CN100497169C - Artificial diamond purification technique - Google Patents
Artificial diamond purification technique Download PDFInfo
- Publication number
- CN100497169C CN100497169C CNB2007100544250A CN200710054425A CN100497169C CN 100497169 C CN100497169 C CN 100497169C CN B2007100544250 A CNB2007100544250 A CN B2007100544250A CN 200710054425 A CN200710054425 A CN 200710054425A CN 100497169 C CN100497169 C CN 100497169C
- Authority
- CN
- China
- Prior art keywords
- diamond
- acid
- ball milling
- graphite
- sulfuric acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 41
- 239000010432 diamond Substances 0.000 title claims abstract description 41
- 238000000746 purification Methods 0.000 title claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 32
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 23
- 230000015572 biosynthetic process Effects 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- 238000003786 synthesis reaction Methods 0.000 claims description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 15
- 239000010439 graphite Substances 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 6
- 238000013467 fragmentation Methods 0.000 claims description 2
- 238000006062 fragmentation reaction Methods 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 239000002253 acid Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000003595 mist Substances 0.000 abstract description 3
- FPVGTPBMTFTMRT-NSKUCRDLSA-L fast yellow Chemical compound [Na+].[Na+].C1=C(S([O-])(=O)=O)C(N)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 FPVGTPBMTFTMRT-NSKUCRDLSA-L 0.000 abstract description 2
- KCLANYCVBBTKTO-UHFFFAOYSA-N Proparacaine Chemical compound CCCOC1=CC=C(C(=O)OCCN(CC)CC)C=C1N KCLANYCVBBTKTO-UHFFFAOYSA-N 0.000 abstract 1
- 229940087458 alcaine Drugs 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000003672 processing method Methods 0.000 description 6
- 239000012535 impurity Substances 0.000 description 3
- 239000001117 sulphuric acid Substances 0.000 description 3
- 235000011149 sulphuric acid Nutrition 0.000 description 3
- 238000011109 contamination Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Abstract
The invention discloses a process to purify diamond, which comprises the following steps: grinding diamond synthesized block into particles; putting into autoclave; adding into the water solution of sulfuric acid or azotic acid or alcaine with density at 10-20%; reacting at normal temperature for 36-48 h; stripping metal; balling; sluicing; clearing black lead; drying; getting the purified diamond. This method does not use concentrated nitric sulfuric mixed acid and can eliminate a good deal of yellow acid mist, which can improve the safety in industrial process.
Description
Technical field
The invention belongs to the synthetic purification techniques field of superhard material, is a kind of artificial diamond purification technique.
Background technology
In technique known, purification for superhard materials such as powder method diamond synthesis piece or cubic boron nitrides, generally adopt the nitric-sulfuric acid reaction method of high density, utilize the strong oxidizing property and the impurity reactions such as metal in the superhard material and graphite of nitric-sulfuric acid, reach the purpose that removal of impurities is purified.There is the problem of following several respects in this processing method:
1, contained metal and strong acid form surface passivation easily in the diamond synthesis block in reaction process, need react → ball milling → elutriations → more than ten cyclical operation processes repeatedly such as reaction, take a lot of work, time-consuming, take and expect.
2, contained impurity such as graphite also are to remove by the oxidizing reaction of nitric-sulfuric acid in the diamond synthesis block, therefore, need to consume a large amount of concentrated nitric acid and the vitriol oil.
3, in whole synthetic purification process, because dense nitric-sulfuric acid participates in reaction, produce the yellow waste gas of a large amount of nitre sulfuric acid, production environment and atmospheric environment are caused severe contamination, poison HUMAN HEALTH, easily the operator is worked the mischief, even lead to the accident of burning.
4, discharge a large amount of spent acid solutions, severe contamination soil property, water quality, cost of sewage disposal height behind diamond synthesis block and the concentrated acid reaction.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can avoid environmental pollution, reduce the artificial diamond purification technique of raw materials consumption and cost of labor.
Realize that the technical scheme that purpose of the present invention is taked is: undertaken by following purifying technique step:
(1) fragmentation: it is the particle that is not more than 2mm that diamond synthesis block is broken into particle diameter;
(2) reaction removes metal: the ground grains material is put into reactor, add then in the sulfuric acid or nitric acid or aqueous hydrochloric acid of 10～20% concentration, the weight proportion of feed liquid is a material: sulfuric acid liquid or nitric acid liquid or hydrochloric acid solution=and 1: 5, reacted at normal temperatures 36～48 hours, waste reaction solution is emitted, take out reaction mass;
(3) ball milling: reaction mass was added in the ball mill ball milling 2～3 hours, and ball, material were by 2: 1 weight proportion;
(4) eluriate clear graphite: the material behind the ball milling is eluriated clean Ex-all graphite extremely fully with clear water, draw wet diamond;
(5) oven dry: will eluriate clean diamond and put into baking oven and dry, the taking-up sorting of sieving promptly gets high purity diamond finished product.
