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Preparation method of composite molybdate hollow microspheres and application thereof

一种复合钼酸盐、空心微球的技术,应用在化学仪器和方法、催化剂活化/制备、镍化合物等方向,能够解决制备成本高、形貌不可控等问题,达到高孔隙率、高有效接触面积、优越催化活性的效果

Active Publication Date: 2018-05-01
ZHEJIANG ZHISHENG ELECTRONIC TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for preparing multi-component molybdate hollow microspheres, which uses urea as a precipitating agent, in view of the key problems such as high preparation cost and uncontrollable morphology in the above preparation process. The multi-component molybdate hollow microsphere structure was successfully synthesized by applying the hydrothermal synthesis method; this synthesis method provides technical support for the systematic study of the structure-activity relationship between the microstructure and properties of multi-component molybdate nanomaterials, and also promotes the development of materials. An important step towards low-cost mass production

Method used

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  • Preparation method of composite molybdate hollow microspheres and application thereof
  • Preparation method of composite molybdate hollow microspheres and application thereof
  • Preparation method of composite molybdate hollow microspheres and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Take CuCl 2 Dissolve 1mmol in 20mL of water to obtain solution A; then dissolve 1mmol of molybdic acid in 20mL of water to obtain solution B; mix the two;

[0027] 2. Dissolve 10mmol urea in 40mL water, add the above solution; stir for 30min, move to the reaction kettle, react at 160°C for 8h; filter and wash with water, dry in a vacuum oven at 40°C; calcinate in a muffle furnace at 500°C for 2h; the sample composition is CuMoO 4 ;

Embodiment 2

[0029] 1. Take CuCl 2 x mmol, NiCl 2 y mmol, CoCl 2 Dissolve (1-x-y)mmol in 20mL water to obtain solution A; then take 2mmol of molybdic acid and dissolve it in 20mL water to obtain solution B; mix the two;

[0030] 2. Take 20mmol of urea and dissolve it in 40mL of water, add the above solution; stir for 30min, move to the reaction kettle, react at 120°C for 12h; filter and wash with water, dry in a vacuum oven at 60°C; calcinate in a muffle furnace at 500°C for 2h; the sample composition is Cu x co y Ni 1-x-y MoO 4 ;

Embodiment 3

[0032] 1. Take CuCl 2 x mmol, NiCl 2 y mmol, CoCl 2 Dissolve (1-x-y)mmol in 20mL water to obtain solution A; then take 2mmol of molybdic acid and dissolve it in 20mL water to obtain solution B; mix the two;

[0033] 2. Dissolve 30mmol of urea in 40mL of water, add the above solution; stir for 30min, move to the reaction kettle, react at 160°C for 8h; filter and wash with water, dry in a vacuum oven at 40°C; calcinate in a muffle furnace for 2h at 350°C; Cu x co y Ni 1-x-y MoO 4 ;

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Abstract

The invention discloses a preparation method of composite molybdate hollow microspheres, which comprises the following steps of: (1) taking 1 to 4mmol of MCl2 to dissolve into 20mL of water to obtainsolution A, then taking 1 to 4mmol of molybdic acid to dissolve into 20mL of water to obtain solution B, and mixing the solution A and the solution B, wherein M represents Co, Ni, and Cu; (2) taking 10 to 40mmol of urea to dissolve into 40mL of water, adding the solution and uniformly stirring; (3) transferring the mixed solution to a reaction kettle, and performing a reaction for 6 to 12h at a temperature of 120 to 160 DEG C; (4) carrying out extraction filtration and washing, and drying by a vacuum drying oven at a temperature of 40 to 60 DEG C; (5) calcining for 2 to 4h by a muffle furnaceat a temperature of 350 to 500 DEG C. The composite molybdate hollow microspheres prepared by the invention have a large effective contact area and high porosity; a process is simple, and raw materials are cheap and easy to obtain; in the preparing process, a surfactant and the like are not used as structure-directing agents for controlling the morphology; the synthetic polybasic molybdate hollowmicrospheres, due to microstructure characteristics, are expected to show the excellent catalytic activity as a high-activity catalyst in the aspect of producing hydrogen by catalyzing ammonia boraneto hydrolyze for example.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to a method for preparing composite molybdate hollow microspheres and its application in catalyzing the hydrolysis of ammonia borane to produce hydrogen. Background technique [0002] The molybdate compound is combined with (MoO4)2- and one or more cations to form molybdates with different properties. For example, it can be combined with La, Eu, etc. to form a fluorescent powder material; it can be formed with Co, Ni, and Cu Catalyst with superior catalytic performance. Different combinations of molybdates can perform well in the fields of optics, electronics, catalysis, and medical treatment, so molybdates are important members of inorganic functional materials. [0003] In recent years, the preparation method of molybdate nanomaterials has been a research hotspot. The traditional high-temperature solid-phase method requires higher temperatures, and cannot guarantee t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/885C01B3/04
CPCC01B3/042B01J23/002B01J23/885B01J2523/00B01J35/70B01J35/52B01J2235/15B01J2235/30B01J2523/17B01J2523/68B01J2523/845B01J2523/847B01J37/031C01B3/065Y02E60/36C01G39/00C01G51/006C01P2004/03C01P2004/04C01P2002/72C01P2006/12C01G53/006C01P2004/16B01J35/397B01J35/613B01J37/009B01J37/04B01J37/06B01J37/08C01B3/06C01G39/006C01G53/40C01P2004/34B01J35/51
Inventor 廖锦云卢东升李浩肖定书
Owner ZHEJIANG ZHISHENG ELECTRONIC TECH CO LTD
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