CN103754913A - Simple preparation method of aluminum hydroxide nanoparticle material - Google Patents

Simple preparation method of aluminum hydroxide nanoparticle material Download PDF

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CN103754913A
CN103754913A CN201410041307.6A CN201410041307A CN103754913A CN 103754913 A CN103754913 A CN 103754913A CN 201410041307 A CN201410041307 A CN 201410041307A CN 103754913 A CN103754913 A CN 103754913A
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particulate material
nano particulate
aluminium hydrate
thiocyanate
solution
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CN201410041307.6A
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CN103754913B (en
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徐伟
田果
孙倩
肖星星
夏鹏
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Fudan University
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Fudan University
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Abstract

The invention belongs to the technical field of nanometer materials and in particular relates to a simple preparation method of an aluminum hydroxide nanoparticle material. The method comprises the following steps: by taking an aluminum ion-thiocyanate radical system as a precursor, synthesizing the aluminum hydroxide nanoparticle material. The method is simple in process, mild in conditions and easy for production; the cost is low, the emission load is low, and industrialization is easily realized.

Description

A kind of simple method for preparing of aluminium hydrate nano particulate material
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of simple method for preparing of aluminium hydrate nano particulate material.
Background technology
Recently, we find that the reaction of cuprous thiocyanate and sodium hydroxide solution can directly prepare nano cuprous oxide wire.We think, this simple preparation method is relevant with the special property of thiocyanate-.[(1) xuwei, Xiao Xingxing, Xia Peng, a kind of nano cuprous oxide wire porous membrane and its preparation method and application, application for a patent for invention number: 2014100140030; (2) xuwei, Xiao Xingxing, Xia Peng, Sun Qian, field fruit, a kind of nano cuprous oxide wire material and simple method for preparing thereof, application for a patent for invention number: 2014100188097; (3) xuwei, Xiao Xingxing, Xia Peng, Sun Qian, field fruit, a kind of preparation method of nano cuprous oxide wire material, application for a patent for invention number: 2014100314653; (4) xuwei, field fruit, Xiao Xingxing, Xia Peng, Sun Qian, a kind of preparation method of trimanganese tetroxide nano particulate material, application for a patent for invention number: 2014100314102.]
As the presoma of aluminum oxide, aluminium hydroxide plays a part crucial in fabrication of new materials process.Such as, aspect fire retardant, the consumption of aluminium hydroxide accounts for the more than 80% of inorganic combustion inhibitor, accounts for the more than 50% of fire retardant total amount.Nano-aluminum hydroxide has many advantages such as Heat stability is good, is widely used in fire retardant, plastics, rubber, paper and fiber.Nano-aluminum hydroxide is also used to expansion steel-structure fireproofing coating.The main method of preparing nano-aluminum hydroxide has: hydrothermal synthesis method, carbon method and sol-gel method etc.But method with practical value is also few.
The present invention finds that " aluminum ion-thiocyanate ion " system also has special character, can be used for preparing the aluminium hydroxide material of nanoscale, and with practical value.
Summary of the invention
The object of the invention is to propose take " aluminum ion-thiocyanate ion " system as presoma, synthesize aluminium hydrate nano particulate material.
The preparation method of the aluminium hydrate nano particulate material that the present invention proposes, is to prepare aluminum rhodanate with the mixed aqueous solution of trivalent aluminium salt and thiocyanate-, then reacts with alkaline solution, prepares aluminium hydrate nano particulate material.
In the present invention, described trivalent aluminium salt can adopt Tai-Ace S 150; Thiocyanate-can adopt Sodium Thiocyanate 99; Alkaline solution can adopt aqueous sodium hydroxide solution.
The concrete preparation process of the inventive method is as follows:
Aluminum sulfate aqueous solution and sodium thiocyanate water solution are mixed; Mix again reaction for some time with aqueous sodium hydroxide solution; Then suction filtration, washing, dry, obtain aluminium hydrate nano particulate material.
The concentration of described aluminum sulfate aqueous solution and sodium thiocyanate water solution is 0.3 ~ 1 mol/L; The concentration of described aqueous sodium hydroxide solution is 0.03 ~ 0.5 mol/L.
Reaction times is 1 ~ 24 hour.
In the present invention, in the process of described reaction, can adopt that ultrasonic wave is auxiliary synthetic, mechanical stirring, Stirring (containing stirrer) or mix after the reaction method such as standing again.Specifically can select according to actual needs one kind of.
Scanning electronic microscope (SEM) is observed and is shown that the aluminium hydroxide making is nano-particle material, and particle diameter is less than 100 nanometers.Under some synthesis condition, in product, may be mixed with alumina component.
The preparation method that the present invention proposes is very simple, easily produces.In actual production process, can amplify as the case may be industrial scale, comprise raising strength of solution.
The thiocyanate-using in the present invention can reclaim and recycle in actual production process, both cost-saving, also reduces quantity discharged.Compared with the method for other nano materials, the easier industrialization of the present invention.
This aluminium hydrate nano particulate material that the present invention makes has been widely used, such as: as precursor synthesis nano aluminium oxide; As flame retardant materials; As filler and additive application in all kinds of industrial and agricultural products; And be applied to aerospace and national defence field etc.
Accompanying drawing explanation
Fig. 1 is the SEM image of aluminium hydrate nano particulate material.
Fig. 2 is under high resolving power more, the SEM image of aluminium hydrate nano particulate material.
Fig. 3 is the SEM image of aluminium hydrate nano particulate material.
Embodiment
The preparation method of the aluminium hydrate nano particulate material that the invention is further illustrated by the following examples proposes.
embodiment 1
In reaction flask, add 15 milliliters of aluminum sulfate aqueous solutions (concentration: 0.5 mol/L), add again 90 milliliters of sodium thiocyanate water solutions (concentration: 0.5 mol/L), after stirring, again the aqueous sodium hydroxide solution of 450 milliliters (concentration: 0.05 mol/L) is joined in this mixing solutions, react 1 hour, standing, suction filtration, washing, dry, obtain aluminium hydrate nano particulate material.
Powder x-ray diffraction (XRD) analysis shows that this sample does not have peak crystallization, is non-crystalline material.
Fig. 1 shows that solid material is formed by nano particle accumulation.
The size of Fig. 2 signify hydrogen aluminum oxide nanoparticle is less than 70 nanometers.
In actual applications, can amplify production, comprise according to practical situation and improve strength of solution.
embodiment 2
In reaction flask, add 15 milliliters of zinc sulfate solutions (concentration: 0.5 mol/L), add again 90 milliliters of sodium thiocyanate water solutions (concentration: 0.5 mol/L), after mixing, again this mixing solutions is added in the aqueous sodium hydroxide solution (concentration: 0.05 mol/L) that fills 450 milliliters, mix rear reaction 1 hour, standing, suction filtration, washing, dry, obtain aluminium hydrate nano particulate material.
Powder x-ray diffraction (XRD) analysis shows that this sample does not have peak crystallization, is non-crystalline material.
Fig. 3 is the typical SEM image of this aluminium hydrate nano particulate material, and the size of signify hydrogen aluminum oxide nanoparticle is less than 100 nanometers.
In actual applications, can amplify production, comprise according to practical situation and improve strength of solution.

