CN112479201B - Artificial diamond purification method - Google Patents
Artificial diamond purification method Download PDFInfo
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- CN112479201B CN112479201B CN202011371313.XA CN202011371313A CN112479201B CN 112479201 B CN112479201 B CN 112479201B CN 202011371313 A CN202011371313 A CN 202011371313A CN 112479201 B CN112479201 B CN 112479201B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
Abstract
The invention discloses a method for purifying artificial diamond. Introducing nitrogen into a rough artificial diamond in an atmosphere furnace, introducing carbon dioxide gas, reacting for 30-60min under the atmosphere, cooling, taking out the material to obtain a reaction material, placing the reaction material into a high-pressure reaction kettle, heating to 50-120 ℃, introducing carbon monoxide to make the pressure be 1-10MPa, reacting for 30-60min, then decompressing, introducing the generated gas into ethanol, cooling to a temperature less than 25 ℃, adding absolute ethanol into the material in the high-pressure reaction kettle, mixing and stirring for 10-20min to obtain a solid-liquid mixture; and (3) carrying out solid-liquid separation on the solid-liquid mixture, washing with absolute ethyl alcohol, and drying in vacuum to obtain the composite material. The invention can effectively purify the metal, unconverted carbon and the like in the diamond, has high efficiency and finally has high purity of the diamond.
Description
Technical Field
The invention relates to a method for purifying artificial diamond, and belongs to the technical field of new energy lithium battery materials.
Background
Diamond is commonly called "diamond," which is a mineral composed of pure carbon and is the hardest substance in nature. Since the 18 th century confirmed that diamond is composed of pure carbon, research on artificial diamond was started, and the research and rapid development of artificial diamond was achieved only in the 50 th century by the development of high-voltage research and high-voltage experimental techniques.
By utilizing static ultrahigh pressure (50-100 kb, namely 5-10 GPa) and high temperature (1100-3000 ℃), the carbon raw materials such as graphite and the like react with certain metals (alloys) to generate diamond, and the typical crystalline state of the diamond is cubic (hexahedron), octahedron, hexaoctahedron and transition forms of the cubic (hexahedron), octahedron and hexaoctahedron. With the development of high temperature and high pressure technology, the maximum size of the artificial single crystal diamond can be made to 8 mm. By the 20 th century, 70 s, developing metal sintered polycrystalline diamond (PCD), synthetic diamond material has become the only alternative to natural single crystal diamond.
The polycrystalline diamond is formed by sintering diamond micropowder and a small amount of binding agent at high temperature and high pressure, has the characteristics of high wear resistance, strong impact toughness, good thermal stability, compact and uniform structure and the like, and is widely applied to the manufacture of petroleum, geological drill bits, machining tools, gem processing and the like.
Generally, synthetic diamond contains metal such as nickel and impurities such as carbon, and purification is required.
Disclosure of Invention
In view of the above, the invention provides a method for purifying artificial diamond, which can effectively purify metals, unconverted carbon and the like in the artificial diamond, and has high efficiency and high purity of the final diamond.
The invention solves the technical problems through the following technical means:
the invention relates to a method for purifying artificial diamond, which comprises the following steps:
(1) introducing nitrogen into the rough artificial diamond in an atmosphere furnace to ensure that the volume concentration of oxygen in the atmosphere furnace is lower than 5ppm, then heating to the temperature of 700-800 ℃, then introducing carbon dioxide gas to ensure that the volume concentration of oxygen in the atmosphere furnace is lower than 2ppm and the volume concentration of carbon dioxide is higher than 99%, reacting for 30-60min in the atmosphere, then cooling to the temperature of less than 100 ℃, and taking out the material to obtain a reaction material;
(2) putting the reaction materials into a high-pressure reaction kettle, heating to 50-120 ℃, introducing carbon monoxide to make the pressure 1-10MPa, then reacting for 30-60min, then decompressing, introducing the generated gas into ethanol, then cooling to a temperature less than 25 ℃, adding the materials in the high-pressure reaction kettle into absolute ethanol, mixing and stirring for 10-20min to obtain a solid-liquid mixture;
(3) and (3) carrying out solid-liquid separation on the solid-liquid mixture, then washing with absolute ethyl alcohol, and drying in vacuum to obtain the finished product.
