CN106006605A - Preparation method of highly-pure nanocarbon - Google Patents
Preparation method of highly-pure nanocarbon Download PDFInfo
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- CN106006605A CN106006605A CN201610376491.9A CN201610376491A CN106006605A CN 106006605 A CN106006605 A CN 106006605A CN 201610376491 A CN201610376491 A CN 201610376491A CN 106006605 A CN106006605 A CN 106006605A
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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Abstract
The invention discloses a preparation method of highly-pure nanocarbon. The preparation method comprises the following steps: spraying a sugar solution prepared from a carbohydrate material into concentrated sulfuric acid being in a high-speed stirring or ultrasonic vibrating state, keeping high-speed stirring or ultrasonic vibrating to obtain a reaction product, carrying out solid-liquid separation to obtain a solid product and a filtrate, repeatedly washing the solid product with pure water until the solid product is neutral and contains no sulfate radicals, and drying the washed solid product to obtain the highly-pure nanocarbon. The highly-pure nanocarbon can be directly obtained through a simple liquid phase reaction, so the purity is fully guaranteed, the production process is simplified, and the cost is reduced. The carbon content of the highly-pure nanocarbon reaches 99.99%, the average granularity is less than 30nm, the apparent density is about 1.0g/cm<3>, and the dry basis yield the product reaches 40%. The purity of the highly-pure nanocarbon is higher than requirements of national GB/T 3518-95, so the method is suitable for producing diamond, graphene, highly-pure graphite and highly-pure carbon products.
Description
Technical field
The invention belongs to environment-friendly type nano carbon technique field, relate to the preparation method of a kind of high-purity nm carbon element.
Background technology
Charcoal element is the general designation of charcoal and graphite material, is the nonmetal solid material based on carbon, the material that wherein Carbon Materials is substantially made up of non-graphite matter carbon, the material that graphite material is then substantially made up of graphite carbon.
Carbon materials is a widely used class material in modern industry and life, relies on its inherent character, is widely used in various different field and industry.As by using the difference of function, carbon product being divided into special conductive materials, special construction material and specific function material three major types: special conductive materials (such as electric arc furnace or burried arc furnace graphite electrode, carbonaceous electrode, natural electrode, electrode paste, electrolysis carbon anode or graphite anode, brush and spark machined mold materials, battery material etc.)；Special construction material is (such as iron-smelting furnace, ferro-alloy furnace, furnace of calcium carbide, the furnace lining of aluminium cell, the decelerating material of nuclear reactor and reflecting material, rocket or the head of guided missile or Nozzle Lining material, the corrosion-resistant graphite equipment of chemical industry, the high-abrasive material of mechanical industry and brush material, iron and steel and the crystallizer graphite liner of non-ferrous metal metallurgy industry casting continuously, quasiconductor and high-purity material are smelted with high purity graphite device etc.)；Specific function material (such as charcoal, glass-like carbon, Carbon foam, various classification pyrolytic carbons and pyrolytic graphite, recrystallized graphite, carbon fiber and composite, compound between graphite layers, fowler carbon, CNT etc.).Some carbon materials such as carbon fiber and composite thereof are to have structural material and the extraordinary carbon materials of the two-way performance of specific function material concurrently.
Carbon industry belongs to basic raw material industry, at the basic material that the national economic development is indispensable.Owing to physicochemical property and the mechanical performance of carbon material are better than metal material and macromolecular material under certain condition, there is good electric conductivity, heat stability and chemical stability, and there is the features such as the high intensity under higher corrosion resistance, the condition of high temperature, self lubricity, therefore, carbon industry is also a high-tech industry.Carbon material and goods thereof have been widely used in the fields such as metallurgy, electronics, chemical industry, machinery, sports equipment, medical treatment, the energy, Aero-Space, nuclear industry and military affairs, be all listed in and give priority to content in the technology development policies of national all previous issue.
Although China has been that carbonaceous product produces and big export country at present, but high-end product difficulty in the international market has right of speech, the carbon product of high-tech content, is to meet quasiconductor, solar power silicon crystal growing furnace large scale, high-purity, fine texture, the graphite of high intensity.The development of high-tech content carbon product, exploitation, application are boundless.In nuclear industry, atomic pile neutron moderator, reflective agent, produce isotope plume graphite, HTGR graphite, rocket and the jet pipe throat lining of guided missile, jet vane, combustor, nose cone and protective cover etc. are all special graphite goods.
