CN101033065A - Method of purifying environment-friendly type ultra-fine diamond - Google Patents
Method of purifying environment-friendly type ultra-fine diamond Download PDFInfo
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Abstract
This invention relates to a purification method for super-fine diamond including the following steps: 1, mixing a salt solution with super-fine diamond micro-powder to get a solid-liquid mixture, in which, the weight ratio of the micro-powder and the salt in the salt solution is 1 : 0.25-5 and the concentration of the solution is 5-50% g*ml-1, the solid-liquid mixture is scattered by ultrasonic for 0.5-3h, 2, moving the processed mixture into a reaction kettle in the filling degree of 20%-60%V/V under 120-220deg.C for 2-18h, 3, taking out the solid-liquid mixture from the kettle, adding acid adjusting solution to get the pH value under 3 to be processed with ultrasonic for 0.5-1h, taking separated diamond micro-powder to clean it to pH=3-4, 4, drying it to get the product.
Description
Technical field
The present invention relates to the method for purification of ultra-fine diamond, belong to field of new.
Background technology
Adamantine synthetic have static pressure method, blast lash method and detonation method etc., these synthetic methods can obtain the diamond of different-grain diameter grade, must just can be applied to different fields through after purification and the classification.In recent years, the application of nanometer (ultra-fine) yardstick diamond at the aspects such as modification, polymer composites, computer chip and printed wiring of super finishing polish, scuff-resistant coating, lubricating oil shown very fine prospect.Yet more and more high to the requirement of its purity along with going deep into of ultra-fine diamond applied research, for specific end use, the content requirement of its impurity (mainly referring to graphite, agraphitic carbon, silicon-dioxide and some metallic element) is very tight.Seek out the high pure and ultra-fine diamond that meets this requirement, adopt conventional method of purification to be difficult to accomplish.In the synthetic and production process of man-made diamond, purifying technique is the most complicated, and required time is also longer, and purification costs accounts for 60% of total cost, and the result who purifies directly affects adamantine ultimate yield, purity and surface property, and is therefore most important in whole process of production.For adamantine purification processes, purification process mainly comprises three parts: 1. remove metal solvent, acid treatment, electrolysis process or two kinds of technologies are combined.2. remove graphite and agraphitic carbon,, use separately or the use of composition mixing acid, need to add inorganic oxidizer (as potassium permanganate and potassium bichromate) sometimes with nitric acid, sulfuric acid and perchloric acid etc.
Traditional method is: nitric acid, sulfuric acid and perchloric acid etc. use separately or form potassium permanganate and the potassium bichromate that mixing acid uses or inorganic oxidizer is made in interpolation in acid, to remove graphite and agraphitic carbon.As the patent of invention of Xu Kang etc.: with the submergence of diamond work in-process, be heated to boiling with the vitriol oil, and in reactant, add concentrated nitric acid, whole oxidized the removing of non-diamond carbon in the diamond work in-process with speed slowly.The novel process that Jia Yongsheng removes graphite is: powder level graphite is removed in flotation behind the ball milling diamond, and adds the sulfuric acid infiltration with nitric acid.When reaching the vitriolic reaction conditions, improved speed of response like this, not only graphite has been removed, also residues such as contained little metal Ni, Co can have been removed.Deutsches Wirtschafts Patent DD224575A proposes to utilize copper salt solution when being higher than 450 ℃ of temperature, is decomposed into cupric oxide or Red copper oxide, is blended in oxygenation reaction under 540 ℃ of high temperature with copper salt solution and diamond, and product goes out pickling with hydrochloric acid or nitric acid boiling back water.United States Patent (USP) 3,348918 has proposed under the temperature of 250～500 ℃ of scopes the plumbous oxide of making catalyzer to be mixed with diamond, by removing non-diamond carbon with the selective oxidation of molecular oxygen.
Under the high pressure high temperature condition, graphite is transformed into the reaction process that diamond is a complexity.Post reaction mixture also has catalyst metal and chemical combination thereof except that diamond and graphite.Remove catalyst metal: the processing to catalyst alloy has two kinds of different methods: acidleach facture, treatment with electrolytic method.The former is oxidized to solvable new salt with metal with acid with strong oxidizing property, removes through washing.Though this method can be loose with graphite oxidation when removing metallic impurity, expends ample resources, also is unfavorable for producer's health.Electrolytic process has better economic benefit and environmental effect comparatively speaking, and technology is ripe relatively, is extensively adopted in the world at present.But this method cost is too high.
