CN101838850A - Method for preparing nano-tube aluminum borate whisker with sol precursor - Google Patents
Method for preparing nano-tube aluminum borate whisker with sol precursor Download PDFInfo
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- CN101838850A CN101838850A CN 201010184314 CN201010184314A CN101838850A CN 101838850 A CN101838850 A CN 101838850A CN 201010184314 CN201010184314 CN 201010184314 CN 201010184314 A CN201010184314 A CN 201010184314A CN 101838850 A CN101838850 A CN 101838850A
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- borate whisker
- aluminum borate
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Abstract
The invention relates to a method for preparing nano-tube aluminum borate whisker with a sol precursor, in particular to the method for preparing the nano-tube aluminum borate whisker. The method comprises the following steps: taking borax (containing ten crystal water) and aluminum nitrate (containing nine crystal water) as raw materials; dissolving the raw materials into a certain amount of deionized water according to a certain proportion; under the condition of continuously stirring, controlling reaction temperature, and dropwise adding aluminum nitrate solution to borax solution with a small amount of dispersing agent; adjusting pH value of the solution, and then filtering after reaction for a certain time; while filtering, washing for a plurality of times with hot distilled water and methanol respectively to obtain white sol; drying the white sol to obtain white xerogel, i.e. the precursor; grinding the precursor into powder, placing the powder into a porcelain crucible, calcining in a calcining furnace under the condition of controlling a certain temperature and time to obtain the nano-tube aluminum borate whisker. The invention provides the production method of the nano-tube aluminum borate whisker; and the method has high product quality and high added value, thus bringing economic benefits for enterprises.
Description
Technical field
The present invention relates to a kind of method of producing nano-tube aluminum borate whisker, particularly relate to a kind of have high Young's modulus, excellent mechanical intensity, thermotolerance, chemical proofing, acid resistance, electrical insulating property, neutron absorptive character, with the production technology of the nano-tube aluminum borate whisker of metal covalency.It not only is applied to thermal insulation, heat-resisting and anticorrosive material, also can be used for the strengthening agent of thermoplastic resin, thermosetting resin, cement, pottery and metal.Also can be used for strengthening aspects such as metal matrix (aluminium base, magnesium base), ceramic base, plastics, glass, fiber, coating.
Background technology
In recent years, China's boron industry has obtained certain development, but compares with developed country such as U.S., also is in the starting stage, also has some relatively distinct issues in the development and use of resource.The boron product processes falls behind, and comprehensive utilization of resources is poor.At present, geographic boron converted products such as Dandong also only limits to primary products such as " two boron ", and added value of product is low, deficiency in economic performance.The boron deep processed product of the U.S. has kind more than 300, and major part belongs to new high-tech product, and value-added content of product is very high.As being the derived product-boron nitride of raw material production with " two boron ", be the important source material of special cermacis, corrosion-and high-temp-resistant and superhard material, its product market price is about 500,000 yuan/ton.And the market value of its raw material borax is at present about 4000 yuan.
Boron should transfer resources advantage to industrial advantage and economic advantages as early as possible as a resources advantage, thereby promotes this area rapid economy development.Forming as early as possible based on " two boron " product, is the industrial system of pillar with boron essence, deep processed product.Developing the boron intensive processing product high in technological content, that added value of product is high, good in economic efficiency is the main direction of industry development from now on.
The employing borax is a raw material, add the paucidisperse agent, react with aluminum nitrate, control reaction temperature, reaction times, rate of addition, reactant ratio and solution pH value, after washing, heavyization, drying, obtain xerogel, as presoma, after the precursor grinding, under certain temperature and time conditions, calcining obtains nano-tube aluminum borate whisker.Technological element of a product height, added value height, quality height, business economic is profitable, and is significant to the development and the technical progress of boron industry.
Summary of the invention
The object of the present invention is to provide a kind of borax (containing ten crystal water) and aluminum nitrate (containing nine crystal water) of utilizing is raw material, add the paucidisperse agent, adopt sol-gel method to prepare presoma, after the precursor grinding, produce the method for nano-tube aluminum borate whisker by calcining, with the product that this method is produced, quality height, added value height, remarkable in economical benefits.
