CN101891164A - Method for purifying cubic boron nitride - Google Patents
Method for purifying cubic boron nitride Download PDFInfo
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- CN101891164A CN101891164A CN 201010223167 CN201010223167A CN101891164A CN 101891164 A CN101891164 A CN 101891164A CN 201010223167 CN201010223167 CN 201010223167 CN 201010223167 A CN201010223167 A CN 201010223167A CN 101891164 A CN101891164 A CN 101891164A
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Abstract
The invention discloses a method for purifying cubic boron nitride. The method is mainly characterized in that: sulphuric acid is mixed with sodium chlorate or sodium hypochlorite, the mixture is diluted with water, and concentrate which is processed with a shaking table undergoes reaction in the state of low-temperature heating. The method has the advantages of capability of removing graphite and metallic impurities mixed in the cubic boron nitride, no toxic and harmful gases, capability of effectively avoiding environmental pollution, short process flow because the graphite and metal can be removed by one process, high purification efficiency, recyclable reacted acid liquor, low consumption of acid and water resources, and capability of greatly reducing production cost due to low acid content of waste water and easy treatment of the waste water.
Description
Technical field
The invention belongs to the superhard material synthesis technical field, particularly a kind of method for purifying cubic boron nitride.
Background technology
In technique known, cubic boron nitride is selected the cubic boron nitride fine fodder with the synthetic rod immersion and with tabling after high temperature and high pressure method is synthetic, and then graphite and metal in the removal fine fodder of purifying, obtains purified cubic boron nitride crystal.The purifying technique of present cubic boron nitride branch two procedures usually carries out, promptly separate graphite with the vitriol oil with concentrated nitric acid or perchloric acid immersion earlier, the mixing acid of usefulness nitric acid and hydrochloric acid immersion separating metal, and water again carries out repeated multiple times to be eluriated, and obtains purified cubic boron nitride at last.The major defect of this method of purification is: 1) need to soak, eluriate with a large amount of concentrated acids and water, the resource consumption is big, the production cost height, and cause operator's health corrosion injury easily; Produce a large amount of toxic gases when 2) concentrated acid soaks reaction, the dense pale brown look smog of emerging, the severe contamination air, working conditions is abominable, is detrimental to health; 3) discharge a large amount of acid solutions, severe contamination water, native environment, sewage disposal expense height in the elutriation process; 4) purification process is longer, and is time-consuming, and purification production efficiency is low.
Summary of the invention
The purpose of this invention is to provide a kind of
Realize that the technical scheme that purpose of the present invention is taked is: this method is to carry out according to the following steps:
1) preparation acid solution: water intaking respectively, sulfuric acid and sodium chlorate or clorox, and it is even to inject container for stirring according to the weight part proportioning of 0.01～0.1 part of 1～1.5 part in water, 0.2～0.8 part in sulfuric acid, sodium chlorate or clorox, it is standby to make mixed solution;
2) Reaction Separation: the mixed solution of getting preparation injects in the reactor, by the cubic boron nitride fine fodder: the weight proportion of mixed solution=1: 1.0～1.2 adds the cubic boron nitride fine fodder after conventional tabling is handled, heating then, under 60～90 ℃ of temperature condition, react 30～90 minutes, and it is standby to be cooled to normal temperature;
3) filter to clean: the reacted feed liquid of step 3) is leached acid solution recycles, with filter cubic boron nitride clean with flushing with clean water, put into the drying baker oven dry and get final product.
Method for purifying cubic boron nitride of the present invention, the mixed solution that utilizes dilute sulphuric acid and sodium chlorate or clorox can be that carbon monoxide or carbonic acid gas are overflowed with the graphite oxidation in the shaking table preliminary election fine fodder in the redox reaction that is lower than under 60～90 ℃ the temperature with graphite and metal; Metal simple-substance is oxidized to metal ion enters solution.In the reactive separation process,, thereby avoided the topsoil in the purification production process because temperature of reaction is lower, thereby can not produce toxic gas.After reaction finished, the acid solution that press filtration is discharged still can be recycled, and reduces the consumption of sulfuric acid and sodium chlorate or clorox thus, in the finally discharged waste water acid content seldom, the corresponding intractability that reduced.
The method of purification of synthesizing cubic boron nitride of the present invention, adopt the reaction of diluted acid mixed solution low-temperature condition, not only can remove the graphite and the metallic impurity that are mingled in the cubic boron nitride neatly, and not have any toxic and harmful generation and discharging, avoid environmental pollution effectively.Simultaneously, this method is finished removing one procedure of graphite and metal, thereby process flow is short, the purification efficiency height.In addition, reacted acid solution recycles, and acid and water resources consumption amount are few, and acid content is seldom handled easily, thereby production cost is reduced greatly in the waste water in addition.
Embodiment
Method for purifying cubic boron nitride of the present invention be by the contriver on the basis that each component materials physico-chemical property of purification material is studied for a long period of time, through the repetition test gained.Test shows that after this method was handled, graphite and the metal full scale clearance that shaking table can be handled in the fine fodder were clean, and the cubic boron nitride that obtains can be seen surface clean with stereoscopic microscope, and color is bright.And no obnoxious flavour produces in treating processes, has eliminated environmental pollution.Below in conjunction with embodiment method of purification of the present invention is described further.
