CN100591616C - Technical method for electrorefining diamond - Google Patents
Technical method for electrorefining diamond Download PDFInfo
- Publication number
- CN100591616C CN100591616C CN200710054424A CN200710054424A CN100591616C CN 100591616 C CN100591616 C CN 100591616C CN 200710054424 A CN200710054424 A CN 200710054424A CN 200710054424 A CN200710054424 A CN 200710054424A CN 100591616 C CN100591616 C CN 100591616C
- Authority
- CN
- China
- Prior art keywords
- diamond
- grams per
- per milliliters
- electrolysis
- electrolyzer
- 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 42
- 239000010432 diamond Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 9
- 239000010439 graphite Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000001376 precipitating effect Effects 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 20
- 230000015572 biosynthetic process Effects 0.000 claims description 18
- 238000003786 synthesis reaction Methods 0.000 claims description 18
- 239000000696 magnetic material Substances 0.000 claims description 13
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 241000080590 Niso Species 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 239000008151 electrolyte solution Substances 0.000 claims description 5
- 238000013467 fragmentation Methods 0.000 claims description 4
- 238000006062 fragmentation reaction Methods 0.000 claims description 4
- 239000011236 particulate material Substances 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 6
- 238000000746 purification Methods 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract 2
- 230000005611 electricity Effects 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 abstract 1
- 229910017604 nitric acid Inorganic materials 0.000 abstract 1
- 235000011149 sulphuric acid Nutrition 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000003672 processing method Methods 0.000 description 6
- 239000004575 stone Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000007670 refining Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 206010006895 Cachexia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 208000016318 wasting Diseases 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
This invention relates to a method for purifying diamond by electrolysis. The method comprises: immersing diamond synthesized by powder method into the electrolyte in an electrolytic tank as the anode, electrolyzing, precipitating metals in the synthetic diamond onto the cathode plate under current action, and removing graphite by washing with water to obtain high-purity diamond. The method utilizes electricity power as a substitute for H2SO4 and HNO3 thus can effectively eliminate environmental pollution during the purification process, and the operation is safe and reliable. Metals in the synthetic diamond can be recovered, and the recovery rate is 80-90%.
Description
Technical field
The invention belongs to the synthetic purification techniques field of man-made diamond, especially for a kind of technical method for electrorefining diamond of powder method diamond synthesis.
Background technology
In technique known, for the purification of powder method diamond synthesis piece, generally adopt the nitric-sulfuric acid reaction method of high density, utilize strong oxidizing property and the metal in the diamond synthesis block and the graphite reaction of nitric-sulfuric acid, reach the purpose that removal of impurities is purified.This processing method is on the one hand owing to form surface passivation easily in the reaction process of metal and strong acid, need react → the cyclical operation process repeatedly of ball milling → elutriations → ten multiple working procedures such as reaction, take a lot of work, time-consuming, take and expect.On the other hand, contained graphite also is to remove by the oxidizing reaction of nitric-sulfuric acid in the diamond synthesis block, thereby this method need consume a large amount of concentrated nitric acids and the vitriol oil.Simultaneously, this processing method produces the yellow waste gas of a large amount of nitre sulfuric acid because dense nitric-sulfuric acid participates in reaction, is difficult for absorbing and handles, and production environment and atmospheric environment are caused severe contamination, also easily the operator is worked the mischief, even leads to the accident of burning.In addition, the metal in the diamond synthesis block comprises contained 30%～50% precious metal, and enters reaction solution behind the acid-respons, discharge with spent acid solution, cause a large amount of wastings of resources thus, be unfavorable for resource recovery, simultaneously, also need spent acid solution is administered, control expense is high.
Summary of the invention
The purpose of this invention is to provide a kind of technical method for electrorefining diamond, realize cleaner production, eliminate environmental pollution, can reclaim the metal in the diamond synthesis piece simultaneously, be beneficial to resource recovery.
