CN106564896A - Method for extracting diamonds - Google Patents
Method for extracting diamonds Download PDFInfo
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- CN106564896A CN106564896A CN201510647767.8A CN201510647767A CN106564896A CN 106564896 A CN106564896 A CN 106564896A CN 201510647767 A CN201510647767 A CN 201510647767A CN 106564896 A CN106564896 A CN 106564896A
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Abstract
The invention discloses a method for extracting diamonds from diamond composite materials and waste diamond products. The method comprises the following steps of firstly, putting the crushed diamond composite materials into a reactor, and removing air in the reactor by vacuumizing or by a method of nitrogen and inert gas replacement; secondly, filling the reactor with carbon monoxide until certain pressure is formed, enabling the carbon monoxide to react with catalyst metal iron and nickel in the diamond composite materials to generate iron pentacarbonyl and nickel carbonyl, releasing and cooling iron pentacarbonyl and nickel carbonyl, and filling a sealed storage tank with the cooled iron pentacarbonyl and nickel carbonyl for standby; thirdly, after reaction ends, removing residual carbon monoxide in the reactor by vacuumizing or by the method of nitrogen and inert gas replacement; and fourthly, releasing diamonds and graphite which do not react in the reactor, and separating the diamonds from the graphite by physical methods including rinsing, screening and the like to obtain diamond and graphite pure substances. By use of the method, pollution brought to environment since aqua regia and the like are used for traditional diamond extraction is avoided, all resources can be efficiently utilized, ''three wastes'' discharge is eliminated, extraction efficiency is high, and economic benefit is good.
Description
Technical field
The invention belongs to superhard material field, is related to one kind from diamond synthesis block（Rod）And extract in waste and old diamond composition（It is pure）The method and apparatus of diamond.
Background technology
Diamond synthesis are by carbon（Graphite powder or carbon plate）With the metallic element as catalyst（The mainly transition metal such as ferrum, nickel and other microelement powders end or alloy sheet）, blended compacting（Lamination）Into pre-synthesis block（Rod）, thereafter under high-temperature and high-pressure conditions, graphite is changed to diamond.After end of synthesis, diamond particles are tightly wrapped up by the motlten metal as catalyst and unconverted graphite mixture so that diamond is extracted from Synthetic block becomes one necessary operation of diamond manufacturer.
Existing extracting method mainly has acid（Chloroazotic acid）Solution, electrolysis, reactor acid plumping method etc..
Acid hydrolyzation, is to use chloroazotic acid（The mixture of concentrated hydrochloric acid and concentrated nitric acid）, corrode the broken diamond synthesis blocks of Jing, make the metal in Synthetic block by aqua regia dissolution, by rinsing, separate, obtain diamond particles.
Electrolysis, it is that diamond synthesis block crushing is loaded anode cloth bag into after certain particle size to be electrolysed, after dissolving metal in Synthetic block is metal ion by electrolyte, the electric discharge on minus plate is reduced into metal, remaining graphite and diamond Jing ball millings, rinsing, sorting etc. again in cloth bag, obtains diamond particles.
Reactor acid plumping method, be by chloroazotic acid be put into reactor certain pressure, at a temperature of, accelerate graphite expansion and dissolving metal by stirring, through the method that rinsing sorting obtains diamond particles.
Above-mentioned three kinds of existing diamond extraction processes, either chloroazotic acid or electrolyte, all be unable to do without the strong acid such as hydrochloric acid, nitric acid, sulphuric acid, and environmental pollution is serious, and high cost, efficiency are low, become " fatal weakness " of diamond synthesizing industry.
The content of the invention
It is an object of the invention to provide a kind of completely new approach for extracting diamond, extracts diamond using oxo synthesis.I.e. at a temperature of certain pressure, with carbon monoxide and diamond synthesis block（Including waste and old diamond composition, similarly hereinafter）In ferrum, the reaction of the transition metal such as nickel, generate iron pentacarbonyl, nickel carbonyl, reach the ferrum nickel decomposed in diamond synthesis block, extract the purpose of diamond.The whole for the method achieving resource is recycled, three-waste free discharge, environmental friendliness, low cost, efficiency high.