Embodiment 1
The purification of cubic boron nitride of the present invention is to carry out by the following method: water intaking at first respectively, sulfuric acid and sodium chlorate or clorox, and it is even to inject container for stirring according to the weight part proportioning of 0.1 part of 1 part in water, 0.8 part in sulfuric acid, sodium chlorate or clorox, makes mixed solution.Mixed solution with preparation injects in the reactor again, press the cubic boron nitride fine fodder: the weight proportion of mixed solution=1: 1.2 adds the cubic boron nitride fine fodder after shaking table is handled, be heated to 90 ℃ then, can observe the solution becomes muddiness, and a small amount of gas evolution arranged, afterreaction stopped in 30 minutes, and solution becomes is clear.Be cooled to normal temperature at reacted mixed solution, filter discharge acid solution and recycle, with filter cubic boron nitride clean with flushing with clean water, put into the drying baker oven dry and promptly obtain purified cubic boron nitride crystal grain.
Embodiment 2
The method of purification of present embodiment is substantially the same manner as Example 1, and difference is: preparation during mixed solution the weight part proportioning of each raw material be: 0.05 part of 1.3 parts in water, 0.5 part in sulfuric acid, sodium chlorate or clorox; The weight proportion of cubic boron nitride fine fodder and mixed solution is the cubic boron nitride fine fodder during reacting by heating: mixed solution=1: 1.1, Heating temperature are 80 ℃, and the reaction times is 60 minutes.
Embodiment 3
The method of purification of present embodiment is substantially the same manner as Example 1, and difference is: preparation during mixed solution the weight part proportioning of each raw material be: 0.01 part of 1.5 parts in water, 0.2 part in sulfuric acid, sodium chlorate or clorox; The weight proportion of cubic boron nitride fine fodder and mixed solution is the cubic boron nitride fine fodder during reacting by heating: mixed solution=1: 1.0, Heating temperature are 60, and the reaction times is 90 minutes.
Claims (1)
1. method for purifying cubic boron nitride, it is characterized in that: it is to carry out according to the following steps:
1) preparation acid solution: water intaking respectively, sulfuric acid and sodium chlorate or clorox, and it is even to inject container for stirring according to the weight part proportioning of 0.01～0.1 part of 1～1.5 part in water, 0.2～0.8 part in sulfuric acid, sodium chlorate or clorox, it is standby to make mixed solution;
2) Reaction Separation: the mixed solution of getting preparation injects in the reactor, by the cubic boron nitride fine fodder: the weight proportion of mixed solution=1: 1.0～1.2 adds the cubic boron nitride fine fodder after conventional tabling is handled, heating then, under 60～90 ℃ of temperature condition, react 30～90 minutes, and it is standby to be cooled to normal temperature;
3) filter to clean: the reacted feed liquid of step 3) is leached acid solution recycles, with filter cubic boron nitride clean with flushing with clean water, put into the drying baker oven dry and get final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102231676A CN101891164B (en) | 2010-07-12 | 2010-07-12 | Method for purifying cubic boron nitride |
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| CN2010102231676A CN101891164B (en) | 2010-07-12 | 2010-07-12 | Method for purifying cubic boron nitride |
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| CN101891164A true CN101891164A (en) | 2010-11-24 |
| CN101891164B CN101891164B (en) | 2011-12-07 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043658A (en) * | 2012-12-14 | 2013-04-17 | 河南富耐克超硬材料股份有限公司 | Method for purifying diamond or cubic boron nitride abrasive |
| CN105016317A (en) * | 2015-08-13 | 2015-11-04 | 郑州中南杰特超硬材料有限公司 | Cubic boron nitride monocrystal purification method |
| CN105110327A (en) * | 2015-07-01 | 2015-12-02 | 中南钻石有限公司 | Superhard abrasive material surface high-cleaning treatment method |
| CN110773109A (en) * | 2019-11-01 | 2020-02-11 | 成都理工大学 | Preparation method of boron nitride nanoflower |
| CN113772636A (en) * | 2021-09-27 | 2021-12-10 | 郑州中南杰特超硬材料有限公司 | Method for purifying cubic boron nitride single crystal |
-
2010
- 2010-07-12 CN CN2010102231676A patent/CN101891164B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 《金刚石与磨料磨具工程》 19801231 张为成 立方氮化硼的一种新提纯方法 第29-30页 1 , 第1期 2 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043658A (en) * | 2012-12-14 | 2013-04-17 | 河南富耐克超硬材料股份有限公司 | Method for purifying diamond or cubic boron nitride abrasive |
| CN103043658B (en) * | 2012-12-14 | 2014-09-17 | 河南富耐克超硬材料股份有限公司 | Method for purifying diamond or cubic boron nitride abrasive |
| CN105110327A (en) * | 2015-07-01 | 2015-12-02 | 中南钻石有限公司 | Superhard abrasive material surface high-cleaning treatment method |
| CN105016317A (en) * | 2015-08-13 | 2015-11-04 | 郑州中南杰特超硬材料有限公司 | Cubic boron nitride monocrystal purification method |
| CN105016317B (en) * | 2015-08-13 | 2017-02-01 | 郑州中南杰特超硬材料有限公司 | Cubic boron nitride monocrystal purification method |
| CN110773109A (en) * | 2019-11-01 | 2020-02-11 | 成都理工大学 | Preparation method of boron nitride nanoflower |
| CN113772636A (en) * | 2021-09-27 | 2021-12-10 | 郑州中南杰特超硬材料有限公司 | Method for purifying cubic boron nitride single crystal |
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| CN101891164B (en) | 2011-12-07 |
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Effective date of registration: 20170719 Address after: 450001, No. 08, building 12, building No. 228, West Fourth Ring Road, Zhengzhou hi tech Industrial Development Zone, Henan, 6 Patentee after: Zhengzhou Rui Li superhard material Co., Ltd Address before: 450001 Zhengzhou high tech Industrial Development Zone, Henan, Holly Street, No. 95 Patentee before: Zhengzhou Zhongnan Jete Superabrasives Co., Ltd. |
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