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A kind of ionothermal synthesis method of microspherical porous basic magnesium borate and magnesium borate nano superstructure

A synthesis method and technology of magnesium borate, applied in borate, nanotechnology, nanotechnology and other directions, to achieve the effects of low synthesis temperature, suitable for industrial promotion and low energy consumption

Active Publication Date: 2016-06-01
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

ChenAimin et al. used surfactants polyvinylpyrrolidone (PVP) and sodium dodecyl sulfate (SDS) to assist water bath-calcination thermal conversion method to synthesize magnesium borate salt microspheres[ Mater. Lett. ,2012,68,187-189; Adv. Mater. Res. ,2012,486,260-264], and the use of ionothermal method to synthesize borate nanomaterials has not yet been published

Method used

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  • A kind of ionothermal synthesis method of microspherical porous basic magnesium borate and magnesium borate nano superstructure
  • A kind of ionothermal synthesis method of microspherical porous basic magnesium borate and magnesium borate nano superstructure
  • A kind of ionothermal synthesis method of microspherical porous basic magnesium borate and magnesium borate nano superstructure

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Experimental program
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Effect test

Embodiment 1

[0031] Use KOH as a pH regulator to adjust the pH of N,N-dimethylformamide nitrate ionic liquid to 8.0-9.0, and 4.066gMgCl 2 ?6H 2 O is added to the ionic liquid with a pH of 8.0-9.0 under stirring, and then press Mg 2+ :H 3 BO 3 Add H to the mixture at a molar ratio of 1:2 3 BO 3 , after stirring for 10 minutes, transfer it to a polytetrafluoroethylene-lined reaction kettle, raise the temperature to 160oC for 12 hours, cool down naturally after the reaction, wash, filter and dry the product to obtain porous basic magnesium borate superstructure nanomaterials, and the filtrate Recover as a solvent for recycling; place the obtained product in an air roaster, heat up to 650oC at a heating rate of 2oC / min for 6h, and the obtained product is washed, filtered, and dried to become a porous magnesium borate superstructure nanomaterial.

[0032] 82% of the size distribution of the basic magnesium borate nano-superstructure prepared in this example is 4.5-5.5 μm, and 80% of the si...

Embodiment 2

[0034] Use NaOH as the pH regulator to adjust the pH of the N,N-dimethylformamide nitrate ionic liquid to 8.0-8.5, and then add 4.066gMgCl 2 ?6H 2 O is added to the ionic liquid with a pH of 8.0-8.5 under stirring, and then press Mg 2+ :H 3 BO 3 Add H to the mixture at a molar ratio of 2:3 3 BO 3 , stirred for 10 minutes, added a small amount of NaOH to ensure that its pH was maintained at 8.0-8.5, then transferred it to a polytetrafluoroethylene-lined reactor, raised the temperature to 150oC and reacted for 12 hours, and cooled down naturally after the reaction, and the product was washed, Filtrate and dry to obtain porous basic magnesium borate superstructure nanomaterials, and the filtrate is recovered as a solvent for recycling; the resulting product is placed in an air roaster, and the temperature is raised to 600oC at a heating rate of 5oC / min for 12h, and the obtained product is washed, Filtration and drying are porous magnesium borate superstructure nanomaterials....

Embodiment 3

[0037] Use NaOH as a pH regulator to adjust the pH of the mixture of N,N-dimethylformamide hydrochloride ionic liquid and water at a volume ratio of 6:1 to 7.5-8.5, and then add 5.128gMg(NO 3 ) 2 ?6H 2 O is added to the ionic liquid with a pH of 8.0-8.5 under stirring, and then press Mg 2+ :Na 2 B 4 o 7 10H 2 O molar ratio is 2:1, adds Na in the mixed solution 2 B 4 o 7 10H 2 O, stir for 10 minutes, add a small amount of KOH to ensure that the pH is maintained at 8.0-8.5, then transfer it to a polytetrafluoroethylene-lined reactor, heat up to 140oC for 12 hours, cool down naturally after the reaction, and wash the product , filtered, and dried to obtain porous basic magnesium borate superstructure nanomaterials, and the filtrate is recycled as a solvent for recycling; the resulting product is placed in an air roaster, and the temperature is raised to 700oC at a heating rate of 10oC / min for 2 hours, and the obtained product is washed , filtering, and drying are porous...

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Abstract

The invention relates to micro-spherical porous basic magnesium borate and an ionothermal synthesis method of a magnesium borate nano-superstructure, relating to the synthesis, self-assembly and preparation of nano materials. The method comprises the following steps: by adopting mixed liquid of ionic liquid and a certain volume of water as a solvent, adopting inorganic alkali as a pH value regulator and taking inorganic magnesium salt and borate as raw materials, dissolving the raw materials into the ionic liquid for performing ion thermal reaction to achieve confined self-assembly growth of a product by virtue of the technological conditions of controlling the raw material ratio and controlling the volume ratio of the ionic liquid to water, thereby preparing a basic magnesium borate nano-superstructure, and then roasting to obtain the magnesium borate nano-superstructure. Compared with a conventional three-dimensional nano-material hydrothermal synthesis process, the synthesis method disclosed by the invention has the advantages that the synthesis method is simple in process, mild in condition and cheap and easily-available in raw material, does not have any additives, and can be used for achieving controllable self-assembly of a basic magnesium borate nano material by using micro bubbles in the ionic liquid; moreover, the ionic liquid can be recycled, so that the synthesis method is easy in industrial popularization.

Description

technical field [0001] The invention relates to an ion thermal synthesis method of microspherical porous basic magnesium borate nano superstructure, which belongs to the technical field of inorganic chemical industry. Background technique [0002] In recent years, the preparation of three-dimensional nanomaterials by self-assembly of low-dimensional nanostructure units has attracted more and more attention due to its unique structure, high specific surface area, and low density. At present, three-dimensional nanomaterials have been widely used in sewage treatment, catalysts and catalyst carriers, electrochemistry, drug sustained release and other fields, showing significant application advantages compared with low-dimensional nanomaterials. However, at present, the synthesis of three-dimensional nanomaterials mainly uses hydrothermal method and solvothermal method, which usually require the addition of additional templates to assist in inducing their growth. The templates ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/12B82Y40/00B82Y30/00
Inventor 朱万诚张照强于游王汝国张琳琳朱林张强
Owner QUFU NORMAL UNIV
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