The objective of the invention is to be achieved through the following technical solutions:
The method of preparing nano-tube aluminum borate whisker with sol precursor, this method comprises the steps: at first aluminum nitrate solution dropwise to be added drop-wise in the borax soln that has added dispersion agent, then with the solution suction filtration, and with hot distilled water and methyl alcohol wash respectively the several, obtain leucosol, promptly obtaining white xerogel after the drying is presoma, then presoma is ground into powder, puts into calcining furnace and calcine, obtain the tubulose aluminium borate whisker.
The method of described preparing nano-tube aluminum borate whisker with sol precursor, its tubulose aluminium borate whisker diameter 0.5～1.0 μ m, length is 3.0～5.0 μ m.
The method of described preparing nano-tube aluminum borate whisker with sol precursor, its raw material is the aluminum nitrate that contains the borax of ten crystal water and contain nine crystal water, its raw material should satisfy following weight percent content: borax content 〉=95% that contains ten crystal water,, contain aluminum nitrate content 〉=99% of nine crystal water.
The method of described preparing nano-tube aluminum borate whisker with sol precursor, its this method has adopted sol-gel method to prepare presoma in technological process, and to grinding after the precursor drying, calcining at last obtains the tubulose aluminium borate whisker.
Advantage of the present invention and effect are:
1. present method has proposed a kind of both good in economic efficiency, easy and simple to handle nano-tube aluminum borate whisker production method, the quality product height, and the added value height can bring remarkable economic efficiency to enterprise.
2. with borax (containing ten crystal water), aluminum nitrate (containing nine crystal water) is a raw material, adopts.Adopt sol-gel method to prepare presoma, after precursor is ground, produce nano-tube aluminum borate whisker by calcining.
3. product tubulose aluminium borate whisker diameter 0.5～1.0 μ m, length is 3.0～5.0 μ m.
Description of drawings
Fig. 1 is a technological process block-diagram of the present invention.
Embodiment
The present invention is described in detail with reference to the accompanying drawings.
1. ultimate principle of the present invention
In conjunction with the sol-gel production technology characteristic, adopt the reaction of borax and aluminum nitrate to generate wet gel, obtain xerogel after the drying.After xerogel ground, under certain temperature and time conditions, the calcining xerogel obtained the tubular nanometer aluminium borate whisker, and production cost is low, technology is simple, not high to equipment requirements.
Adopt borax and aluminum nitrate in the aqueous solution, to prepare the aluminum borate gel.By the method for regulator solution pH value, avoid the generation of aluminum hydroxide precipitation, its reaction formula (1) is as follows:
nNa
2B
4O
7+2mAl(NO
3)
3→mAl
2O
3·nB
2O
3+2nNa
++6mNO
3 - (1)
After the wet gel process washing drying that obtains, obtain xerogel, calcining obtains the tubular nanometer aluminium borate whisker to xerogel, and its reaction formula (2) is as follows:
mAl
2O
3·nB
2O
3→2Al
2O
3·B
2O
3 (2)
After aluminium salt was water-soluble, because aluminum ions high electric charge and small ion radius, very easily hydrolysis generated multiple mononuclear coordination compound and polynuclear coordination compound.After increasing to a certain degree, the PH of the aqueous solution just generates Al (OH)
3Precipitation.In addition, the various distribution of aluminium salt hydrolysis polymerization is except outside the Pass the PH with solution has, and is also relevant with strength of solution, therefore, just can avoid Al (OH) by the PH of regulator solution and the concentration of control aluminum solutions
3Sedimentary generation.According to the synthetic thermomechanical analysis of aluminum borate as can be known:
2Al
2O
3+B
2O
3＝2Al
2O
3·B
2O
3 (3)
9Al
2O
3+2B
2O
3＝9Al
2O
3·2B
2O
3 (4)
2(2Al
2O
3·B
2O
3)+5Al
2O
3＝9Al
2O
3·2B
2O
3 (5)
2(9Al
2O
3·2B
2O
3)+5B
2O
3＝9(2Al
2O
3·B
2O
3) (6)
2. general planning of the present invention
With borax (containing ten crystal water) and aluminum nitrate (containing nine crystal water) is raw material, be dissolved in respectively in a certain amount of aqueous solution by certain solid-to-liquid ratio and proportioning, and adding paucidisperse agent in borax soln, under certain stirring velocity condition, control reaction temperature, after reaction for some time, stop to stir.With hot distilled water and methanol wash several, obtain leucosol, ageing for some time, being drying to obtain white xerogel then is presoma.
Performed polymer is put into calcining furnace calcine, promptly get the tubulose aluminium borate whisker.