Because contained metal, graphite and diamond is equally distributed on substantially in the diamond synthesis block, by adopting the metal reaction in dilute sulphuric acid or rare nitric acid or dilute hydrochloric acid and the synthetic piece, remove the metal in the synthetic piece earlier, remaining diamond and graphite will be fluffy naturally, by ball milling, elutriation, remove graphite, the diamond after obtaining purifying.The chemical formula of reaction is: M+2H
+→ M
2++ H
2In the present invention, because to the diamond synthesis block employing is dilute sulphuric acid or rare nitric acid or dilute hydrochloric acid reaction, these diluted acids and graphite do not react substantially, can effectively reduce purification process Central Plains material usage thus, and dilute sulphuric acid or rare nitric acid or dilute hydrochloric acid do not have volatility basically, acid mist can be do not produced, pollution can be eliminated environment.
According to processing method of the present invention the synthetic piece of man-made diamond is purified, its beneficial effect is: can eliminate fully and adopt a large amount of yellow acid mist that produces in the dense nitric-sulfuric acid production process, eliminate the pollution of purification process to environment.And in the purification process, only need carry out ball milling, eluriate operation, circulating reaction, ball milling, elutriation repeatedly, compared with prior art, processing method of the present invention reduces with the acid amount more than 70% than original method, reduce artificial consumption more than 50%, and do not use the vitriol oil, concentrated nitric acid, can improve the security of production process greatly.
Embodiment
Man-made diamond method of purification of the present invention is: diamond synthesis block is broken for the particle that particle diameter is not more than 2mm, put into reactor, add then in the sulfuric acid or nitric acid or aqueous hydrochloric acid of 10～20% concentration, the feed liquid weight ratio is a material: sulfuric acid liquid or nitric acid liquid or hydrochloric acid solution=and 1: 5, reacted at normal temperatures 36～48 hours, the metal in the synthetic material is peeled off fully, enter in sulfuric acid liquid or nitric acid liquid or the hydrochloric acid solution, the venting spent acid solution takes out reaction mass then.Dispeling of graphite is in the diamond synthesis block: reaction mass was added in the ball mill ball milling 2～3 hours, and ball, material weight ratio are 2: 1; Material behind the taking-up ball milling is eluriated with clear water, and the graphite in the Ex-all material draws wet diamond; The diamond that will wet is at last put into baking oven dries, and the sorting of sieving promptly gets the high purity diamond.
Embodiment 1
Processing method according to above-mentioned diamond synthesis is purified is broken into small-particle with diamond synthesis block earlier, puts into reactor, adds sulfuric acid or the nitric acid or the aqueous hydrochloric acid of 10% concentration, reacts at normal temperatures 48 hours, removes metal.Take out reaction mass then, remove graphite through ball milling, elutriation, the sorting of sieving after the oven dry promptly gets the diamond finished product.
Embodiment 2
Processing method according to above-mentioned diamond synthesis is purified is broken into small-particle with diamond synthesis block earlier, puts into reactor, adds sulfuric acid or the nitric acid or the aqueous hydrochloric acid of 15% concentration, reacts at normal temperatures 42 hours, removes metal.Take out reaction mass then, remove graphite through ball milling, elutriation, the sorting of sieving after the oven dry promptly gets the diamond finished product.
Embodiment 3
Processing method according to above-mentioned diamond synthesis is purified is broken into small-particle with diamond synthesis block earlier, puts into reactor, adds sulfuric acid or the nitric acid or the aqueous hydrochloric acid of 20% concentration, reacts at normal temperatures 40 hours, removes metal.Take out reaction mass then, remove graphite through ball milling, elutriation, the sorting of sieving after the oven dry promptly gets the diamond finished product.
