Biocarbon powder, extraction method of biocarbon powder and preparation method of diamond

Through high-temperature decomposition and magnesium replacement reaction, high-purity biological carbon powder is extracted from the biological carbon source, solving the problem of high impurity content after carbonization of biological carbon sources and improving the quality of diamond preparation.

CN115849343BActive Publication Date: 2025-02-14FUNIK ULTRAHARD MATERIAL

Patent Information

Application Number
CN202211733262.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-12-22
Publication Date
2025-02-14
Estimated Expiration
2042-12-22

AI Technical Summary

Technical Problem

The carbon source components in organisms are complex, the impurity content after carbonization is high and the purity is low, which affects the quality of diamond preparation.

Method used

Biocarbon sources such as hair and ashes are used to decompose high temperatures, collect gases, alkali acid reactions and magnesium replacement reactions, and finally obtain high-purity biocarbon powder through filtration and washing.

Benefits of technology

The high purity (over 99.99%) extraction of biocarbon powder is achieved, impurities are removed, and the quality of diamond preparation is improved.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a method for extracting biocarbon powder, which mainly involves first fully burning a biocarbon source and collecting the generated gas products; then alkali dissolving and acid dissolving the collected gas products in turn to further decompose carbon dioxide gas; then the decomposed carbon dioxide gas undergoes a substitution reaction with a magnesium bar to produce carbon powder, and then separates biocarbon powder with a particle size of about 50 to 100 nm. Therefore, the above extraction method eliminates the presence of N, H, O, S and other metals in the biocarbon source, the purity of the carbon powder reaches more than 99.99%, the extraction effect is high in purity, and the carbon requirements of synthetic diamonds are met; and the biocarbon source is not limited to animal hair and bone ashes, and various organic materials can be used, with strong versatility. The present invention also provides a method for preparing diamonds using the above biocarbon powder, by which diamonds with a color of D‑E level and a clarity of FL level can be obtained.
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Description

Technical Field

[0001] The invention relates to the field of diamond manufacturing, and in particular to biological carbon powder and an extraction method thereof, and a diamond preparation method. Background Art

[0002] Diamond is the oldest gem in the world. The formation of diamond requires a long historical process. Among the mines currently mined, most diamonds were formed in the two periods of 3.3 billion years ago and 1.2 to 1.7 billion years ago. It is formed in the high temperature and high pressure environment deep in the earth. Scientists have discovered that diamond is a crystal structure of carbon and can be converted from carbon. Humans have used high temperature and high pressure presses to simulate the crust environment to synthesize diamonds from carbon. There are a lot of carbon elements in organisms on the earth, such as: plant tissues, animal ashes or hair, human ashes, tissues or hair, etc. Extracting carbon from organisms can synthesize biological diamonds. Organisms are preserved forever in another way.

[0003] To this end, Chinese invention patent application CN 106517141 A discloses a novel hair carbonization method, which comprises first removing impurities, degreasing, washing the hair, drying, and crushing the hair, and then placing the crushed hair into a vacuum carbonization machine and evacuating the hair to 10 -3 pa, then heat the hair to 600℃, keep it warm for 30 min, then heat it to 1000℃, keep it warm for 10 min, then heat it to 1250℃, keep it warm for 10 min, and finally cool it to room temperature to complete the carbonization. This method has a simple carbonization process, little pollution to the environment, and a high carbonization rate. It can basically completely carbonize the carbon-containing substances in the hair, which is beneficial to the graphitization treatment in the process of making artificial diamonds. The carbonization method has a wide range of uses. It can be applied not only to human or animal hair, but also to the carbonization of human or animal bones, providing a new type of raw material for the production of artificial diamonds. The carbonized hair can also be used to make souvenirs and handicrafts, which has high artistic and commercial value.