Realize that the technical scheme that purpose of the present invention is taked is: undertaken by following electrolytic purification technology step:
(1) fragmentation: diamond synthesis block is broken for the particle that particle diameter is less than or equal to 6mm;
(2) pack: the good particle of fragmentation is packed in the bag that silk or fibers material or other anticorrosive material make;
(3) insert in the particulate pocket of packing into by graphite or stainless steel or copper or platinum material and make positive plate, the big I of positive plate is decided according to the size of bag;
(4) pocket that will insert positive plate is hung in the electrolyzer;
(5) add electrolytic aqueous solution in electrolyzer, the dosage of electrolytic aqueous solution is:
NiSO
4Or NiCl
2100～200 (grams per milliliters)
FeSO
4Or FeCl
25～40 (grams per milliliters)
NaCl 5～10 (grams per milliliter)
H
2SO
45～10 (grams per milliliters)
(6) will hang in the electrolyzer by the negative plate that stainless steel or copper or platinum material are made;
(7) the energising electrolysis is 72～144 hours, and current density is 0.5～6A/dm
2
(8) metal in the diamond synthesis particulate material enters electrolytic solution by galvanic action, and after negative plate is separated out, and takes out the negative plate that has precipitating metal, and this plate can be used as that the regeneration back is nickeliferous sells with starting material;
(9) ball milling: the diamond synthesis particulate material after the electrolysis is taken out from bag, put into the ball mill ball milling 2～3 hours, ball, material weight ratio are 4: 1;
(10) eluriate: the material behind the ball milling is eluriated Ex-all graphite with clear water;
(11) material after will eluriating carries out screening and separating, is separated into high magnetic material and low magnetic material;
(12) with the electrolysis again of high magnetic material diamond (repeating 2～11 processing steps);
(13) will hang down the magnetic material and wash in a pan clean oven dry, the high grade diamond finished product.
According to above-mentioned processing method powder method diamond synthesis piece is purified, substitute the chemical method of concentrated acid reaction with electrolytic process, the high-grade diamond of not only can purifying, and can eliminate in the purification process pollution to environment, operational safety is reliable, can reclaim simultaneously the metal in the synthetic piece of powder method, metal recovery rate reaches 80～90%, realizes resource recovery.
Embodiment
Technical method for electrorefining diamond of the present invention be powder method synthetic Buddha's warrior attendant stone as anode, carry out electrolysis in the electrolytic solution in the electrolyzer of submerging, the metal in the diamond synthesis block enters electrolytic solution by galvanic action, and separates out on negative plate.Concrete grammar is as follows:
At first synthetic Buddha's warrior attendant stone is broken for the particle that particle diameter is less than or equal to 6mm, pack in the bag that silk or fibers material or other anticorrosive material make, and in bag, insert by graphite or stainless steel or copper or platinum material is made, with the positive plate of bag size coupling, hang together and insert in the electrolyzer; Add electrolytic aqueous solution then in electrolyzer, liquid level should exceed the diamond sack, and the dosage of electrolytic aqueous solution is: NiSO
4Or NiCl
2100～200 (grams per milliliters), FeSO
4Or Fe Cl
25～40 (grams per milliliters), NaCl 5～10 (grams per milliliter), H
2SO
45～10 (grams per milliliters) are hung in electrolyzer by stainless steel or copper or platinum material again and are made negative plate; The electrolysis 72～144 hours of can switching on, current density is 0.5～6A/dm
2Make the metal in the synthetic piece enter electrolytic solution by galvanic action, and separate out at negative plate, after treating that metal in the Buddha's warrior attendant stone is separated out fully, taking-up has the negative plate that metal is separated out, this plate with mainly containing precious metal such as nickel in the metal of separating out, thereby can be used as the high-grade starting material of regeneration and sell and utilize.Buddha's warrior attendant building stones after the electrolysis are taken out from bag, put into the ball mill ball milling 2～3 hours, the ball of packing in the ball mill, material weight ratio are 4: 1; Material behind the ball milling is eluriated totally with clear water, removed graphite, carry out screening and separating, be separated into high magnetic material and low magnetic material; To hang down the magnetic material; To hang down the magnetic diamond and eluriate the oven dry of clean back, finished product.The high magnetic material diamond of screening and separating can pack as stated above again and carry out electrolysis again, makes it all make low magnetic material diamond, also can mix pack during electrolysis with the Buddha's warrior attendant building stones piece through pulverizing and carry out electrolysis.