Claims (4)

1. a simple method for preparing for aluminium hydrate nano particulate material, is characterized in that, take " aluminum ion-thiocyanate ion " system as presoma, and synthetic aluminium hydrate nano particulate material; Specifically with the mixed aqueous solution of trivalent aluminium salt and thiocyanate-, prepare aluminum rhodanate, then react with alkaline solution, prepare aluminium hydrate nano particulate material.
2. the preparation method of aluminium hydrate nano particulate material according to claim 1, is characterized in that, described trivalent aluminium salt adopts Tai-Ace S 150; Described thiocyanate-adopts Sodium Thiocyanate 99; Described alkaline solution adopts aqueous sodium hydroxide solution.
3. according to the preparation method of the aluminium hydrate nano particulate material described in claim 2, it is characterized in that, concrete preparation process is as follows:
Aluminum sulfate aqueous solution and sodium thiocyanate water solution are mixed; Mix again reaction for some time with aqueous sodium hydroxide solution; Then suction filtration, washing, dry, obtain aluminium hydrate nano particulate material;
The concentration of described aluminum sulfate aqueous solution and sodium thiocyanate water solution is 0.3 ~ 1 mol/L; The concentration of described aqueous sodium hydroxide solution is 0.03 ~ 0.5 mol/L;
Reaction times is 1 ~ 24 hour.
4. the simple method for preparing of aluminium hydrate nano particulate material according to claim 3, is characterized in that in the process of described reaction, adopt that ultrasonic wave is auxiliary synthetic, mechanical stirring, Stirring or mix after standing reaction method again.
CN201410041307.6A 2014-01-28 2014-01-28 A kind of simple method for preparing of aluminum hydroxide nanoparticle material Active CN103754913B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108408694A (en) * 2018-03-01 2018-08-17 复旦大学 The environment-friendly preparation method thereof of metal oxide nano-material
CN108502910B (en) * 2018-03-01 2021-04-30 复旦大学 Insoluble inorganic salt micro-nano material and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001074713A1 (en) * 2000-04-03 2001-10-11 The University Of Queensland Improved mesoporous catalysts
CN1608997A (en) * 2004-10-27 2005-04-27 上海大学 Prepn process of nano aluminium hydroxide
CN1887715A (en) * 2006-08-14 2007-01-03 中国铝业股份有限公司 Prepn process of nanometer alumium hydroxide
CN101624216A (en) * 2008-07-10 2010-01-13 中国石油化工股份有限公司 Method for preparing nano nickel oxide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001074713A1 (en) * 2000-04-03 2001-10-11 The University Of Queensland Improved mesoporous catalysts
CN1608997A (en) * 2004-10-27 2005-04-27 上海大学 Prepn process of nano aluminium hydroxide
CN1887715A (en) * 2006-08-14 2007-01-03 中国铝业股份有限公司 Prepn process of nanometer alumium hydroxide
CN101624216A (en) * 2008-07-10 2010-01-13 中国石油化工股份有限公司 Method for preparing nano nickel oxide

Non-Patent Citations (2)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108408694A (en) * 2018-03-01 2018-08-17 复旦大学 The environment-friendly preparation method thereof of metal oxide nano-material
CN108502910B (en) * 2018-03-01 2021-04-30 复旦大学 Insoluble inorganic salt micro-nano material and preparation method and application thereof

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