[0004] However, since the composition of carbon sources in organisms is complex, in addition to carbon, they also contain N, H, O, S, P and a small amount of metal elements. Although the above invention patent application completely carbonizes the carbon-containing substances in hair to form hair biochar, the hair biochar may also contain O, S, P and a small amount of metal elements, resulting in a high impurity content and low purity in the hair biochar, which seriously affects the quality of diamonds prepared using biochar. Summary of the invention

[0005] In view of this, the present invention is indeed necessary to provide a bio-carbon powder, a method for extracting high-purity bio-carbon powder using animal or human ashes, hair, nails and other tissues as raw materials, and a method for preparing diamonds using the bio-carbon powder as raw material.

[0006] Specifically, the technical solution adopted by the present invention is as follows:

[0007] A method for extracting carbon from an organism comprises the following steps:

[0008] Carbon source decomposition: In an oxygen environment, the biocarbon source is completely decomposed at high temperature to form gas products and ash, wherein the gas products include carbon dioxide, oxygen, water vapor, sulfur dioxide and nitrogen dioxide;

[0009] Carbon dioxide collection: firstly, the gas product is introduced into a degassed alkaline solution for a full reaction, then the first acidic solution is added for a full reaction to generate carbon dioxide gas, and the carbon dioxide gas is collected in a carbon source gas collection device;

[0010] Preparation of carbon powder: placing a burning magnesium bar in a carbon source gas collection device for collecting carbon dioxide gas to react to generate magnesium oxide and bio-carbon powder. After the reaction is completed, the carbon source gas collection device is washed with water and the magnesium oxide and bio-carbon powder therein are collected to obtain a turbid liquid; a second acidic solution is added to the turbid liquid until the magnesium oxide reacts completely, and the bio-carbon powder is obtained by filtering.

[0011] The biocarbon source is derived from plant, animal or human hair, animal bones or toenails, human nails or ashes. In addition to a large amount of carbon, the biocarbon source also contains a small amount of N, H, O, S, P and trace metal elements.

[0012] Based on the above, the step of decomposing the carbon source includes: placing the biological carbon source in a muffle furnace and a pure oxygen environment, and fully burning at 1200°C to 1500°C to form the gas product and ash; and collecting the gas product in a mixed gas collection device. In this way, after the biological carbon source is fully burned and decomposed, the elements such as C, N, H, O, S, and P therein mainly form the gas product, and the metal elements and other substances therein remain in the ash, and the raw materials are initially removed from impurities.

[0013] Preferably, the biocarbon source is kept at 1200° C. to 1500° C. for 30 to 60 minutes in a muffle furnace and a pure oxygen environment to allow the biocarbon source to be fully burned.

[0014] Based on the above, the step of collecting carbon dioxide includes: slowly passing the gas product in the mixed gas collection device into the degassed alkaline solution for sufficient reaction to generate sulfate, nitrate and carbonate to form a mixed salt solution; adding the first acidic solution to the mixed salt solution to allow the carbonate therein to fully react to generate carbon dioxide gas and collect it in the carbon source gas collection device.

[0015] Preferably, the degassed alkaline solution is a degassed alkaline solution, and the alkaline solution is a strong alkaline solution, for example, a saturated NaOH or KOH solution. The first acidic solution is a strong acidic solution such as H2SO4, HCl or HNO3.

[0016] In the step of collecting carbon dioxide, the main reactions occurring during the process of adding the degassed alkaline solution to form the mixed salt solution are as follows:

[0017] CO2+2NaOH=Na2CO3+H2O;

[0018] O2+2SO2+4NaOH=2Na2SO4+2H2O;

[0019] NO2+NaOH—NaNO3+H2O.

[0020] The reaction that occurs after adding the first acidic solution to the mixed salt solution is mainly:

[0021] Na2CO3+H2SO4=Na2SO4+H2O+CO2↑.

[0022] Thus, after the above-mentioned step of collecting carbon dioxide, the gas collected in the carbon source gas collection device is mainly CO2 gas, thereby achieving further impurity removal.