The volume concentration of oxygen in the nitrogen in the step (1) is lower than 1ppm, and the preparation method of the nitrogen is cryogenic air separation nitrogen preparation, pressure swing adsorption nitrogen preparation or membrane separation nitrogen preparation.
The mass ratio of the materials in the high-pressure reaction kettle in the step (2) to the absolute ethyl alcohol is 1: 3-5.
And (4) the solid-liquid separation equipment in the step (3) is a centrifugal machine.
In the step (3), the drying temperature is 40-60 ℃, and the vacuum degree is-0.08 to-0.05 MPa in the drying process in the vacuum drying oven.
And (3) absorbing the ethanol of the gas in the step (2), and separating the gas from the ethanol through reduced pressure distillation.
According to the invention, carbon dioxide is introduced at high temperature, so that incandescent carbon can be effectively oxidized into carbon monoxide gas to volatilize out, carbon is removed, carbon monoxide is introduced at low temperature and high pressure, so that a metal carbonyl compound is formed, a part of the metal carbonyl compound is changed into gas, the gas is volatilized during pressure relief and is absorbed by ethanol, a small amount of liquid carbonyl compound is added with ethanol, the ethanol can be dissolved and filtered out, and then the ethanol is adopted for washing, so that metal is removed, and the artificial diamond with higher purity is obtained.
The invention has the beneficial effects that: can effectively purify the metal, unconverted carbon and the like, has high efficiency and finally has high purity of the diamond.
Detailed Description
The present invention will be described in detail below with reference to specific examples: the method for purifying the artificial diamond comprises the following steps:
(1) introducing nitrogen into the rough artificial diamond in an atmosphere furnace to ensure that the volume concentration of oxygen in the atmosphere furnace is lower than 5ppm, then heating to the temperature of 700-800 ℃, then introducing carbon dioxide gas to ensure that the volume concentration of oxygen in the atmosphere furnace is lower than 2ppm and the volume concentration of carbon dioxide is higher than 99%, reacting for 30-60min in the atmosphere, then cooling to the temperature of less than 100 ℃, and taking out the material to obtain a reaction material;
(2) putting the reaction materials into a high-pressure reaction kettle, heating to 50-120 ℃, introducing carbon monoxide to ensure that the pressure is 1-10MPa, then reacting for 30-60min, then decompressing, introducing the generated gas into ethanol, then cooling to a temperature of less than 25 ℃, adding the materials in the high-pressure reaction kettle into absolute ethanol, mixing and stirring for 10-20min to obtain a solid-liquid mixture;
(3) and (3) carrying out solid-liquid separation on the solid-liquid mixture, washing with absolute ethyl alcohol, and drying in vacuum to obtain the composite material.
The volume concentration of oxygen in the nitrogen in the step (1) is lower than 1ppm, and the nitrogen preparation method is cryogenic air separation nitrogen preparation, pressure swing adsorption nitrogen preparation or membrane separation nitrogen preparation.
The mass ratio of the materials in the high-pressure reaction kettle in the step (2) to the absolute ethyl alcohol is 1: 3-5.
And (4) the solid-liquid separation in the step (3) adopts a centrifugal machine.
In the drying process in the vacuum drying oven in the step (3), the drying temperature is 40-60 ℃, and the vacuum degree is-0.08 to-0.05 MPa.
And (3) absorbing the ethanol of the gas in the step (2), and separating the gas from the ethanol through reduced pressure distillation.