Chemical method is mainly still adopted in purification for ultra-fine diamond at present, as:
People such as Shi Wensheng (functional materials 1997,28 (5) 522-525 pages or leaves) handle and hydrofluoric acid water bath processing detonation method synthesizing superfine diamond with concentrated nitric acid and the boiling of vitriol oil mixed solution, remove most of impurity, but the chemical ingredients detected result is not provided.People such as Wang Dazhi (Journal of Inorganic Materials Vol.10, No.3Sept., 1995,281-287 page or leaf) handle detonation method synthetic ultra-fine diamond down with the hydrofluoric acid normal pressure after soaking with perchloric acid and nitric acid mixing acid again.
Chinese patent application publication number CN 1385366 A (method of purification of Nano diamond) then adopt the vitriol oil and potassium permanganate mixed solution oxidizing reaction, handle detonation method synthetic ultra-fine diamond.People such as Chen Pengwan (Chinese Journal Of High Pressure Physics Vol.13, No.1Mar., 1999,59-63 page or leaf) adopt the vitriol oil and potassium permanganate mixed solution purification detonation method synthetic ultra-fine diamond, analyze collection of illustrative plates but provided laser Raman spectroscopy, at 1600cm
-1Near shown the Raman peak of graphite broadening.Chinese patent application publication number CN 1480252A (method of cerium salt purifying Nano diamond particle) is at detonation method synthetic ultra-fine diamond, with ceric ammonium nitrate or ammonium cerous sulfate oxidation non-diamond carbon, analyze with X-ray diffraction, only explained adamantine strong peak, and not mentioned non-diamond carbon is residual.Chinese patent application publication number CN1400162A (the half-finished purification process of diamond synthesis that contains non-diamond carbon) is with the vitriol oil and concentrated nitric acid oxidation detonation method synthetic diamond, different is to adopt to add nitric acid in batches, and the impurity analysis result is not provided.Day disclosure is speciallyyed permit flat 63-303806 blast lash method synthetic diamond and is handled with chloroazotic acid, nitrosonitric acid or concentrated nitric acid earlier, perhaps add potassium permanganate, sodium chlorate, hydrogen peroxide as required and carry out oxide treatment, can not remove graphite fully, handle also residual graphite three times with the nitration mixture of the vitriol oil, strong phosphoric acid and concentrated nitric acid again.
In sum, in numerous diamond methods of purification, the reagent that relates generally to is severe corrosive acid, and seriously polluted to environment is to having relatively high expectations of equipment for purifying.China is man-made diamond big producing country, a large amount of diadusts is arranged, the not flammable residue of most of products between 0.5～10wt%, dioxide-containing silica is greater than 0.3wt%, often between 1～3wt%, and containing a spot of non-diamond carbon, these micro mists all need to be further purified.Therefore the novel process of purification diadust of developing a kind of environment-friendly type is extremely urgent.
Summary of the invention
The object of the present invention is to provide a kind of method of purification that operator's health is endangered the environment-friendly type ultra-fine diamond little, that environmental pollution is few, low for equipment requirements.
To achieve these goals, technical scheme of the present invention is: a kind of method of purification of environment-friendly type ultra-fine diamond is characterized in that it comprises the steps:
1), salts solution and ultra-fine diamond micro mist are mixed, solid-liquid mixtures, wherein the weight ratio of the salt of ultra-fine diamond micro mist and salts solution (being the solid content of salts solution) is 1: 0.25～5, the concentration of salts solution is 5～50%g*ml
-1(5～50%g*ml
-1Contain 5～50g salt in the expression 100ml solvent); Solid-liquid mixtures is handled with ultrasonic dispersing, 0.5～3 hour treatment time;
2), will move in the reactor through the solid-liquid mixtures of ultrasonication, the compactedness of reactor is 20%～60%V/V (V represents volume), temperature of reaction is controlled at 120～220 ℃, the reaction times is 2～18 hours;
3) from reactor, take out solid-liquid mixtures, add below the acid-conditioning solution pH value to 3 ultrasonication 0.5～1 hour; Adopt whizzer or membrane filter plant to isolate diadust, diadust with deionized water wash to pH=3～4;
4) diamond after the taking-up washing adopts oven dry, spraying drying or lyophilize or vacuum-drying, gets product (promptly obtaining not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide).