3. technological method of the present invention
This project adopts sol-gel method to prepare aluminium borate whisker, adopts precursor-drying and grinding-calcination method to obtain the tubulose aluminium borate whisker.Sol-gel method becomes a kind of method relatively more commonly used of current preparation nano material because its production cost is low, technology is simple etc. characteristics.
4. specific embodiment of the present invention
Borax (containing ten crystal water) and aluminum nitrate (containing nine crystal water) reaction ratio (B/Al) get 3: 1～8: 1, the amount 450ml of distilled water, with Al (NO
3)
3The speed that solution drips with 3～5s/ adds in the borax water liquid, stir speed (S.S.) is 400rpm, 63 ℃ of temperature of reaction, control solution pH value be 7～8, reaction times 3～8h, with hot distilled water 1000ml and methyl alcohol 500ml washing for several times with the sol-gel that obtains, obtain leucosol, promptly obtaining white xerogel after dry 12～24 hours then is presoma.
Presoma is ground into powder, places porcelain crucible then, put into calcining furnace, calcine in the temperature ranges at 800～1200 degree, calcination time is under 2～6 hours the condition, to obtain nano-tube aluminum borate whisker, diameter 0.5～1.0 μ m, length is 3.0～5.0 μ m.
Claims (4)
1. the method for preparing nano-tube aluminum borate whisker with sol precursor, it is characterized in that this method comprises the steps: at first aluminum nitrate solution dropwise to be added drop-wise in the borax soln that has added dispersion agent, then with the solution suction filtration, and with hot distilled water and methyl alcohol wash respectively the several, obtain leucosol, promptly obtaining white xerogel after the drying is presoma, then presoma is ground into powder, puts into calcining furnace and calcine, obtain the tubulose aluminium borate whisker.
2. the method for preparing nano-tube aluminum borate whisker with sol precursor according to claim 1 is characterized in that tubulose aluminium borate whisker diameter 0.5～1.0 μ m, and length is 3.0～5.0 μ m.
3. the method for preparing nano-tube aluminum borate whisker with sol precursor according to claim 1, it is characterized in that raw material is the aluminum nitrate that contains the borax of ten crystal water and contain nine crystal water, its raw material should satisfy following weight percent content: borax content 〉=95% that contains ten crystal water,, contain aluminum nitrate content 〉=99% of nine crystal water.
4. the method for preparing nano-tube aluminum borate whisker with sol precursor according to claim 1, it is characterized in that this method has adopted sol-gel method to prepare presoma in technological process, to grinding after the precursor drying, calcining at last obtains the tubulose aluminium borate whisker.
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| CN 201010184314 CN101838850B (en) | 2010-05-27 | 2010-05-27 | Method for preparing nano-tube aluminum borate whisker with sol precursor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010184314 CN101838850B (en) | 2010-05-27 | 2010-05-27 | Method for preparing nano-tube aluminum borate whisker with sol precursor |
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| Publication Number | Publication Date |
|---|---|
| CN101838850A true CN101838850A (en) | 2010-09-22 |
| CN101838850B CN101838850B (en) | 2013-01-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109423692A (en) * | 2017-08-26 | 2019-03-05 | 慈溪市嘉和新材料科技有限公司 | A kind of synthesis technology of aluminium borate whisker |
| CN110577413A (en) * | 2019-08-27 | 2019-12-17 | 广东工业大学 | Aluminum borate whisker and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1936104A (en) * | 2006-09-08 | 2007-03-28 | 清华大学 | Magnesium borate whisker hydrothermal synthesis preparation method |
| CN101323979A (en) * | 2008-07-15 | 2008-12-17 | 沈阳化工学院 | Method for preparing nanometer plate-like aluminum borate crystal whisker |
-
2010
- 2010-05-27 CN CN 201010184314 patent/CN101838850B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1936104A (en) * | 2006-09-08 | 2007-03-28 | 清华大学 | Magnesium borate whisker hydrothermal synthesis preparation method |
| CN101323979A (en) * | 2008-07-15 | 2008-12-17 | 沈阳化工学院 | Method for preparing nanometer plate-like aluminum borate crystal whisker |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109423692A (en) * | 2017-08-26 | 2019-03-05 | 慈溪市嘉和新材料科技有限公司 | A kind of synthesis technology of aluminium borate whisker |
| CN110577413A (en) * | 2019-08-27 | 2019-12-17 | 广东工业大学 | Aluminum borate whisker and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN101838850B (en) | 2013-01-23 |
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