The present invention is achieved by the following scheme：
By diamond synthesis block crushing into appropriately sized granule（It is advisable with not damaging diamond, little the carrying out for being conducive to reacting of granule）, load medium-pressure or high pressure reactor after the metering of diamond synthesis block crushing material, close all valves of reactor and feed inlet and outlet, using evacuation or nitrogen, the method for inert gas replacement, make no oxygen in reactor；
CO (carbon monoxide converter) gas are put into into reactor, after reaching certain pressure, the metal reaction such as ferrum, nickel in CO and diamond synthesis material generates iron pentacarbonyl, nickel carbonyl；In the relatively low environment of temperature, after to reactor supply carbon monoxide, it is necessary to the appropriate heating of reactor, to activate its reaction；
The raising of reaction pressure and combined coefficient positive correlation, generally, as long as an oxidation contact with ferrum, nickel, will slow reaction, press and above synthesis pressure in present invention selection, preferred high-pressure synthesis pressure（>10Mpa）, particularly preferred 12-30Mpa；
Reaction temperature is selected at 60 DEG C to 260 DEG C, preferably 130 DEG C to 200 DEG C；
To implementing stirring in reactor in building-up process, or reactor is carried out overturning, rolled, contribute to the raising of combined coefficient, but the manufacturing cost of reactor, the present invention preferably stirred reactor and standing and reacting device can be greatly improved.
Metal carbonyl synthetic reaction is exothermic reaction, after reaction starts, is the safety for ensureing reactor, it is necessary to which reactor is cooled down；
In time the iron pentacarbonyl generated in reactor, nickel carbonyl are released, and basin are put into through cooling standby；
According to contained ferrum in the filled diamond synthesis material of reactor, nickel, and iron pentacarbonyl, the nickel carbonyl of synthesis output, judge that synthesis carries out situation by calculating, after Theoretical Calculation ferrum, nickel reactant are finished, put back to the carbon monoxide for not having to consume in reactor, using evacuation or nitrogen, the method for inert gas replacement, no carbon monoxide in reactor is made；
Reactor drain hole is opened, the graphite and diamond of oxo process in releasing synthesis, is not involved in；Using physical method for separation graphite and diamond.
The present invention makes the melting catalyst metal reactions such as the ferrum in diamond synthesis material, nickel generate iron pentacarbonyl, nickel carbonyl by oxo synthesis；Iron pentacarbonyl and nickel carbonyl are to produce micron or nanometer carbonyl iron powder, the intermediate of nikel powder, and these products are different according to its particle diameter, commercially available price in ten thousand yuan/ton of 4-40, while and diamond synthesis catalyst material；The intermediate raw material of iron pentacarbonyl, nickel carbonyl or some high-technology fields；The carbon monoxide that iron pentacarbonyl, nickel carbonyl are decomposited is utilized for synthesis cycle.
The Objective extraction thing diamond of the present invention, after the catalyst metals such as the ferrum in diamond synthesis material, nickel are synthesized reaction, is only left clean graphite, diamond matrix, it is only necessary to which physical method for separation is obtained clean diamond and graphite.
The by-product graphite of the present invention, it is only necessary to by common process such as drying under grinding, anaerobic state, be exactly the good raw material of diamond synthesis.
Suitable for passing through oxo process with the waste and old diamond composition that ferrum, nickel are main carcass material, output iron pentacarbonyl, nickel carbonyl extract diamond to the present invention.
Claims (8)
1. a kind of method for extracting diamond, it is characterised in that with the catalyst metal ferrum in carbon monoxide and diamond synthesis material, nickel reactant, generate iron pentacarbonyl, nickel carbonyl, catalyst metal is separated from diamond synthesis material；After reaction, only it is left diamond and the graphite mixture for being not engaged in reacting in reactor, through isolated diamond and graphite powder.
