CN1186375C - Nano composite carbon/chromium trioxide powder and its prepn - Google Patents
Nano composite carbon/chromium trioxide powder and its prepn Download PDFInfo
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- CN1186375C CN1186375C CNB031160212A CN03116021A CN1186375C CN 1186375 C CN1186375 C CN 1186375C CN B031160212 A CNB031160212 A CN B031160212A CN 03116021 A CN03116021 A CN 03116021A CN 1186375 C CN1186375 C CN 1186375C
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Abstract
The present invention relates to nano composite carbon/ chromium oxide powder and a preparation method thereof. The nano composite carbon/ chromium oxide powder is prepared by the following steps: a hexavalent chrome compound and aniline are oxidized and polymerized to generate a sediment mixture of polyaniline and chromium hydroxide; nano composite polyaniline / chromium hydroxide powder is obtained after washing and drying; then the nano composite polyaniline / chromium hydroxide powder is heated to a high temperatureunder the condition that the air is isolated, and nano composite carbon/ chromium oxide powder in which carbon is wrapped on the surfaces of nano chromium oxide particles is obtained. The method of the present invention reduces the particle size of the powder and improves the use effect of the carbon/ chromium oxide powder as an antiwear additive, and the nano composite carbon/ chromium oxide powder is suitable for large-scale production.
Description
Technical field:
The present invention relates to a kind of carbon/chromium sesquioxide nano composite powder and preparation method thereof, belong to the inorganic composite materials technical field in the material type.
Background technology:
Chromium sesquioxide (claiming chromic oxide again) nanometer powder is a kind of anti-wear additive, is applied to improve the surface abrasion resistance of materials such as plastics, rubber.The method for preparing at present the chromium sesquioxide nanometer powder can be divided into two kinds, mechanical ball milling method and chemical precipitation method.The mechanical ball milling method is to have the chromium sesquioxide commodity mechanical disintegration of micron-scale to nano-scale.Because chromium sesquioxide has very high hardness and wear resisting property, so the application machine method is difficult to the particle size that reaches tiny, and power consumption is very high, the utensil wearing and tearing are big.Chemical precipitation method is under the protection of tensio-active agent and organic solvent, adds alkali in trivalent chromium solutions, obtains the chromium hydroxide nanoparticle precipitate, and high-temperature calcination obtains the chromium sesquioxide nanometer powder again.Be subjected to the restriction of tensio-active agent at the adsorption effect of chromium hydroxide particle surface, chemical precipitation method is difficult to the particle size that reaches tiny.There is agglomeration in the particle size of the chromium sesquioxide nanometer powder that these two kinds of methods obtain all greater than 100nm between the particle, be difficult to homodisperse in other body material.
Summary of the invention:
The objective of the invention is at the deficiencies in the prior art, a kind of method for preparing carbon/chromium sesquioxide nano composite powder is provided, reduce the particle size of gained composite powder, improve its result of use as anti-wear additive.
For realizing such purpose, technical scheme of the present invention is: use hexavalent chromium compound oxypolymerization aniline, form the throw out of polyaniline and chromium hydroxide blend, after washing and drying, obtain polyaniline/chromium hydroxide nano composite powder, again polyaniline/chromium hydroxide nano composite powder is heated to high temperature under the situation of secluding air, obtains carbon/chromium sesquioxide nano composite powder.
Polyaniline can be obtained by dichromate oxypolymerization aniline.It has been generally acknowledged that during dichromate oxypolymerization aniline, the reduzate of dichromate is water-soluble trivalent chromic ion.But find that in experiment the reduzate of dichromate also can be the chromium hydroxide that is insoluble in water in this process; Particularly under solutions of weak acidity, it is chromium hydroxide that 70% dichromate reduzate is arranged approximately; Chromium hydroxide is agglomerated into nano particle, and polyaniline is wrapped in around the chromium hydroxide nano particle; The final product of dichromate oxypolymerization aniline is actually polyaniline/chromium hydroxide nano-complex.Under the condition of high temperature secluding air, polyaniline is a carbon with pyrolysis, and chromium hydroxide is a chromium sesquioxide with pyrolysis, and polyaniline/chromium hydroxide nano-complex is converted into carbon/chromium sesquioxide nano-complex thereupon.