[0023] Based on the above, the steps of preparing the carbon powder include: placing the burning magnesium strip into the carbon source gas collection device so that the carbon dioxide therein reacts with magnesium to generate magnesium oxide and bio-carbon powder, and after the reaction is completed, washing the carbon source gas collection device with ultrapure water to form the turbid liquid; adding the second acidic solution to the turbid liquid and stirring it to convert the magnesium oxide therein into a soluble magnesium salt, and then filtering, washing to neutrality, and drying to obtain the bio-carbon powder. The particle size of the carbon powder is about 50 to 100 nm.

[0024] Preferably, the biochar powder is filtered out, washed to neutrality, and then placed in a vacuum drying oven at 80° C. to 120° C. to dry for 5 to 10 hours. The yield of the biochar powder obtained in this step is 11% to 15%.

[0025] The invention also provides a method for obtaining biochar powder by the extraction method.

[0026] The present invention also provides a method for preparing diamond, comprising the steps of:

[0027] Carbon powder graphitization: The above-mentioned biocarbon powder is graphitized to obtain 2H hexagonal graphite;

[0028] Diamond rough material synthesis: using the 2H-type hexagonal graphite as a raw material, synthesizing diamond rough material under the conditions of 5-7 GPa and 1200° C.-1500° C.;

[0029] Preparation of finished diamond products: The rough diamond material is crushed and cut to obtain finished diamond products.

[0030] The step of synthesizing the rough diamond material mainly uses the bio-carbon powder as raw material, adopts the existing method, and uses a six-sided top press to synthesize it under the conditions of 5-7 GPa and 1200℃-1500℃.

[0031] Based on the above preparation method, the step of graphitizing the carbon powder includes: in an inert gas environment, the carbon powder is treated at 2800°C to 3000°C in a graphitization furnace for 30 to 60 minutes, and then the 2H hexagonal graphite is obtained as the graphitization furnace is cooled. The inert gas is helium, neon, argon or xenon.

[0032] The extraction method of the above-mentioned biocarbon powder provided by the present invention mainly comprises the following steps: firstly, the biocarbon source is fully burned, and the generated gas products are collected; then, the collected gas products are sequentially alkali-dissolved and acid-dissolved to further decompose carbon dioxide gas; then, the decomposed carbon dioxide gas undergoes a substitution reaction with a magnesium bar to produce biocarbon powder, and then the biocarbon powder with a particle size of about 50 to 100 nm is separated. Thus, N, H, O, S and other metals in the biocarbon source cannot exist, and the purity of the biocarbon powder reaches more than 99.99%. Moreover, the biocarbon source is not limited to animal hair and bone ashes, and various organic materials can be used. Therefore, the extraction method has high extraction effect, purity and strong versatility.

[0033] Therefore, the purity of the bio-carbon powder provided by the present invention is relatively high, meeting the requirements of carbon for synthetic diamonds.

[0034] Furthermore, the preparation method of the above-mentioned diamond provided by the present invention first uses the above-mentioned biological carbon powder as a raw material, obtains 2H hexagonal graphite that can be used as a diamond raw material through graphitization treatment, and then uses 2H hexagonal stone as a raw material to synthesize diamond rough by an existing method, and then crushes, cuts and other treatments on the diamond rough to obtain a diamond finished product, and the diamond finished product reaches the color DE level and the clarity FL level. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 This is a SEM image of carbon powder extracted by the method for extracting carbon from a living organism provided by Example 1 of the present invention.

[0036] Figure 2 This is an XRD diagram of a product prepared by graphitizing the carbon powder in the preparation method provided in Example 2 of the present invention.

[0037] Figure 3 This is a photograph of a finished diamond product obtained by the preparation method provided in Example 2 of the present invention.

[0038] Figure 4 This is a photograph of a finished diamond product obtained by the preparation method provided by Example 4 of the present invention.

[0039] Figure 5 This is a photograph of a finished diamond product obtained by the preparation method provided in Example 6 of the present invention. DETAILED DESCRIPTION

[0040] The technical solution of the present invention is further described in detail below through specific implementation methods.

