CN101049929A - Technical method for electrorefining diamond - Google Patents

Technical method for electrorefining diamond Download PDF

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Publication number
CN101049929A
CN101049929A CNA2007100544246A CN200710054424A CN101049929A CN 101049929 A CN101049929 A CN 101049929A CN A2007100544246 A CNA2007100544246 A CN A2007100544246A CN 200710054424 A CN200710054424 A CN 200710054424A CN 101049929 A CN101049929 A CN 101049929A
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China
Prior art keywords
diamond
grams per
electrolysis
electrolyzer
magnetic material
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CNA2007100544246A
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CN100591616C (en
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刘善跃
刘杰
李璞
李玉健
沈远
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Zhongnan Diamond Co Ltd
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Nanyang Zhongnan Diamond Co Ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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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 method for electrorefining diamond
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 3
(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) high magnetic material diamond returned again separate (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 FeCL 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 3Make 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, FeSO 4Or FeCL 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, FeSO 4Or FeCL 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, FeSO 4Or FeCL 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 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 225~40 (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 3
(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 (repeating 2~11 processing steps);
(13) will hang down magnetic material diamond and wash in a pan clean oven dry, the high grade diamond finished product.
CN200710054424A 2007-05-18 2007-05-18 Technical method for electrorefining diamond Expired - Fee Related CN100591616C (en)

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Application Number Priority Date Filing Date Title
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CN100591616C CN100591616C (en) 2010-02-24

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Cited By (18)

* Cited by examiner, † Cited by third party
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
CN101906632A (en) * 2010-07-06 2010-12-08 中南钻石股份有限公司 Method for washing anode bag for electrolyzing synthetic diamonds
CN103320845A (en) * 2013-07-16 2013-09-25 安庆市凯立金刚石科技有限公司 Electrolyte formula
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
CN103806018A (en) * 2012-11-12 2014-05-21 浙江蓝龙科技有限公司 Melting system of artificial diamond composite column
CN103924286A (en) * 2014-03-12 2014-07-16 张家港市港威超声电子有限公司 High-efficiency extracting machine of artificial diamond
CN103922332A (en) * 2014-04-01 2014-07-16 安庆市凯立金刚石科技有限公司 Purification method of artificial diamond
CN104046785A (en) * 2014-04-09 2014-09-17 中南大学 Method for processing waste copper/iron-based diamond tool bit
CN104195591A (en) * 2014-09-17 2014-12-10 陈忠 Comprehensive recovery method for waste iron-based diamond tool
CN104562080A (en) * 2013-10-18 2015-04-29 浙江蓝龙科技有限公司 Electrolyte solution for electrolyzing diamond synthesis column and using method of electrolyte solution
CN104716358A (en) * 2013-12-13 2015-06-17 中国科学院大连化学物理研究所 Purification method of graphite material
WO2015185898A1 (en) * 2014-06-04 2015-12-10 Cambridge Enterprise Ltd Method for producing synthetic diamonds
CN106365161A (en) * 2016-08-19 2017-02-01 富耐克超硬材料股份有限公司 Diamond purification method and use thereof
CN106927460A (en) * 2015-12-30 2017-07-07 曾舟华 Reaction accelerator and its application method that diamond is reclaimed
CN108048914A (en) * 2017-12-08 2018-05-18 郑州人造金刚石及制品工程技术研究中心有限公司 A kind of method of electrorefining diamond large single crystal 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

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1029487C (en) * 1991-06-22 1995-08-09 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

Cited By (28)

* Cited by examiner, † Cited by third party
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
CN101906632A (en) * 2010-07-06 2010-12-08 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
CN103806018A (en) * 2012-11-12 2014-05-21 浙江蓝龙科技有限公司 Melting system of artificial diamond composite column
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
CN103320845A (en) * 2013-07-16 2013-09-25 安庆市凯立金刚石科技有限公司 Electrolyte formula
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
CN104562080A (en) * 2013-10-18 2015-04-29 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
CN104716358A (en) * 2013-12-13 2015-06-17 中国科学院大连化学物理研究所 Purification method of graphite material
CN103924286A (en) * 2014-03-12 2014-07-16 张家港市港威超声电子有限公司 High-efficiency extracting machine of artificial diamond
CN103922332A (en) * 2014-04-01 2014-07-16 安庆市凯立金刚石科技有限公司 Purification method 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
CN104046785A (en) * 2014-04-09 2014-09-17 中南大学 Method for processing waste copper/iron-based diamond tool bit
WO2015185898A1 (en) * 2014-06-04 2015-12-10 Cambridge Enterprise Ltd Method for producing synthetic diamonds
US10556211B2 (en) 2014-06-04 2020-02-11 Northeastern University Method for producing synthetic diamonds
CN106660808A (en) * 2014-06-04 2017-05-10 剑桥企业有限公司 Method for producing synthetic diamonds
CN106660808B (en) * 2014-06-04 2019-04-26 东北大学 The method for preparing rhinestone
CN104195591A (en) * 2014-09-17 2014-12-10 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
CN106365161A (en) * 2016-08-19 2017-02-01 富耐克超硬材料股份有限公司 Diamond purification method and use thereof
CN108048914A (en) * 2017-12-08 2018-05-18 郑州人造金刚石及制品工程技术研究中心有限公司 A kind of method of electrorefining diamond large single crystal Synthetic block
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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