The concrete technology that the present invention prepares carbon/chromium sesquioxide nano composite powder is (the percentage number average of following all components refers to weight percentage): 1) contain 1%～20% aniline, pH value scope at 0～3 acidic solution with the hydrochloric acid preparation; 2) in aforementioned solution, add the polyoxyethylene glycol of 1～10ppm; 3) prepare the acidic solution that contains 1%～20% hexavalent chromium compound, contains 5%～18% hydrochloric acid; 4) the hexavalent chromium compound drips of solution is added in the aniline solution, and adds strong mixing, the mol ratio of hexavalent chromium compound and aniline is 0.5～2 here; 5) resulting throw out is filtered, washs; 6) throw out is soaked in 1%～10% the ammoniacal liquor, mixed solution was stirred 0.1～2 hour; 7) more resulting throw out is filtered, washs; 8) will obtain polyaniline/chromium hydroxide nano composite powder after the throw out oven dry; 9) polyaniline/chromium hydroxide nano composite powder is positioned in the nitrogen atmosphere, in 1000 ℃～1500 ℃ high temperature, heated 1～10 hour, obtain carbon/chromium sesquioxide nano composite powder.The particles of powder size is between 10nm～100nm, and the content of chromium sesquioxide is between 10%～70% (weight), and all the other are carbon.
Hexavalent chromium compound of the present invention is selected from a kind of in potassium bichromate, sodium dichromate 99, the chromium trioxide.
In the resulting carbon of the present invention/chromium sesquioxide nano composite powder, carbon is wrapped in the chromium sesquioxide nano grain surface, this can prevent the reunion between the chromium sesquioxide nano particle on the one hand, combine (being similar to the effect of carbon black Reinforced Rubber) that helps chromium sesquioxide nano particle and body materials such as rubber, plastics on the other hand, be the particle size that to control and to reduce the chromium sesquioxide nanometer powder on the one hand again, and then improve the result of use of chromium sesquioxide nanometer powder as anti-wear additive.The method of synthetic here carbon/chromium sesquioxide nano composite powder is suitable for scale operation.
Embodiment:
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1
1) to contain 1% aniline, pH value be 0 hydrochloric acid soln to preparation 200mL; 2) polyoxyethylene glycol of adding 1ppm in aforementioned solution; 3) preparation 5.2mL contains the solution of 20% chromium trioxide, 18% hydrochloric acid; 4) the chromium trioxide drips of solution is added in the aniline solution, and adds strong mixing, the mol ratio of chromium trioxide and aniline is 0.5 here; 5) resulting throw out is filtered, washes with water totally; 6) throw out is soaked in the ammoniacal liquor of 100mL1%, stirred 2 hours; 7) more resulting throw out is filtered, washs; 8) will obtain polyaniline/chromium hydroxide nano composite powder after the throw out oven dry; 9) polyaniline/chromium hydroxide nano composite powder is positioned in the nitrogen atmosphere, heating is 10 hours in 1000 ℃ high temperature, obtains carbon/chromium sesquioxide nano composite powder.
Embodiment 2
1) to contain 10% aniline, pH value be 3 hydrochloric acid soln to preparation 20mL; 2) polyoxyethylene glycol of adding 5ppm in aforementioned solution; 3) preparation 64mL contains the solution of 10% sodium dichromate 99,10% hydrochloric acid; 4) sodium dichromate solution is added drop-wise in the aniline solution, and adds strong mixing, the mol ratio of sodium dichromate 99 and aniline is 1 here; 5) resulting throw out is filtered, washes with water totally; 6) throw out is soaked in the ammoniacal liquor of 50mL5%, stirred 1 hour; 7) more resulting throw out is filtered, washs; 8) will obtain polyaniline/chromium hydroxide nano composite powder after the throw out oven dry; 9) polyaniline/chromium hydroxide nano composite powder is positioned in the nitrogen atmosphere, heating is 5 hours in 1200 ℃ high temperature, obtains carbon/chromium sesquioxide nano composite powder.