Claims (1)
1, a kind of artificial diamond purification technique, it is characterized in that: it comprises the following steps:
(1) fragmentation: it is the particle that is not more than 2mm that diamond synthesis block is broken into particle diameter;
(2) reaction removes metal: the ground grains material is put into reactor, add then in the sulfuric acid or nitric acid or aqueous hydrochloric acid of 10～20% concentration, the weight proportion of feed liquid is a material: sulfuric acid liquid or nitric acid liquid or hydrochloric acid solution=and 1: 5, reacted at normal temperatures 36～48 hours, waste reaction solution is emitted, take out reaction mass;
(3) ball milling: reaction mass was added in the ball mill ball milling 2～3 hours, and ball, material were by 2: 1 weight proportion;
(4) eluriate clear graphite: the material behind the ball milling is eluriated clean Ex-all graphite extremely fully with clear water, draw wet diamond;
(5) oven dry: will eluriate clean diamond and put into baking oven and dry, the taking-up sorting of sieving promptly gets high purity diamond finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100544250A CN100497169C (en) | 2007-05-18 | 2007-05-18 | Artificial diamond purification technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100544250A CN100497169C (en) | 2007-05-18 | 2007-05-18 | Artificial diamond purification technique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101062769A CN101062769A (en) | 2007-10-31 |
| CN100497169C true CN100497169C (en) | 2009-06-10 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100544250A Expired - Fee Related CN100497169C (en) | 2007-05-18 | 2007-05-18 | Artificial diamond purification technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100497169C (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757044B (en) * | 2012-07-23 | 2013-06-05 | 河南省联合磨料磨具有限公司 | High-cutting-force diamond micro powder and preparation method thereof |
| CN103043632B (en) * | 2012-12-14 | 2015-04-08 | 河南富耐克超硬材料股份有限公司 | Purification method for diamond and cubic boron nitride abrasive or micro-powder |
| 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 |
| CN105253883B (en) * | 2015-09-25 | 2017-09-15 | 郑州华晶金刚石股份有限公司 | A kind of nanometer diamond alkene of the layer structure of controllable type |
| CN105439138B (en) * | 2015-11-20 | 2017-06-27 | 西安文理学院 | A kind of Nano diamond and preparation method thereof |
| CN106927460A (en) * | 2015-12-30 | 2017-07-07 | 曾舟华 | Reaction accelerator and its application method that diamond is reclaimed |
| CN106365685B (en) * | 2016-08-29 | 2021-04-02 | 河南飞孟金刚石工业有限公司 | Purification process of white artificial diamond |
| CN106587046B (en) * | 2016-12-30 | 2018-10-23 | 郑州大学 | A kind of method of purification of diamond |
| CN107128909A (en) * | 2017-06-26 | 2017-09-05 | 湖北鄂信钻石科技股份有限公司 | A kind of method of purification of the diamond of Fe base catalyst |
| CN108793154A (en) * | 2018-07-20 | 2018-11-13 | 河南省亚龙超硬材料有限公司 | A kind of processing method of high-purity diadust impurity |
| CN109678148A (en) * | 2018-12-21 | 2019-04-26 | 河南烯碳合成材料有限公司 | The method of purification of graphite, lithium ion battery graphite cathode material and preparation method thereof in a kind of diamond production waste residue |
| 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 |
| CN115340089B (en) * | 2022-08-24 | 2024-02-06 | 内蒙古唐合科技有限公司 | Method for purifying artificial diamond |
-
2007
- 2007-05-18 CN CNB2007100544250A patent/CN100497169C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101062769A (en) | 2007-10-31 |
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| C06 | Publication | ||
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| ASS | Succession or assignment of patent right |
Owner name: NANYANG SINO-SOUTH AFRICAN DIAMOND COMPANY LIMITE Free format text: FORMER OWNER: HENAN ZHONGNAN INDUSTRIAL CO., LTD. Effective date: 20080111 |
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Effective date of registration: 20080111 Address after: Nanyang City, Henan Province Town South Gao Gou Cun in Fangcheng County Guangyang company hospital post encoding: 473200 Applicant after: Nanyang Zhongnan Diamond Co., Ltd. Address before: Fangcheng County of Nanyang City, Henan province box 101 Henan Zhongnan Industrial Co Ltd postal encoding: 473000 Applicant before: Nanyang Zhongnan Diamond Co., Ltd. |
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Owner name: ZHONGNAN DIAMOND CO., LTD. Free format text: FORMER OWNER: NANYANG SINO-SOUTH AFRICAN DIAMOND COMPANY LIMITED Effective date: 20091127 |
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Effective date of registration: 20091127 Address after: Fangcheng County of Nanyang City, Henan province 101. Patentee after: Zhongnan Diamond Co., Ltd. Address before: Nanyang City, Henan Province Town South Gao Gou Cun in Fangcheng County Guangyang company hospital Patentee before: Nanyang Zhongnan Diamond Co., Ltd. |
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Owner name: ZHONGNAN DIOMAND CO., LTD. Free format text: FORMER NAME: ZHONGNAN DIAMOND CO., LTD. |
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Address after: Fangcheng County of Nanyang City, Henan province 473264 box 101 Patentee after: ZHONGNAN DIAMOND CO., LTD. Address before: Fangcheng County of Nanyang City, Henan province 473200 box 101 Patentee before: Zhongnan Diamond Co., Ltd. |
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Granted publication date: 20090610 Termination date: 20160518 |