[0041] Embodiment 1

[0042] This embodiment provides a method for extracting carbon from an organism, comprising the following steps:

[0043] Carbon source decomposition: 100 g of dog hair is put into a graphite crucible, and then into a tubular muffle furnace. The crucible is placed into the tubular muffle furnace, and pure oxygen is introduced. The tubular muffle furnace is heated to 1200 degrees Celsius and kept warm for 30 minutes to fully burn the hair. The gas products formed by the combustion are collected by a mixed gas collection device; until the reaction is completely completed, the mass of the ash in the crucible no longer changes; wherein the gas products include carbon dioxide, oxygen, water vapor, sulfur dioxide and nitrogen dioxide, and the metal elements and other substances in the dog's hair remain in the ash, and the raw materials are initially cleaned;

[0044] Carbon dioxide collection: slowly pass the gas product in the mixed gas collection device into a beaker containing a degassed sodium hydroxide solution with a concentration of 40%, stir evenly until the reaction is complete, so that the water vapor, carbon dioxide, oxygen, sulfur dioxide and nitrogen oxides therein react in the sodium hydroxide solution to generate sodium sulfate, sodium nitrate and sodium carbonate, and form a mixed salt solution in the beaker; pour dilute sulfuric acid into the beaker containing the mixed salt solution, connect the upper end of the beaker to a gas collecting bottle, stir until the sodium carbonate therein fully reacts to generate carbon dioxide gas, and collect the discharged carbon dioxide gas in the gas collecting bottle;

[0045] Preparation of carbon powder: Place a burning magnesium stick in a gas collecting bottle containing carbon dioxide gas and burn it until magnesium completely replaces the biocarbon powder and the reaction is completed; use ultrapure water to wash the gas collecting bottle, collect the magnesium oxide and biocarbon powder after the reaction, and obtain a turbid liquid; add dilute sulfuric acid to the turbid liquid and stir it, so that magnesium oxide reacts with sulfuric acid to form magnesium sulfate salt, which is completely dissolved in the dilute sulfuric acid. Finally, filter out the carbon powder, wash it to neutrality, and place it in a drying oven at 80°C for 8 hours to obtain 11.2 g of pure, dry biocarbon powder with a particle size of about 50 to 100 nm, amorphous carbon.

[0046] This embodiment also provides a bio-carbon powder obtained by the above extraction method, such as Figure 1 shown.

[0047] The ash content of the pure dry biochar powder was tested by combustion method, and the ash content was less than 40 ppm; in this embodiment, the ash value of the ash test was 0. It can be seen that the purity of the biochar powder reached more than 99.99%.

[0048] Embodiment 2

[0049] This embodiment provides a method for preparing diamond, comprising the steps of:

[0050] Carbon powder graphitization: First, put the biocarbon powder provided in Example 1 into a graphite crucible, then put the graphite crucible containing the biocarbon powder into a graphitization furnace, and evacuate the graphitization furnace to 10 -3 After Pa, the heating was started, and argon gas was filled for protection, and the temperature was heated to 2800℃ and kept for 30 min; then the temperature was cooled and the graphitization furnace was taken out, and the following was obtained: Figure 2 The 2H hexagonal graphite shown; Figure 2 The XRD phase composition diagram shows that the graphitized powder is relatively pure and uniform 2H hexagonal graphite with no impurity peaks, and can be used as a raw material for diamond synthesis.

[0051] Diamond rough material synthesis: the 2H type hexagonal graphite is used as a raw material, uniformly mixed with a metal binder, and a six-sided top press is used to synthesize diamond rough material under the conditions of 5.5 GPa and 1250°C. The metal binder is iron and nickel in a mass ratio of 3:2, and the mass ratio of 2H type hexagonal graphite to metal binder is 4:1;

[0052] Preparation of finished diamond products: crushing and cutting the rough diamonds to obtain Figure 3 The diamond is shown as finished. Figure 3 The polished diamond shown is 3 mm in size, with a clarity of D and a color of FL.