Current high-purity charcoal element is all to purify common charcoal element, and not only process is numerous and diverse but also effect is not satisfactory, and common charcoal element then has a high temperature and with the course of processing polluted, and Nano carbon element the most on the market is Ultrafine Grinding product mostly.At present for the purification of charcoal element, the technique that there is no simple and effective cleaning, chemical method is difficult to find that the single medicament that can simultaneously remove all impurity, and high temperature method is substantially also intended to carry out after removing partial impurities in advance.The production process of high-purity nm charcoal element must be divided into several flow processs at present, and is mostly the process of high energy consumption high pollution high heat effect.
Summary of the invention
In order to optimize the production process of high-purity charcoal element, improving product purity, reduce production cost, reduce the pollution in production process and heat effect, the present invention proposes the preparation method of a kind of high-purity nm carbon element.
The present invention is realized by following technical proposal: the preparation method of a kind of high-purity nm carbon element, through following each step:
(1) it is 1:(3～100 by the pure weight ratio of saccharide material Yu concentrated sulphuric acid), the sugar liquid spraying being made into saccharide material is added in the concentrated sulphuric acid of high-speed stirred or ultrasonic activation, and at 20～160 DEG C, keep high-speed stirred or ultrasonic activation 10 seconds～5 hours, obtain reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element.
Further, the saccharide material of described step (1) is glucose, sucrose or fructose etc..
Further, the sugar liquid of described step (1) is that the pure water of saccharide material 0.5～20 mass times is dissolved gained.
Further, the sugar liquid of described step (1) is substituted by formalin or formaldehyde gas, and formalin is commercial formaldehyde or commercial formaldehyde adds pure water is diluted to the formalin that concentration is 10～40wt%；Formaldehyde gas is the gaseous formaldehyde that commercial formaldehyde is fractionated into obtaining.
Further, described saccharide material or formaldehyde be that top grade is pure, analytical pure or chromatographically pure commercial products.
Further, the high-speed stirred of described step (1) is to stir under rotating speed is 120～1000rpm.
Further, the ultrasonic activation of described step (1) is to vibrate under the ultrasound wave that frequency is 40～45kHZ.
Further, the concentrated sulphuric acid of described step (1) is analytical pure sulfuric acid or analytical pure sulfuric acid adds pure water is configured to the sulfuric acid solution that concentration is 65～98wt%.
Further, it is 65～98wt% that the filtrate of described step (2) is concentrated into concentration, is back in step (1) use as concentrated sulphuric acid.
The invention has the beneficial effects as follows: the present invention sets about from raw material, cast aside the common carbon raw materials being difficult to purify, select the basic chemical industry raw material being easily purified, abandon the flow process of high heat effect high pollution, only carry out simple liquid phase reactor (the most only needing two kinds of material single step reactions) directly obtain high-purity nm charcoal element, if improve raw material to top grade pure or chromatographically pure; can get ultrapure Nano carbon element, both fully ensured that purity, simplify production process, reduce again cost.The present invention is a low energy consumption clean environment firendly step flow process without heat effect, use is easier to purify inexpensive sulphuric acid, saccharide and formaldehyde and makees raw material, can the purity of Reliable guarantee product, make again production process become extremely simple, cost is also below the most current method.The carbon content of gained high-purity nm carbon element reaches 99.99%, particle mean size is less than 30nm, apparent density 1.0g/cm3Left and right, product butt yield reaches 40%.The requirement than national GB/T 3518-95 of the purity of gained high-purity nm carbon element is higher, can be suitably used for producing diamond, Graphene, high purity graphite, high-purity carbon goods.
Detailed description of the invention
Below by embodiment, the present invention will be further described.
Embodiment 1
(1) the pure water 50g dissolving of 0.5 mass times of 100g analytical pure glucose is obtained sugar liquid；It is 1:3 by the pure weight ratio of analytical pure glucose Yu concentrated sulphuric acid, the sugar liquid being made into saccharide material spraying is added in rotating speed as 120rpm under the concentration of high-speed stirred in 90wt% concentrated sulphuric acid, and at 20 DEG C, keep high-speed stirred or ultrasonic activation 5 hours, obtain reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element；Wherein filtrate is concentrated into concentration is 90wt%, is back in step (1) use as concentrated sulphuric acid.
The achievement data of gained high-purity nm carbon element is as once after testing:
Product appearance: black powder, product weight 39.7g, moisture 1.26%, product butt yield 39.2%, carbon content 99.99%, particle mean size 16nm, apparent density 0.91g/cm3。
Embodiment 2
(1) the pure water dissolving of 20 mass times of 100g sucrose is obtained sugar liquid；Being 1:100 by the pure weight ratio of sucrose Yu concentrated sulphuric acid, it is that under 40～45kHZ, the concentration of ultrasonic activation in 65wt% concentrated sulphuric acid, and keeps ultrasonic activation 5 hours at 70 DEG C that the sugar liquid being made into saccharide material spraying is added in frequency, obtains reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element；Wherein filtrate is concentrated into concentration is 65wt%, is back in step (1) use as concentrated sulphuric acid.
