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Micro-spherical porous basic magnesium borate and ionothermal synthesis method of 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 cheap raw materials, good thermal stability and suitable for industrial promotion

Active Publication Date: 2014-11-12
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chen Aimin et al. synthesized magnesium borate salt microspheres by using surfactants polyvinylpyrrolidone (PVP) and sodium dodecyl sulfate (SDS) assisted water bath-calcination thermal conversion method[ Mater. Lett. , 2012, 68, 187-189; Adv. Mater. Res. , 2012, 486, 260-264], and the synthesis of borate nanomaterials by ionothermal method has not yet been published

Method used

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  • Micro-spherical porous basic magnesium borate and ionothermal synthesis method of magnesium borate nano-superstructure
  • Micro-spherical porous basic magnesium borate and ionothermal synthesis method of magnesium borate nano-superstructure
  • Micro-spherical porous basic magnesium borate and ionothermal synthesis method of magnesium borate nano-superstructure

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Experimental program
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Effect test

Embodiment 1

[0031] Using KOH as a pH regulator to adjust the pH of N,N-dimethylformamide nitrate ionic liquid to 8.0-9.0, 4.066 g MgCl 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 min, transfer it to a polytetrafluoroethylene-lined reactor, raise the temperature to 160 oC for 12 hours, cool down naturally after the reaction, wash, filter, and dry the product to obtain porous basic magnesium borate superstructure nanomaterials , the filtrate is recovered as solvent recycling; the product obtained is placed in an air roaster, and the temperature is raised to 650 oC at a heating rate of 2 oC / min for 6 h, and the obtained product is washed, filtered, and dried to obtain a porous magnesium borate superstructure nanomaterials.

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

Embodiment 2

[0034] NaOH was used as the pH regulator to adjust the pH of N,N-dimethylformamide nitrate ionic liquid to 8.0-8.5, and then 4.066 g MgCl 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 min, added a small amount of NaOH to ensure that the pH was maintained at 8.0-8.5, then transferred it to a polytetrafluoroethylene-lined reactor, raised the temperature to 150 oC for 12 h, and cooled down naturally after the reaction. The product was washed, filtered, and dried to obtain a porous basic magnesium borate superstructure nanomaterial, and the filtrate was recovered as a solvent for recycling; the obtained product was placed in an air roaster, and the temperature was raised to 600 oC at a heating rate of 5 oC / min for 12 h. The obtained product is the porous magnesium borate superstructure nano material after washing, filtering and drying.

[0035] 82...

Embodiment 3

[0037] NaOH was used 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 5.128 g Mg(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, stirred for 10 min, added a small amount of KOH to ensure that its pH was maintained at 8.0-8.5, then transferred it to a polytetrafluoroethylene-lined reactor, raised the temperature to 140 °C for 12 h, and cooled down naturally after the reaction. The product was washed, filtered, and dried to obtain a porous basic magnesium borate superstructure nanomaterial, and the filtrate was recovered as a solvent for recycling; the obtained product was placed in an air roaster, and the temperature was raised to 700 oC at a heating rate of 10 oC / min for 2 h. , the obtained product is washed, filte...

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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 Applications(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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