Example 1
A method for purifying artificial diamond comprises the following steps:
(1) introducing nitrogen into the rough artificial diamond in an atmosphere furnace to ensure that the volume concentration of oxygen in the atmosphere furnace is 2.7ppm, then heating to 700 ℃, introducing carbon dioxide gas to ensure that the volume concentration of oxygen in the atmosphere furnace is 1.5ppm and the volume concentration of carbon dioxide is 99.2%, reacting for 60min in the atmosphere, then cooling to 95 ℃, and taking out the material to obtain a reaction material;
(2) putting the reaction materials into a high-pressure reaction kettle, heating to 90 ℃, introducing carbon monoxide to ensure that the pressure is 1.5MPa, then reacting for 60min, then decompressing, introducing generated gas into ethanol, then cooling to 24 ℃, adding the materials in the high-pressure reaction kettle into absolute ethanol, mixing and stirring for 10min to obtain a solid-liquid mixture;
(3) and (3) carrying out solid-liquid separation on the solid-liquid mixture, then washing with absolute ethyl alcohol, and drying in vacuum to obtain the finished product.
The volume concentration of oxygen in the nitrogen in the step (1) is lower than 1ppm, and the nitrogen preparation method is pressure swing adsorption nitrogen preparation or membrane separation nitrogen preparation.
The mass ratio of the materials in the high-pressure reaction kettle in the step (2) to the absolute ethyl alcohol is 1: 3.
And (4) the solid-liquid separation equipment in the step (3) is a centrifugal machine.
And (4) in the step (3), in the drying process in the vacuum drying oven, the drying temperature is 40 ℃, and the vacuum degree is-0.08 MPa.
And (3) absorbing the ethanol of the gas in the step (2), and separating the gas from the ethanol through reduced pressure distillation.
Example 2
A method for purifying artificial diamond comprises the following steps:
(1) introducing nitrogen into the rough artificial diamond in an atmosphere furnace to ensure that the volume concentration of oxygen in the atmosphere furnace is 4.6ppm, then heating to 800 ℃, introducing carbon dioxide gas to ensure that the volume concentration of oxygen in the atmosphere furnace is 1.9ppm and the volume concentration of carbon dioxide is 99.7%, reacting for 30min in the atmosphere, then cooling to 85 ℃, and taking out the material to obtain a reaction material;
(2) putting the reaction materials into a high-pressure reaction kettle, heating to 120 ℃, introducing carbon monoxide to ensure that the pressure is 2MPa, then reacting for 30min, then decompressing, introducing the generated gas into ethanol, then cooling to 23 ℃, adding the materials in the high-pressure reaction kettle into absolute ethanol, mixing and stirring for 10min to obtain a solid-liquid mixture;
(3) and (3) carrying out solid-liquid separation on the solid-liquid mixture, then washing with absolute ethyl alcohol, and drying in vacuum to obtain the finished product.
The volume concentration of oxygen in the nitrogen in the step (1) is lower than 1ppm, and the nitrogen preparation method is a cryogenic air separation nitrogen preparation method.
The mass ratio of the materials in the high-pressure reaction kettle in the step (2) to the absolute ethyl alcohol is 1: 5.
And (4) the solid-liquid separation in the step (3) adopts a centrifugal machine.
And (3) in the vacuum drying oven, drying at 60 ℃ and under a vacuum degree of-0.065 MPa.
And (3) absorbing the ethanol of the gas in the step (2), and separating the gas from the ethanol through reduced pressure distillation.
Example 3
A method for purifying artificial diamond comprises the following steps:
(1) introducing nitrogen into the rough artificial diamond in an atmosphere furnace to ensure that the volume concentration of oxygen in the atmosphere furnace is 1.5ppm, then heating to the temperature of 750 ℃, introducing carbon dioxide gas to ensure that the volume concentration of oxygen in the atmosphere furnace is 1.1ppm and the volume concentration of carbon dioxide is 99.5%, reacting for 45min in the atmosphere, then cooling to the temperature of 99 ℃, and taking out the material to obtain a reaction material;
(2) putting the reaction materials into a high-pressure reaction kettle, heating to 50 ℃, introducing carbon monoxide to make the pressure 10MPa, then reacting for 30min, then decompressing, introducing the generated gas into ethanol, then cooling to 20 ℃, adding the materials in the high-pressure reaction kettle into absolute ethanol, mixing and stirring for 10min to obtain a solid-liquid mixture;
(3) and (3) carrying out solid-liquid separation on the solid-liquid mixture, then washing with absolute ethyl alcohol, and drying in vacuum to obtain the finished product.