2. the method comprises the following steps：
A. the diamond synthesis material for into reactor adding Jing broken（Including waste and old diamond composition, similarly hereinafter）, close charge door and each valve in addition to vacuum-pumping valve；
B. reactor evacuation, the air in purge reactor are given（Oxygen）, close and evacuate valve；
C. carbon monoxide is put into reactor, to required reaction pressure；
D. reaction temperature is reached to reactor heating, reaction opens cooling water after starting, give reaction cooling, ensure that reaction safety is carried out.
In 3.e. courses of reaction and after reaction terminates, reaction product iron pentacarbonyl, nickel carbonyl are released in time, Jing cooling storages are standby.
4.f. reactions to reactor evacuation or use nitrogen displacement after terminating, and remove carbon monoxide.
5.g. releases the diamond and graphite compound that reaction is had neither part nor lot in reactor, separated to wait post processing to obtain diamond and graphite.
6. reaction pressure according to claim 1 be 1Mpa and more than, preferred 12-30Mpa.
7. reaction temperature according to claim 1, selects at 60-260 DEG C, preferred 130-200 DEG C.
8. the reactor described in claim 1, can stand, may also be and stand with stirring, or upset or rolling, preferred to stand the reactor with stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510647767.8A CN106564896B (en) | 2015-10-09 | 2015-10-09 | A method of extraction diamond |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510647767.8A CN106564896B (en) | 2015-10-09 | 2015-10-09 | A method of extraction diamond |
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| CN106564896A true CN106564896A (en) | 2017-04-19 |
| CN106564896B CN106564896B (en) | 2018-08-31 |
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| CN201510647767.8A Active CN106564896B (en) | 2015-10-09 | 2015-10-09 | A method of extraction diamond |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479201A (en) * | 2020-11-30 | 2021-03-12 | 上海征世科技有限公司 | Artificial diamond purification method |
| CN114477251A (en) * | 2021-12-06 | 2022-05-13 | 金华博蓝特新材料有限公司 | Method for recycling aluminum oxide from sapphire cutting solid waste |
Citations (5)
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| CN201753267U (en) * | 2010-07-07 | 2011-03-02 | 中南钻石股份有限公司 | Artificial diamond purifying and decontaminating device |
| CN102616776A (en) * | 2012-04-09 | 2012-08-01 | 江苏金海丰硬质材料科技有限公司 | Purification method of nano diamond ash material |
| 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 |
| CN103303914A (en) * | 2013-07-01 | 2013-09-18 | 中南钻石股份有限公司 | Diamond purification technology |
| CN103482623A (en) * | 2013-09-05 | 2014-01-01 | 大连理工大学 | Method for preparing nano diamonds by using direct-current arc process |
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2015
- 2015-10-09 CN CN201510647767.8A patent/CN106564896B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201753267U (en) * | 2010-07-07 | 2011-03-02 | 中南钻石股份有限公司 | Artificial diamond purifying and decontaminating device |
| CN102616776A (en) * | 2012-04-09 | 2012-08-01 | 江苏金海丰硬质材料科技有限公司 | Purification method of nano diamond ash material |
| 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 |
| CN103303914A (en) * | 2013-07-01 | 2013-09-18 | 中南钻石股份有限公司 | Diamond purification technology |
| CN103482623A (en) * | 2013-09-05 | 2014-01-01 | 大连理工大学 | Method for preparing nano diamonds by using direct-current arc process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479201A (en) * | 2020-11-30 | 2021-03-12 | 上海征世科技有限公司 | Artificial diamond purification method |
| CN114477251A (en) * | 2021-12-06 | 2022-05-13 | 金华博蓝特新材料有限公司 | Method for recycling aluminum oxide from sapphire cutting solid waste |
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| CN106564896B (en) | 2018-08-31 |
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