[0053] Embodiment 3

[0054] This embodiment provides a method for extracting carbon from an organism. The extraction method is basically the same as the extraction method provided in Example 1, and the main differences are as follows:

[0055] Carbon source decomposition: 100 g chicken bones were used as the biocarbon source and heated to 1450 °C in a tubular muffle furnace for 60 min;

[0056] Carbon dioxide collection: 42% KOH solution is used as the alkaline solution, and dilute hydrochloric acid is used as the first acidic solution;

[0057] Preparation of carbon powder: Add the second acidic solution of dilute hydrochloric acid to the turbid liquid and completely dissolve it in the dilute hydrochloric acid. Finally, filter out the biocarbon powder, wash it to neutrality, and put it in a drying oven at 100°C for 8 hours to obtain 13.4 g of pure dry amorphous biocarbon powder with a particle size of about 40 to 90 nm.

[0058] This embodiment also provides a method for obtaining Figure 1 Basically the same amorphous bio-toner.

[0059] The ash content of the pure and dry biochar powder was tested by combustion method, and the ash content was less than 0.01%, which shows that the purity of the biochar powder is above 99.99%.

[0060] Embodiment 4

[0061] This embodiment provides a method for preparing diamond, comprising the steps of:

[0062] Carbon powder graphitization: First, put the biocarbon powder provided in Example 3 into a graphite crucible, then put the graphite crucible containing the biocarbon powder into a graphitization furnace, and evacuate the graphitization furnace to 10 -3 After Pa, the heating was started, and argon gas was filled for protection, and the temperature was heated to 3000℃ and kept for 45 min; then the temperature was cooled and the graphitization furnace was taken out, and the graphitization furnace was obtained. Figure 2 Basically the same graphitized powder: 2H hexagonal graphite;

[0063] Diamond rough material synthesis: the 2H hexagonal graphite is used as a raw material, uniformly mixed with a metal binder, and a six-sided top press is used to synthesize diamond rough material under the conditions of 6 GPa and 1400°C. The metal binder is iron and nickel in a mass ratio of 3:2, and the mass ratio of 2H hexagonal graphite to metal binder is 4:1;

[0064] Preparation of finished diamond products: crushing and cutting the rough diamonds to obtain Figure 4 The diamond is shown as finished. Figure 4The finished diamond shown is 4 mm in size, with a clarity of E and a color of FL.

[0065] Embodiment 5

[0066] This embodiment provides a method for extracting carbon from an organism. The extraction method is basically the same as the extraction method provided in Example 1, and the main differences are as follows:

[0067] Carbon source decomposition: 100 g of human hair was used as the biocarbon source and heated to 1300 °C in a tubular muffle furnace for 45 min;

[0068] Carbon dioxide collection: dilute nitric acid is used as the first acidic solution;

[0069] Preparation of carbon powder: Add the second acidic solution of dilute nitric acid to the turbid liquid and completely dissolve it in the dilute nitric acid. Finally, filter out the biocarbon powder, wash it to neutrality, and put it in a drying oven at 120°C for 5 h to obtain 14.7 g of pure dry amorphous biocarbon powder with a particle size of about 60 to 80 nm.

[0070] This embodiment also provides a method for obtaining Figure 1 Basically the same amorphous bio-toner.

[0071] The ash content of the pure and dry biochar powder was tested by combustion method, and the ash content was less than 0.01%, which shows that the purity of the biochar powder is above 99.99%.

