Method for preparing nanometer molybdenum disulfide by aid of microemulsion system

A nano-molybdenum disulfide and microemulsion technology, which is applied in the direction of molybdenum sulfide and nanotechnology, can solve the problems that have not been seen in the preparation of nano-molybdenum disulfide, and achieve the effect of uniform particles, controllable particle size, and good stability

Inactive Publication Date: 2012-08-01
XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] So far, there is no report on the preparat...

Method used

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  • Method for preparing nanometer molybdenum disulfide by aid of microemulsion system
  • Method for preparing nanometer molybdenum disulfide by aid of microemulsion system
  • Method for preparing nanometer molybdenum disulfide by aid of microemulsion system

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Experimental program
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Effect test

Embodiment 1

[0019] A kind of method adopting microemulsion system to prepare nano molybdenum disulfide comprises the steps:

[0020] Step 1, adding oxalic acid to the sodium molybdate solution with a concentration of 0.05mol / L to reduce it to tetravalent sodium molybdate, the ratio of sodium molybdate to oxalic acid is 1:1, and the reaction temperature is 65°C. The reaction time is 75 minutes;

[0021] Step 2, adding sodium sulfide to the solution obtained in step 1 to make it vulcanized, the ratio of the amount of sodium sulfide to sodium molybdate in step 1 is 3: 1, the reaction temperature is 75 ° C, and the reaction time is 90 min;

[0022] Step 3, use TritonX100, isoamyl alcohol, n-heptane, the solution obtained in the above step 2 and secondary deionized water to configure microemulsion a; use TritonX100, isoamyl alcohol, n-heptane, 1mol / L hydrochloric acid and secondary Prepare microemulsion b with deionized water, then add all microemulsion b into microemulsion a, carry out acid ...

Embodiment 2

[0026] A kind of method adopting microemulsion system to prepare nano molybdenum disulfide comprises the steps:

[0027] Step 1, add hydroxylamine hydrochloride in the potassium molybdate solution that concentration is 0.03mol / L and reduce it to tetravalent potassium molybdate, the ratio of the amount of potassium molybdate and hydroxylamine hydrochloride substance is 1: 1.3, and the reaction temperature is 75 ℃, reaction time 85min;

[0028] Step 2, adding potassium sulfide to the solution obtained in step 1 to make it vulcanized, the ratio of potassium sulfide to the amount of potassium molybdate in step 1 is 4: 1, the reaction temperature is 85 ° C, and the reaction time is 100 min;

[0029] Step 3, use TritonX100, isoamyl alcohol, n-heptane, the solution obtained in the above step 2 and secondary deionized water to configure microemulsion a; use TritonX100, isoamyl alcohol, n-heptane, 1mol / L hydrochloric acid and secondary Prepare microemulsion b with deionized water, the...

Embodiment 3

[0033] A kind of method adopting microemulsion system to prepare nano molybdenum disulfide comprises the steps:

[0034] Step 1, in the ammonium molybdate solution that concentration is 0.04mol / L, add hydroxylamine hydrochloride and reduce it to tetravalent ammonium molybdate, the ratio of the amount of ammonium molybdate and hydroxylamine hydrochloride substance is 1: 1.2, and the reaction temperature is 70 ℃, reaction time 80min;

[0035] Step 2, adding sodium sulfide to the solution obtained in step 1 to make it vulcanized, the ratio of sodium sulfide to the amount of ammonium molybdate in step 1 is 3: 1, the reaction temperature is 80 ° C, and the reaction time is 95 min;

[0036]Step 3, use TritonX100, isoamyl alcohol, n-heptane, the solution obtained in the above step 2 and secondary deionized water to configure microemulsion a; use TritonX100, isoamyl alcohol, n-heptane, 1mol / L hydrochloric acid and secondary Prepare microemulsion b with deionized water, then add all m...

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Abstract

The invention provides a method for preparing nanometer molybdenum disulfide by the aid of a microemulsion system. The method includes steps of chemically reducing hexamolybdate, then adding sulfide into the hexamolybdate to perform sulfidation reaction so as to generate thiomolybdate sulfite; adding the thiomolybdate sulfite into TritonX100, isoamyl alcohol, normal heptane and secondary deionized water to form microemulsion a; adding hydrochloric acid into TritonX100, soamyl alcohol, normal heptane and secondary deionized water to form microemulsion b; adding the microemulsion b into the microemulsion a; fast mixing and stirring; leading acid sinking reaction to be thorough to obtain a product; and obtaining the nanometer molybdenum disulfide after the product is separated centrifugally, washed and dried in a vacuum manner. The preparation method is simple, reaction conditions are easy to be controlled, stability is good, generated particles are uniform, appearances are neat, and the nanometer molybdenum disulfide is expectably prepared on a large scale.

Description

technical field [0001] The invention belongs to the technical field of preparation of molybdenum-based inorganic nanometer materials, and in particular relates to a method for preparing nanomolybdenum disulfide by using a microemulsion system. Background technique [0002] Due to the advantages of large specific surface area, strong adsorption capacity, high reactivity, and strong catalytic performance, nano-molybdenum disulfide has broad application prospects in the fields of catalysis, hydrogen storage, lubrication, semiconductors, and electrode materials. The currently reported nano-molybdenum disulfide preparation methods can generally be divided into chemical methods, physical methods, and physicochemical comprehensive methods; if the state of the preparation system is different, they can also be divided into solid-phase methods, liquid-phase methods, and gas-phase methods. The chemical method is to prepare MoS through chemical reaction 2 , and achieve the purpose of r...

Claims

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Application Information

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IPC IPC(8): C01G39/06B82Y40/00
Inventor 周军兰新哲邢相栋张秋利宋永辉
Owner XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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