Above-mentioned salt is that the first kind salt and the second class salt mix, and the weight ratio of the first kind salt and the second class salt is 1: 5～8: 1; Described first kind salt is any one or any mixing that (contains any two kinds) more than two kinds in ceric sulfate, ammonium cerous sulfate, cerium oxide, potassium permanganate, Potassium Persulphate, Sodium Persulfate, ammonium persulphate, saltpetre, SODIUMNITRATE, ammonium nitrate, sodium oxide, sodium peroxide, potassium oxide, the Potassium peroxide, any when (containing any two kinds) more than two kinds and mixing, be any proportioning; The described second class salt is any one or any mixing that (contains any two kinds) more than two kinds in Potassium monofluoride, Sodium Fluoride, Neutral ammonium fluoride, potassium hydroxide, the sodium hydroxide, and is any when (containing any two kinds) more than two kinds and mixing, and is any proportioning.
Above-mentioned ultra-fine diamond micro mist is meant common commercially available ultra-fine diamond micro mist, granularity＜5 μ m, 1000 ℃ of burning decrement＞90wt%.
Above-mentioned acid is nitric acid or hydrochloric acid.
The present invention compares maximum characteristics and is not adopt volatile acid to make oxygenant with the method for purification of routine, but adopt salts solution to replace severe corrosive acid to remove non-diamond carbon and silicon-containing compound in the diamond, the operator is endangered little, environmentally friendly, reduced requirement equipment.This processing unit is simple, and the reaction times is short.Using this technology can obtain the remaining high-purity diadust less than 0.1wt% of noncombustibles, is a kind of effective method of purification that obtains ultrapure ultra-fine diamond at present.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
The former powder of diamond is pulverized through airflow milling, obtained ultra-fine (ultra-fine finger granularity＜5 μ m) diadust.
Take by weighing 1.01g ultra-fine diamond micro mist (this micro mist is through 1000 ℃ of calcinations, and burning decrement is 97.10wt%, and dioxide-containing silica is 2.50wt%), in 6ml teflon-lined reactor, adding 1.5ml concentration is 50%g*ml
-1Ammonium fluoride solution (50%g*ml
-1Contain 50g Neutral ammonium fluoride solute in the expression 100ml solvent), 0.5ml concentration is 45%g*ml
-1Ammonium cerous sulfate solution (45%g*ml
-1Contain 45g ammonium cerous sulfate solute in the expression 100ml solvent), ultrasonication 0.5 hour; Reactor is put into baking oven, in 160 ℃ of heating 8 hours, after the cooling, takes out reactor; Pour out supernatant liquid after the cooling, flush out diamond, add nitric acid regulator solution pH value below 3, ultrasonication 30min; Centrifuge washing repeats above-mentioned washing step, washs to pH=3; The direct spraying drying of suspension obtains the ultra-fine adamantine stone powder.After testing: 1000 ℃ of burning decrement 99.94wt% (weight percentage), dioxide-containing silica 0.0025wt%.
Embodiment 2:
Take by weighing 1.00g through broken ultra-fine diamond micro mist (this micro mist is through 1000 ℃ of calcinations, and burning decrement equals 99.70wt%, and dioxide-containing silica equals 0.25wt%); In 60ml teflon-lined reactor, adding 15ml concentration is 4%g*ml
-1Fluorinse, 5ml concentration are 15%g*ml
-1Ammonium persulfate solution, 5ml concentration are 65%g*ml
-1Ceric sulfate solution, ultrasonication 0.5 hour; Put into baking oven, in 200 ℃ of heating 10 hours; After the cooling, open reactor and pour out supernatant liquid, flush out diamond, add nitric acid regulator solution pH value below 3, ultrasonication 60min, centrifuge washing add the some ultra-sonic dispersion of deionized water to pH=4, and the oven dry of centrifugal back obtains the ultra-fine adamantine stone powder.After testing: 1000 ℃ of burning decrement 99.96wt%, dioxide-containing silica 0.0023wt%.