The achievement data of gained high-purity nm carbon element is as once after testing:
Product appearance: black powder, product weight 43.53g, moisture 1.43%, product butt yield 41.92%, carbon content ＞ 99.99%, particle mean size 19nm, apparent density 0.97g/cm3。
Embodiment 3
(1) taking the pure concentration of 200mL top grade is the formalin of 40wt%；Being 1:5 by the pure weight ratio of formalin Yu concentrated sulphuric acid, formalin spraying is added in the analytical pure concentration that frequency is ultrasonic activation under 45kHZ is in 98wt% concentrated sulphuric acid, and keeps ultrasonic activation 5 minutes at 60 DEG C, obtains reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element；Wherein filtrate is concentrated into concentration is 98wt%, is back in step (1) use as concentrated sulphuric acid.
The achievement data of gained high-purity nm carbon element is as once after testing:
Product appearance: black powder, product weight 35.6g, moisture 1.03%, product butt yield 39.15%, carbon content ＞ 99.99%, particle mean size 13nm, apparent density 1.17g/cm3。
Embodiment 4
(1) take the chromatographically pure formalin of 200mL and add pure water to be diluted to concentration be 10wt%；Being 1:20 by the pure weight ratio of formalin Yu concentrated sulphuric acid, formalin spraying is added in rotating speed is during under 1000rpm, the concentration of high-speed stirred is 95wt% concentrated sulphuric acid, and keeps high-speed stirred 2 minutes at 90 DEG C, obtains reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element；Wherein filtrate is concentrated into concentration is 95wt%, is back in step (1) use as concentrated sulphuric acid.
The achievement data of gained high-purity nm carbon element is as once after testing:
Product appearance: black powder, product weight 36.1g, moisture 1.36%, product butt yield 39.58%, carbon content ＞ 99.99%, particle mean size 11nm, apparent density 1.21g/cm3。
Embodiment 5
(1) the pure water dissolving of 2 mass times of 200g analytical pure sucrose is obtained sugar liquid；Be 1:10 by the pure weight ratio of saccharide material Yu concentrated sulphuric acid, the sugar liquid being made into saccharide material spraying is added in rotating speed as 800rpm under the concentration of high-speed stirred in 90wt% concentrated sulphuric acid, and keep high-speed stirred 10 seconds at 160 DEG C, obtain reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element；Wherein filtrate is concentrated into concentration is 90wt%, is back in step (1) use as concentrated sulphuric acid.
The achievement data of gained high-purity nm carbon element is as once after testing:
Product appearance: black powder, product weight 85.1g, moisture 1.38%, product butt yield 41.96%, carbon content 99.99%, particle mean size 28nm, apparent density 1.03g/cm3。
Embodiment 6
(1) the pure water dissolving of 5 mass times of pure for 200g top grade fructose is obtained sugar liquid；Be 1:12 by the pure weight ratio of saccharide material Yu concentrated sulphuric acid, the sugar liquid being made into saccharide material spraying is added in rotating speed as 1000rpm under the concentration of high-speed stirred in 95wt% concentrated sulphuric acid, and keep high-speed stirred 5 minutes at 65 DEG C, obtain reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element；Wherein filtrate is concentrated into concentration is 95wt%, is back in step (1) use as concentrated sulphuric acid.
The achievement data of gained high-purity nm carbon element is as once after testing:
Product appearance: black powder, product weight 80.1g, moisture 1.02%, product butt yield 39.64%, carbon content 99.99%, particle mean size 15nm, apparent density 0.93g/cm3。
Embodiment 7
(1) it is 1:50 by the pure weight ratio of formaldehyde Yu concentrated sulphuric acid, pure for top grade formaldehyde is fractionated into the formaldehyde gas 50g obtained, formaldehyde gas is passed through during under rotating speed is 800rpm, the concentration of high-speed stirred is 75wt% concentrated sulphuric acid, and at 50 DEG C, keep high-speed stirred or ultrasonic activation 10 minutes, obtain reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element；Wherein filtrate is concentrated into concentration is 75wt%, is back in step (1) use as concentrated sulphuric acid.