Embodiment 1
Carrying out according to above-mentioned processing method in the process of diamond synthesis refining, the dosage of used electrolytic aqueous solution can be: NiSO
4Or NiCl
2100 grams per milliliters, Fe SO
4Or Fe Cl
25 grams per milliliters, NaCl 5～10 grams per milliliters, H
2SO
45 grams per milliliters.
Embodiment 2
Carrying out according to above-mentioned processing method in the process of diamond synthesis refining, the dosage of used electrolytic aqueous solution also can be: NiSO
4Or NiCl
2150 grams per milliliters, Fe SO
4Or Fe Cl
220 grams per milliliters, NaCl 7 grams per milliliters, H
2SO
47 grams per milliliters.
Embodiment 3
Carrying out according to above-mentioned processing method in the process of diamond synthesis refining, the dosage of used electrolytic aqueous solution can also be: NiSO
4Or NiCl
2200 grams per milliliters, Fe SO
4Or Fe Cl
240 grams per milliliters, NaCl 10 grams per milliliters, H
2SO
410 grams per milliliters.
Claims (1)
1, a kind of technical method for electrorefining diamond, it is characterized in that: it may further comprise the steps:
(1) fragmentation: diamond synthesis block is broken for the particle that particle diameter is less than or equal to 6mm;
(2) pack: the good particle of fragmentation is packed in the bag that silk or fibers material or other anticorrosive material make;
(3) insert in the diamond synthesis block particulate pocket of packing into by graphite or stainless steel or copper or platinum material and make positive plate, the big I of positive plate is decided according to the size of bag;
(4) pocket that will insert positive plate is hung in the electrolyzer;
(5) add electrolytic aqueous solution in electrolyzer, the dosage of electrolytic aqueous solution is:
NiSO
4Or NiCl
2100～200 grams per milliliters
FeSO
4Or FeCl
25～40 grams per milliliters
NaCl 5～10 grams per milliliters
H
28O
45～10 grams per milliliters
(6) will hang in the electrolyzer by the negative plate that stainless steel or copper or platinum material are made;
(7) the energising electrolysis is 72～144 hours, and current density is 0.5～6A/dm
2
(8) metal in the diamond synthesis particulate material enters electrolytic solution by galvanic action, and after negative plate is separated out, takes out the negative plate that has precipitating metal;
(9) ball milling: the diamond synthesis particulate material after the electrolysis is taken out from bag, put into the ball mill ball milling 2～3 hours, ball, material weight ratio are 4: 1;
(10) eluriate: the material behind the ball milling is eluriated Ex-all graphite with clear water;
(11) material after will eluriating carries out screening and separating, is separated into high magnetic material diamond and low magnetic material diamond;
(12) with the electrolysis again of high magnetic material diamond, its method is undertaken by processing step 2～11;
(13) will hang down magnetic material diamond and wash in a pan clean oven dry, the high grade diamond finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710054424A CN100591616C (en) | 2007-05-18 | 2007-05-18 | Technical method for electrorefining diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710054424A CN100591616C (en) | 2007-05-18 | 2007-05-18 | Technical method for electrorefining diamond |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101049929A CN101049929A (en) | 2007-10-10 |
| CN100591616C true CN100591616C (en) | 2010-02-24 |
Family
ID=38781568