Embodiment 3:
A kind of method of purification of environment-friendly type ultra-fine diamond, it comprises the steps:
1) be 5%g*ml, with 12ml concentration
-1Mixing salt solution (the mixing salt solid content is 0.6g) and 2.4g ultra-fine diamond micro mist mix, get solid-liquid mixtures, mixing salt is potassium permanganate, Potassium Persulphate and Potassium monofluoride, and the solid content of potassium permanganate, Potassium Persulphate, Potassium monofluoride is respectively in the mixing salt solution: 0.05g, 0.05g, 0.5g (weight ratio that is the first kind salt and the second class salt is 1: 5); Solid-liquid mixtures is handled with ultrasonic dispersing, 0.5 hour treatment time;
2), will move into (this moment, the compactedness of reactor was 20%V/V) in the 60ml teflon-lined reactor through the solid-liquid mixtures of ultrasonication, temperature of reaction is controlled at 120 ℃, the reaction times is 2 hours;
3) from reactor, take out solid-liquid mixtures, add hydrochloric acid conditioning solution pH value to 2, ultrasonication 0.5 hour; Adopt whizzer to isolate diadust, diadust with deionized water wash to pH=3;
4) diamond after the taking-up washing, oven dry gets product (promptly obtaining not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide).
Embodiment 4:
A kind of method of purification of environment-friendly type ultra-fine diamond, it comprises the steps:
1) be 30%g*ml, with 24ml concentration
-1Mixing salt solution (the mixing salt solid content is 7.6g) and 2.4g ultra-fine diamond micro mist mix, get solid-liquid mixtures, mixing salt is SODIUMNITRATE, ammonium nitrate, sodium oxide, sodium peroxide, potassium hydroxide and sodium hydroxide, and the solid content of SODIUMNITRATE, ammonium nitrate, sodium oxide, sodium peroxide, potassium hydroxide, sodium hydroxide is respectively in the mixing salt solution: 1.2g, 1.2g, 1.2g, 1.2g, 1.2g, 1.2g; Solid-liquid mixtures is handled with ultrasonic dispersing, 2.0 hours treatment times;
2), will move into (this moment, the compactedness of reactor was 40%V/V) in the 60ml teflon-lined reactor through the solid-liquid mixtures of ultrasonication, temperature of reaction is controlled at 180 ℃, the reaction times is 10 hours;
3) from reactor, take out solid-liquid mixtures, add hydrochloric acid conditioning solution pH value to 2.9, ultrasonication 1.0 hours; Adopt membrane filter plant to isolate diadust, diadust with deionized water wash to pH=3.5;
4) diamond after the taking-up washing, lyophilize gets product (promptly obtaining not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide).
Embodiment 5:
A kind of method of purification of environment-friendly type ultra-fine diamond, it comprises the steps:
1) be 50%g*ml, with 36ml concentration
-1Mixing salt solution (the mixing salt solid content is 18g) and 3.6g ultra-fine diamond micro mist mix, get solid-liquid mixtures, mixing salt is saltpetre, potassium oxide, Potassium peroxide, Sodium Persulfate, cerium oxide and Neutral ammonium fluoride, and the solid content of saltpetre, potassium oxide, Potassium peroxide, Sodium Persulfate, cerium oxide, Neutral ammonium fluoride is respectively in the mixing salt solution: 3.2g, 3.2g, 3.2g, 3.2g, 3.2g, 2.0g (weight ratio that is the first kind salt and the second class salt is 8: 1); Solid-liquid mixtures is handled with ultrasonic dispersing, 3.0 hours treatment times;
2), will move into (this moment, the compactedness of reactor was 60%V/V) in the 60ml teflon-lined reactor through the solid-liquid mixtures of ultrasonication, temperature of reaction is controlled at 220 ℃, the reaction times is 18 hours;
3) from reactor, take out solid-liquid mixtures, add hydrochloric acid conditioning solution pH value to 2.5, ultrasonication 1 hour; Adopt membrane filter plant to isolate diadust, diadust with deionized water wash to pH=4;
4) diamond after the taking-up washing adopts lyophilize, gets product (promptly obtaining not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide).
Claims (4)
1. the method for purification of an environment-friendly type ultra-fine diamond is characterized in that it comprises the steps:
1), salts solution and ultra-fine diamond micro mist are mixed, solid-liquid mixtures, wherein the weight ratio of the salt of ultra-fine diamond micro mist and salts solution is 1: 0.25～5, the concentration of salts solution is 5～50%g*ml
-1Solid-liquid mixtures is handled with ultrasonic dispersing, 0.5～3 hour treatment time;
2), will move in the reactor through the solid-liquid mixtures of ultrasonication, the compactedness of reactor is 20%～60%V/V, temperature of reaction is controlled at 120～220 ℃, the reaction times is 2～18 hours;
3) from reactor, take out solid-liquid mixtures, add below the acid-conditioning solution pH value to 3 ultrasonication 0.5～1 hour; Adopt whizzer or membrane filter plant to isolate diadust, diadust with deionized water wash to pH=3～4;
4) diamond after the taking-up washing adopts oven dry, spraying drying or lyophilize or vacuum-drying, gets product.
