CN103910343A - Refining method for carbon-impurity-containing hexagonal boron nitride - Google Patents
Refining method for carbon-impurity-containing hexagonal boron nitride Download PDFInfo
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- CN103910343A CN103910343A CN201310023028.2A CN201310023028A CN103910343A CN 103910343 A CN103910343 A CN 103910343A CN 201310023028 A CN201310023028 A CN 201310023028A CN 103910343 A CN103910343 A CN 103910343A
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Abstract
A disclosed refining method for carbon-impurity-containing hexagonal boron nitride comprises the following process: firstly uniformly mixing a boron nitride crude product and a crystallization auxiliary agent, putting in a mullite-prepared ceramic container; sending into a continuous-type pusher kiln, introducing a mixed gas of oxygen and air, enabling the oxygen partial pressure to be 10-60%, preferably be 25-30%, controlling the kiln temperature at 450-900 DEG, preferably at 550-700 DEG C, keeping the material in the kiln for 2-7 h, and most preferably for 3-5 h; and enabling the material to pass a kiln cooling segment, discharging, washing with diluted hydrochloric acid and water, and drying to obtain the boron nitride refined product. The method breaks through conventional high-temperature refining (1800 DEG C or more) technology, the boron nitride crude product which is relatively low in boron carbon content and reacted in a low-temperature reaction is taken as a raw material, the high-purity hexagonal boron nitride powder is obtained in a temperature scope of 700-800 DEG C. The performances of the product are same to the performances of conventional high-temperature refined products, and the refining method has the advantages of low cost, high efficiency, less energy consumption and the like.
Description
Technical field
The present invention relates to a kind of process for purification of hexagonal boron nitride powder, especially the process for purification of carbon-containing impurities in hexagonal boron nitride.
Background technology
It is high that hexagonal boron nitride has fusing point, has fabulous lubricity, well heat conductivility, very high resist chemical.High dielectric breakdown strength, high volume resistivity, good unreactiveness.Boron nitride main application fields has boron nitride and composite ceramic articles thereof, coated coating industry, as thermal conductor, cosmetic industry and prepare cubic boron nitride etc.In these application, electrical insulation capability, lubricity and the purity of boron nitride powder is all to its application performance important.
In domestic normally used boron nitride preparation method, all adopted graphite as reaction vessel at present, in reaction and treating processes, the particulate of graphite is easy to enter into boron nitride.In addition, because some technique has been used the nitrogenous source (as urea, trimeric cyanamide etc.) of carbon containing, due to the existence of side reaction, also make residual carbon be dispersed in boron nitride, can in the synthetic various stages, introduce carbon-containing impurities, particularly powdered graphite in product.
If have simple substance carbon, free boron oxide etc. in hexagonal boron nitride powder, in ceramic sintering procedure, can destroy the structural performance of ceramic, make the machinery of ceramic and application performance deteriorated.
In order to obtain highly purified boron nitride, technique is in vacuum carbon tube furnace conventionally, rough boron nitride is heated to 1800 DEG C and refines above.This process for purification efficiency is low, and energy consumption is high.
Summary of the invention
Object of the present invention is exactly defect and the deficiency existing for overcoming above-mentioned prior art, and the process for purification of carbon-containing impurities in a kind of hexagonal boron nitride is provided.
The technical scheme adopting is:
The process for purification of carbon-containing impurities in hexagonal boron nitride of the present invention, is characterized in that comprising following technological process:
First boron nitride crude product and crystallization auxiliary are mixed, put into mullite earthenware porcelain receptacle processed.Send in continuous pushed bat kiln, then pass into the mixed gas of oxygen and air, making oxygen partial pressure is 10-60%, be preferably between 25-30%, furnace temperature is 450-900 DEG C, is preferably between 550-700 DEG C, material time in stove is 2-7 hour, and Best Times is 3-5 hour.Through the discharging of stove temperature descending section, after dilute hydrochloric acid washing and drying, obtain boron nitride purified product.
Above-mentioned crystallization auxiliary can be selected the carbonate of the vitriol of the halogenide of alkali-metal halogenide, alkaline-earth metal, alkali-metal fluoroborate, alkali-metal vitriol, alkaline-earth metal, alkali-metal carbonate or alkaline earth, as NaCl, NaCO3, KCl, K2CO3, CaCl2, CaCO3, NaSO4, CaSO4 or KBF4, preferably use NaCl or CaSO4.Crystallization auxiliary can make boron nitride in high-temperature reaction process, forms liquid phase, promotes the generation of boron nitride crystallization.By adjusting kind and the quantity of crystallization auxiliary, can obtain the hexagonal boron nitride of different crystal habits and granularity.
