ammonium tetrathiomolybdate, standing at room temperature after stirred reaction, filtering, cleaning and drying in vacuumto obtain a precursor; thirdly, dissolving the precursor into water and absolute methanol, adding the mesoporous silica molecular sieve, and carrying out ultrasonography after stirred reaction to obtain a solid and liquid mixture; fourthly, placing the solid and liquid mixture into a muffle furnace after filtering, cleaning and drying, raising the temperature to 400-450 DEG C under the protectionof hydrogen, then, preserving the temperature for 1-2h, and cooling to the room temperature to obtain mesoporous molybdenum disulphide powder containing the mesoporous silica molecular sieve; and fifthly, cleaning 1-5 times by using an HF (Hydrogen Fluoride) aqueous solution and drying to obtain the mesoporous molybdenum disulphide. The mesoporous molybdenum disulphide synthesized by using the method provided by the invention is high in catalytic activity, the yield of tar obtained in coal pyrolysis reaction is high, and the using amount of catalysts is small, and no assistant is needed.

Description

technical field [0001] The invention belongs to the technical field of inorganic porous materials, and in particular relates to a method for synthesizing mesoporous molybdenum disulfide by using mesoporous silica molecular sieve as a hard template. Background technique [0002] Compared with the increasingly scarce petroleum resources and the scarce natural gas resources, coal is not only the main energy resource in my country, but also the source of many important chemical raw materials and chemicals. At present, the utilization efficiency of coal in my country is very low. Therefore, how to comprehensively utilize coal resources more reasonably, efficiently and cleanly is not only a major concern of the country, but also of the majority of scientific researchers and related enterprises. [0003] Through coal pyrolysis, the composition and structural characteristics of coal are used to prepare high value-added chemicals and substitute oil and gas products, and the directio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06
Inventor 阎鑫赵鹏艾涛
Owner CHANGAN UNIV
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