2. the method for purification of a kind of environment-friendly type ultra-fine diamond according to claim 1 is characterized in that: described salt is that the first kind salt and the second class salt mix, and the weight ratio of the first kind salt and the second class salt is 1: 5～8: 1; Described first kind salt is any one or any mixing more than two kinds in ceric sulfate, ammonium cerous sulfate, cerium oxide, potassium permanganate, Potassium Persulphate, Sodium Persulfate, ammonium persulphate, saltpetre, SODIUMNITRATE, ammonium nitrate, sodium oxide, sodium peroxide, potassium oxide, the Potassium peroxide, any when mixing more than two kinds, be any proportioning; The described second class salt is any one or any mixing more than two kinds in Potassium monofluoride, Sodium Fluoride, Neutral ammonium fluoride, potassium hydroxide, the sodium hydroxide, and is any when mixing more than two kinds, is any proportioning.
3. the method for purification of a kind of environment-friendly type ultra-fine diamond according to claim 1 is characterized in that: the granularity of described ultra-fine diamond micro mist＜5 μ m, 1000 ℃ of burning decrement＞90wt%.
4. the method for purification of a kind of environment-friendly type ultra-fine diamond according to claim 1 is characterized in that: described acid is nitric acid or hydrochloric acid.
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| CN103043632A (en) * | 2012-12-14 | 2013-04-17 | 河南富耐克超硬材料股份有限公司 | Purification method for diamond and cubic boron nitride abrasive or micro-powder |
| 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 |
| CN104624358A (en) * | 2013-11-07 | 2015-05-20 | 孔龙 | Diamond abrasive material impurity removing method |
| CN105480972A (en) * | 2015-12-25 | 2016-04-13 | 山东重山光电材料股份有限公司 | Continuous preparation method of fluorinated diamond |
| CN106587046A (en) * | 2016-12-30 | 2017-04-26 | 郑州大学 | Purification method of artificial diamond |
| CN109305676A (en) * | 2018-11-26 | 2019-02-05 | 南京金瑞立丰硬质材料科技有限公司 | The minimizing technology of graphitic carbon in a kind of nano diamond ash material being simple and efficient |
| CN109305677A (en) * | 2018-11-26 | 2019-02-05 | 南京金瑞立丰硬质材料科技有限公司 | The minimizing technology of graphitic carbon in a kind of nano diamond ash material |
| CN110980725A (en) * | 2019-11-04 | 2020-04-10 | 三门峡天钻晶体材料有限公司 | Method for removing metal impurities and residual graphite in diamond material |
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| 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 |
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| CN109305676A (en) * | 2018-11-26 | 2019-02-05 | 南京金瑞立丰硬质材料科技有限公司 | The minimizing technology of graphitic carbon in a kind of nano diamond ash material being simple and efficient |
| CN109305677A (en) * | 2018-11-26 | 2019-02-05 | 南京金瑞立丰硬质材料科技有限公司 | The minimizing technology of graphitic carbon in a kind of nano diamond ash material |
| CN109305677B (en) * | 2018-11-26 | 2021-06-29 | 南京金瑞立丰硬质材料科技有限公司 | Method for removing graphite carbon in nano diamond ash |
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| CN110980725A (en) * | 2019-11-04 | 2020-04-10 | 三门峡天钻晶体材料有限公司 | Method for removing metal impurities and residual graphite in diamond material |
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| CN114350318A (en) * | 2022-01-12 | 2022-04-15 | 河南联合精密材料股份有限公司 | Diamond abrasive and preparation method thereof |
| CN114853007A (en) * | 2022-06-24 | 2022-08-05 | 河南省豫星碳材有限公司 | Purification process of super-ultra-fine diamond micro powder |
| CN114853007B (en) * | 2022-06-24 | 2024-06-28 | 河南省豫星碳材有限公司 | Purification process of superfine diamond micropowder |
| CN115340089A (en) * | 2022-08-24 | 2022-11-15 | 内蒙古唐合科技有限公司 | Method for purifying artificial diamond |
| CN115340089B (en) * | 2022-08-24 | 2024-02-06 | 内蒙古唐合科技有限公司 | Method for purifying artificial diamond |
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