The volume concentration of oxygen in the nitrogen in the step (1) is lower than 1ppm, and the nitrogen preparation method is membrane separation nitrogen preparation.
The mass ratio of the materials in the high-pressure reaction kettle in the step (2) to the absolute ethyl alcohol is 1: 5.
And (4) the solid-liquid separation equipment in the step (3) is a centrifugal machine.
And (4) in the step (3), drying in a vacuum drying oven at the drying temperature of 60 ℃ and the vacuum degree of-0.05 MPa.
And (3) absorbing the ethanol of the gas in the step (2), and separating the gas from the ethanol through reduced pressure distillation.
Finally, the results of the tests of the products obtained in examples 1, 2 and 3 of the present invention are as follows:
finally, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A method for purifying artificial diamond is characterized by comprising the following steps:
(1) introducing nitrogen into the rough-made artificial diamond in an atmosphere furnace to ensure that the volume concentration of oxygen in the atmosphere furnace is lower than 5ppm, then heating to the temperature of 700-800 ℃, then introducing carbon dioxide gas to ensure that the volume concentration of oxygen in the atmosphere furnace is lower than 2ppm and the volume concentration of carbon dioxide is higher than 99%, reacting for 30-60min in the atmosphere, then cooling to the temperature of less than 100 ℃, and taking out the material to obtain a reaction material;
(2) putting the reaction materials into a high-pressure reaction kettle, heating to 50-120 ℃, introducing carbon monoxide to make the pressure 1-10MPa, then reacting for 30-60min, then decompressing, introducing the generated gas into ethanol, then cooling to a temperature less than 25 ℃, adding the materials in the high-pressure reaction kettle into absolute ethanol, mixing and stirring for 10-20min to obtain a solid-liquid mixture;
(3) and (3) carrying out solid-liquid separation on the solid-liquid mixture, washing with absolute ethyl alcohol, and drying in vacuum to obtain the composite material.
2. A method of purifying a synthetic diamond according to claim 1, wherein: the volume concentration of oxygen in the nitrogen in the step (1) is lower than 1ppm, and the nitrogen preparation method is cryogenic air separation nitrogen preparation, pressure swing adsorption nitrogen preparation or membrane separation nitrogen preparation.
3. A method of purifying a synthetic diamond according to claim 1, wherein: after the temperature in the step (2) is reduced to be lower than 25 ℃, the mass ratio of the materials in the high-pressure reaction kettle to the absolute ethyl alcohol is 1: 3-5.
4. A method of purifying a synthetic diamond according to claim 1, wherein: and (4) the solid-liquid separation equipment in the step (3) is a centrifugal machine.
5. A method of purifying a synthetic diamond according to claim 1, wherein: in the step (3), the drying temperature is 40-60 ℃, and the vacuum degree is-0.08 to-0.05 MPa in the drying process in the vacuum drying oven.
6. A method of purifying a synthetic diamond according to claim 1, wherein: and (3) absorbing the ethanol of the gas in the step (2), and separating the gas from the ethanol through reduced pressure distillation.
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| CN112479201B true CN112479201B (en) | 2022-07-22 |
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Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9945185B2 (en) * | 2014-05-30 | 2018-04-17 | Baker Hughes Incorporated | Methods of forming polycrystalline diamond |
| KR102328995B1 (en) * | 2014-11-26 | 2021-11-23 | 나노리소스 주식회사 | Separation method of Detonation Nano Diamond |
| CN106564896B (en) * | 2015-10-09 | 2018-08-31 | 江苏天一超细金属粉末有限公司 | A method of extraction 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 |
| CN108190883B (en) * | 2018-03-09 | 2019-11-08 | 郑州航空工业管理学院 | A kind of method of purification of diamond |
| CN109305676B (en) * | 2018-11-26 | 2021-08-03 | 南京金瑞立丰硬质材料科技有限公司 | Simple and efficient method for removing graphite carbon in nano diamond ash |
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