Embodiment 3
1) to contain 20% aniline, pH value be 1 hydrochloric acid soln to preparation 10mL; 2) polyoxyethylene glycol of adding 10ppm in aforementioned solution; 3) preparation 1265mL contains the solution of 1% potassium bichromate, 5% hydrochloric acid; 4) potassium bichromate solution is added drop-wise in the aniline solution, and adds strong mixing, the mol ratio of potassium bichromate and aniline is 2 here; 5) resulting throw out is filtered, washes with water totally; 6) throw out is soaked in the ammoniacal liquor of 20mL10%, stirred 0.1 hour; 7) more resulting throw out is filtered, washs; 8) will obtain polyaniline/chromium hydroxide nano composite powder after the throw out oven dry; 9) polyaniline/chromium hydroxide nano composite powder is positioned in the nitrogen atmosphere, heating is 1 hour in 1500 ℃ high temperature, obtains carbon/chromium sesquioxide nano composite powder.
Claims (3)
1, the preparation method of a kind of carbon/chromium sesquioxide nano composite powder is characterized in that comprising following concrete steps:
1) to contain weight percent be 1%～20% aniline, pH value scope at 0～3. acidic solution with hydrochloric acid preparation;
2) adding weight percent in aforementioned solution is the polyoxyethylene glycol of 1～10ppm;
3) to contain weight percent be 1%～20% hexavalent chromium compound, contain the acidic solution that weight percent is 5%～18% hydrochloric acid in preparation;
4) the hexavalent chromium compound drips of solution is added in the aniline solution, and adds strong mixing, the mol ratio of hexavalent chromium compound and aniline is 0.5～2;
5) resulting throw out is filtered, washs;
6) throw out being soaked in weight percent is in 1%～10% the ammoniacal liquor, and mixed solution was stirred 0.1～2 hour;
7) more resulting throw out is filtered, washs;
8) will obtain polyaniline/chromium hydroxide nano composite powder after the throw out oven dry;
9) polyaniline/chromium hydroxide nano composite powder is positioned in the nitrogen atmosphere, heated 1～10 hour in 1000 ℃～1500 ℃ high temperature, obtain carbon/chromium sesquioxide nano composite powder, particles of powder is of a size of 10nm～100nm.
2,, it is characterized in that described hexavalent chromium compound is selected from a kind of in potassium bichromate, sodium dichromate 99, the chromium trioxide as the preparation method of the said carbon of claim 1/chromium sesquioxide nano composite powder.
3, a kind of carbon/chromium sesquioxide nano composite powder by the said method preparation of claim 1, it is characterized in that in the composite powder, the weight percentage of chromium sesquioxide is 10%～70%, all the other are carbon, particles of powder is of a size of 10nm～100nm, and carbon is wrapped in around the chromium sesquioxide particle.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB031160212A CN1186375C (en) | 2003-03-27 | 2003-03-27 | Nano composite carbon/chromium trioxide powder and its prepn |
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| CNB031160212A CN1186375C (en) | 2003-03-27 | 2003-03-27 | Nano composite carbon/chromium trioxide powder and its prepn |
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| CN1440998A CN1440998A (en) | 2003-09-10 |
| CN1186375C true CN1186375C (en) | 2005-01-26 |
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| CN104037389B (en) * | 2014-06-19 | 2016-08-24 | 合肥国轩高科动力能源有限公司 | The preparation method of transition metal oxide lithium ion battery negative material |
| CN105609310B (en) * | 2016-01-21 | 2018-01-05 | 湘潭大学 | A kind of SnO2The surface modification method of base light anode |
| CN107240687B (en) * | 2017-06-12 | 2020-08-18 | 黎烈龙 | Energy storage material prepared from activated sludge and method and application thereof |
| CN108709020A (en) * | 2018-05-31 | 2018-10-26 | 安徽盛华管业有限公司 | A kind of preparation process of composite PVC pipe |
| CN112607739A (en) * | 2020-11-26 | 2021-04-06 | 安徽盈锐优材科技有限公司 | Preparation method of modified silicon carbide for thermal spraying |
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