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200710054424A Expired - Fee Related CN100591616C (en) | 2007-05-18 | 2007-05-18 | Technical method for electrorefining diamond |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100591616C (en) |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101254917B (en) * | 2007-12-14 | 2010-06-09 | 武汉理工大学 | Laser machining method for improving quality of diamond micropowder |
| CN101307486B (en) * | 2008-01-25 | 2010-08-18 | 郭朝林 | Electric plating synthesis method for diamond under atmospheric pressure |
| CN101906632B (en) * | 2010-07-06 | 2011-12-07 | 中南钻石股份有限公司 | Method for washing anode bag for electrolyzing synthetic diamonds |
| CN103806018B (en) * | 2012-11-12 | 2016-03-02 | 浙江蓝龙科技有限公司 | A kind of man-made diamond synthesis post melting system |
| CN103361672A (en) * | 2013-07-04 | 2013-10-23 | 河南金六方超硬材料有限公司 | Recovery method for electrolytically extracting metal from catalyst after synthesizing diamonds from powder |
| CN103320845B (en) * | 2013-07-16 | 2016-03-16 | 安庆市凯立金刚石科技有限公司 | A kind of diamond production electrolysis electrolytic solution |
| CN104562080B (en) * | 2013-10-18 | 2017-02-15 | 浙江蓝龙科技有限公司 | Electrolyte solution for electrolyzing diamond synthesis column and using method of electrolyte solution |
| CN104716358B (en) * | 2013-12-13 | 2018-04-24 | 中国科学院大连化学物理研究所 | A kind of purification method of graphite material |
| CN103924286B (en) * | 2014-03-12 | 2017-01-11 | 张家港市港威超声电子有限公司 | High-efficiency extracting machine of artificial diamond |
| CN103922332B (en) * | 2014-04-01 | 2016-01-27 | 安庆市凯立金刚石科技有限公司 | A kind of artificial diamond purifying method |
| CN104046785B (en) * | 2014-04-09 | 2016-06-08 | 中南大学 | The treatment process of a kind of waste and old copper iron base diamond cutter head |
| GB201409895D0 (en) * | 2014-06-04 | 2014-07-16 | Cambridge Entpr Ltd | Method for producing synthetic diamonds |
| CN104195591B (en) * | 2014-09-17 | 2017-01-11 | 陈忠 | Comprehensive recovery method for waste iron-based diamond tool |
| CN106927460A (en) * | 2015-12-30 | 2017-07-07 | 曾舟华 | Reaction accelerator and its application method that diamond is reclaimed |
| CN106365161B (en) * | 2016-08-19 | 2018-06-26 | 富耐克超硬材料股份有限公司 | Purification of diamond method and its application |
| CN108048914B (en) * | 2017-12-08 | 2023-11-07 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Method for electrolytic purification of large diamond monocrystal synthetic block |
| CN108277500A (en) * | 2018-04-14 | 2018-07-13 | 新郑市新材料专业孵化器服务中心 | A kind of diamond electrorefining device |
| CN112239205A (en) * | 2019-07-17 | 2021-01-19 | 侯梦斌 | Graphite purification equipment and technology for intervening sodium chloride electrolysis |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1068153A (en) * | 1991-06-22 | 1993-01-20 | 中国有色金属工业总公司矿产地质研究院 | Artificial diamond purifying apparatus using electrical power to remove catalyst metal |
| CN1802458A (en) * | 2003-05-30 | 2006-07-12 | 约瑟夫·利奥波德·斯坦凯维奇 | A process for the recovery of synthetic diamonds |
-
2007
- 2007-05-18 CN CN200710054424A patent/CN100591616C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1068153A (en) * | 1991-06-22 | 1993-01-20 | 中国有色金属工业总公司矿产地质研究院 | Artificial diamond purifying apparatus using electrical power to remove catalyst metal |
| CN1802458A (en) * | 2003-05-30 | 2006-07-12 | 约瑟夫·利奥波德·斯坦凯维奇 | A process for the recovery of synthetic diamonds |
Non-Patent Citations (2)
| Title |
|---|
| 粉状触媒合成金刚石提纯新方法. 宋志昌.金刚石与磨料磨具工程，第3期. 2005 |
| 粉状触媒合成金刚石提纯新方法. 宋志昌.金刚石与磨料磨具工程，第3期. 2005 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101049929A (en) | 2007-10-10 |
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