Method of the present invention has broken through refining (the more than 1800 DEG C) technique of traditional high temperature, the boron nitride of the lower aq generating taking low-temp reaction is as raw material, the temperature range of 700-800 DEG C, obtain highly purified hexagonal boron nitride powder, product performance have reached the performance of conventional high-temperature purified product, have that cost is low, efficiency is high, less cost of power
Embodiment
Embodiment 1:
By 10 kilograms of boron nitride crude products, purity is 94.5%, and carbon content is 0.6%, and 0.2 kilogram, crystallization auxiliary calcium carbonate mixes, and puts into mullite earthenware porcelain receptacle processed.Send in continuous pushed bat kiln, pass into the mixed gas of oxygen and air, making oxygen partial pressure is 25%, and furnace temperature is 600 DEG C, and material time in stove is 3 hours.Through the discharging of stove temperature descending section, after dilute hydrochloric acid washing and drying, obtain boron nitride purified product.
Boron nitride prod after refining, purity is 99.5%, carbon content is 0.02%.
Claims (3)
1. the process for purification of carbon-containing impurities in hexagonal boron nitride, is characterized in that comprising following technological process:
First boron nitride crude product and crystallization auxiliary are mixed, put into mullite earthenware porcelain receptacle processed, send in continuous pushed bat kiln, then pass into the mixed gas of oxygen and air, making oxygen partial pressure is 10-60%, is preferably between 25-30%, and furnace temperature is 450-900 DEG C, be preferably between 550-700 DEG C, material time in stove is 2-7 hour, and Best Times is 3-5 hour, through the discharging of stove temperature descending section, after dilute hydrochloric acid washing and drying, obtain boron nitride purified product.
2. the process for purification of carbon-containing impurities in above-mentioned hexagonal boron nitride according to claim 1, the crystallization auxiliary described in it is characterized in that is selected the carbonate of the vitriol of the halogenide of alkali-metal halogenide, alkaline-earth metal, alkali-metal fluoroborate, alkali-metal vitriol, alkaline-earth metal, alkali-metal carbonate or alkaline earth.
3. the process for purification of carbon-containing impurities in hexagonal boron nitride according to claim 2, is characterized in that described crystallization auxiliary is: NaCl, NaCO3, KCl, K2CO3, CaCl2, CaCO3, NaSO4, CaSO4 or KBF4.
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| CN201310023028.2A CN103910343A (en) | 2013-01-09 | 2013-01-09 | Refining method for carbon-impurity-containing hexagonal boron nitride |
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| CN201310023028.2A CN103910343A (en) | 2013-01-09 | 2013-01-09 | Refining method for carbon-impurity-containing hexagonal boron nitride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829889A (en) * | 2016-12-19 | 2017-06-13 | 郑州中南杰特超硬材料有限公司 | A kind of method for purifying hexagonal boron nitride in synthesizing cubic boron nitride tailing |
| WO2022071225A1 (en) * | 2020-09-30 | 2022-04-07 | デンカ株式会社 | Boron nitride powder and method for producing boron nitride powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891165A (en) * | 2010-07-15 | 2010-11-24 | 丹东市化工研究所有限责任公司 | Production method of macrocrystalline hexagonal boron nitride |
| CN102515120A (en) * | 2011-12-05 | 2012-06-27 | 沈阳大学 | Preparation method of hollow hexagonal boron nitride microsphere |
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2013
- 2013-01-09 CN CN201310023028.2A patent/CN103910343A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891165A (en) * | 2010-07-15 | 2010-11-24 | 丹东市化工研究所有限责任公司 | Production method of macrocrystalline hexagonal boron nitride |
| CN102515120A (en) * | 2011-12-05 | 2012-06-27 | 沈阳大学 | Preparation method of hollow hexagonal boron nitride microsphere |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829889A (en) * | 2016-12-19 | 2017-06-13 | 郑州中南杰特超硬材料有限公司 | A kind of method for purifying hexagonal boron nitride in synthesizing cubic boron nitride tailing |
| WO2022071225A1 (en) * | 2020-09-30 | 2022-04-07 | デンカ株式会社 | Boron nitride powder and method for producing boron nitride powder |
| JPWO2022071225A1 (en) * | 2020-09-30 | 2022-04-07 | ||
| JP7140939B2 (en) | 2020-09-30 | 2022-09-21 | デンカ株式会社 | Boron nitride powder and method for producing boron nitride powder |
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Application publication date: 20140709 |