[0072] Embodiment 6

[0073] This embodiment provides a method for preparing diamond, comprising the steps of:

[0074] Carbon powder graphitization: First, put the biocarbon powder provided in Example 3 into a graphite crucible, then put the graphite crucible containing the biocarbon powder into a graphitization furnace, and evacuate the graphitization furnace to 10 -3 After Pa, the heating was started, and argon gas was filled for protection, and the temperature was heated to 2900℃ and kept for 60 min; then the temperature was cooled and the graphitization furnace was taken out, and the graphitization furnace was obtained. Figure 2 Basically the same graphitized powder: 2H hexagonal graphite;

[0075] Diamond rough material synthesis: the 2H hexagonal graphite is used as a raw material, uniformly mixed with a metal binder, and a six-sided top press is used to synthesize diamond rough material under the conditions of 7 GPa and 1450°C. The metal binder is iron and nickel in a mass ratio of 3:2, and the mass ratio of 2H hexagonal graphite to metal binder is 4:1;

[0076] Preparation of finished diamond products: crushing and cutting the rough diamonds to obtain Figure 5 The diamond is shown as finished. Figure 5 The polished diamond shown is 6 mm in size, with a clarity of D and a color of FL.

[0077] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, ordinary technicians in the field should understand that the specific implementation methods of the present invention can still be modified or some technical features can be replaced by equivalents without departing from the spirit of the technical solution of the present invention, which should be included in the scope of the technical solution for protection of the present invention.

Claims

1. A method for preparing diamond, characterized in that: Includes steps: Carbon source decomposition: placing the biological carbon source in a muffle furnace and a pure oxygen environment, and keeping the temperature at 1200°C to 1500°C for 30 to 60 minutes, so that the biological carbon source is fully burned to form gas products and ash, and the gas products are collected in a mixed gas collection device, wherein the gas products include carbon dioxide, oxygen, water vapor, sulfur dioxide and nitrogen dioxide; Carbon dioxide collection: firstly, the gas product is introduced into a degassed alkaline solution for sufficient reaction, then a first acidic solution is added for sufficient reaction to generate carbon dioxide gas, and the carbon dioxide gas is collected in a carbon source gas collection device, wherein the degassed alkaline solution is a degassed NaOH or KOH solution; the first acidic solution is a H2SO4 solution, a HCl solution or a HNO3 solution; Preparation of carbon powder: placing the burning magnesium strip in the carbon source gas collection device to undergo a replacement reaction to generate magnesium oxide and biocarbon powder, washing the carbon source gas collection device with water after the reaction is completed and collecting the magnesium oxide and biocarbon powder therein to obtain a turbid liquid; adding a second acidic solution to the turbid liquid until the magnesium oxide reacts completely, filtering, washing to neutrality, and placing in a vacuum drying oven at 80°C to 120°C for 5 to 10 hours to obtain the biocarbon powder, and the particle size of the biocarbon powder is 50 to 100 nm; Carbon powder graphitization: In an inert gas environment, the biocarbon powder is treated in a graphitization furnace at 2800° C. to 3000° C. for 30 to 60 minutes, and then the graphitization furnace is cooled to obtain 2H hexagonal graphite; Diamond rough material synthesis: using the 2H-type hexagonal graphite as a raw material, uniformly mixing it with a metal in a mass ratio of 4:1, and synthesizing the diamond rough material using a six-sided top press at 5-7 GPa and 1200° C.-1500° C., wherein the metal is iron and nickel in a mass ratio of 3:2; Preparation of finished diamond products: The rough diamond material is crushed and cut to obtain finished diamond products.

2. The preparation method according to claim 1, characterized in that: The step of collecting carbon dioxide includes: slowly passing the gas product in the mixed gas collection device into the degassed alkaline solution for sufficient reaction to generate sulfate, nitrate and carbonate to form a mixed salt solution; adding the first acidic solution to the mixed salt solution to make the carbonate therein fully react to generate carbon dioxide gas and collect it in the carbon source gas collection device.

3. The preparation method according to claim 1, characterized in that: The steps of preparing the carbon powder include: placing the burning magnesium bar into the carbon source gas collection device so that the carbon dioxide therein reacts with magnesium to generate magnesium oxide and biocarbon powder, and after the reaction is completed, washing the carbon source gas collection device with ultrapure water to form the turbid liquid; adding the second acidic solution to the turbid liquid and stirring it so that the magnesium oxide therein is converted into a soluble magnesium salt, and then filtering, washing to neutrality, and drying to obtain the biocarbon powder.

Citation Information

Patent Citations

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