The achievement data of gained high-purity nm carbon element is as once after testing:
Product appearance: black powder, product weight 19.6g, moisture 1.13%, product butt yield 38.75%, carbon content ＞ 99.99%, particle mean size 9nm, apparent density 1.32g/cm3。
Claims (9)
1. the preparation method of a high-purity nm carbon element, it is characterised in that through following each step:
(1) it is 1:(3～100 by the pure weight ratio of saccharide material Yu concentrated sulphuric acid), the sugar liquid spraying being made into saccharide material is added in the concentrated sulphuric acid of high-speed stirred or ultrasonic activation, and at 20～160 DEG C, keep high-speed stirred or ultrasonic activation 10 seconds～5 hours, obtain reactant；
(2) step (1) gained reactant is obtained solid product and filtrate through solid-liquid separation, with pure water cyclic washing solid product until neutral and sulfate radical-free ion, then drying, i.e. obtain high-purity nm carbon element.
The preparation method of high-purity nm carbon element the most according to claim 1, it is characterised in that: the saccharide material of described step (1) is glucose, sucrose or fructose.
The preparation method of high-purity nm carbon element the most according to claim 1, it is characterised in that: the sugar liquid of described step (1) is that the pure water of saccharide material 0.5～20 mass times is dissolved gained.
The preparation method of high-purity nm carbon element the most according to claim 1, it is characterized in that: the sugar liquid of described step (1) is substituted by formalin or formaldehyde gas, formalin is commercial formaldehyde or commercial formaldehyde adds pure water is diluted to the formalin that concentration is 10～40wt%；Formaldehyde gas is the gaseous formaldehyde that commercial formaldehyde is fractionated into obtaining.
The preparation method of high-purity nm carbon element the most according to claim 1, it is characterised in that: the high-speed stirred of described step (1) is to stir under rotating speed is 120～1000rpm.
The preparation method of high-purity nm carbon element the most according to claim 1, it is characterised in that: the ultrasonic activation of described step (1) is to vibrate under the ultrasound wave that frequency is 40～45kHZ.
The preparation method of high-purity nm carbon element the most according to claim 1, it is characterised in that:, the concentrated sulphuric acid of described step (1) is analytical pure sulfuric acid or analytical pure sulfuric acid adds pure water is configured to the sulfuric acid solution that concentration is 65～98wt%.
The preparation method of high-purity nm carbon element the most according to claim 1, it is characterised in that: it is 65～98wt% that the filtrate of described step (2) is concentrated into concentration, is back in step (1) use as concentrated sulphuric acid.
9. according to the preparation method of the high-purity nm carbon element described in claim 1,2 or 4, it is characterised in that: described saccharide material or formaldehyde are that top grade is pure, analytical pure or chromatographically pure commercial products.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109719512A (en) * | 2019-01-15 | 2019-05-07 | 江苏卡米特激光智能科技有限公司 | A kind of dedicated laser cutting machine of panel beating |
| WO2019166676A1 (en) * | 2018-03-01 | 2019-09-06 | Business Research And Diamonds, S.L. | Method for obtaining synthetic diamonds from sucrose and device for carrying out said method |
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| CN1587032A (en) * | 2004-09-14 | 2005-03-02 | 武汉大学 | Hollow charcoal and its synthetic method and use |
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2016
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| CN1587032A (en) * | 2004-09-14 | 2005-03-02 | 武汉大学 | Hollow charcoal and its synthetic method and use |
| CN103693633A (en) * | 2013-12-04 | 2014-04-02 | 上海交通大学 | Method for green synthesis of fluorescent chiral carbon dots |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019166676A1 (en) * | 2018-03-01 | 2019-09-06 | Business Research And Diamonds, S.L. | Method for obtaining synthetic diamonds from sucrose and device for carrying out said method |
| ES2724214A1 (en) * | 2018-03-01 | 2019-09-09 | Business Res And Diamonds S L | PROCEDURE FOR OBTAINING SYNTHETIC DIAMONDS FROM THE SACAROSE AND EQUIPMENT TO CARRY OUT THIS PROCEDURE (Machine-translation by Google Translate, not legally binding) |
| CN112512968A (en) * | 2018-03-01 | 2021-03-16 | 商业研究与钻石有限公司 | Method for obtaining synthetic diamonds from sucrose and device for implementing said method |
| JP2021515741A (en) * | 2018-03-01 | 2021-06-24 | ビジネス リサーチ アンド ダイアモンズ、エセ．エレ． | A method for obtaining synthetic diamond from sucrose and an apparatus for carrying out the above method. |
| CN112512968B (en) * | 2018-03-01 | 2024-01-12 | 商业研究与钻石有限公司 | Method for obtaining synthetic diamond from sucrose and device for carrying out said method |
| CN109719512A (en) * | 2019-01-15 | 2019-05-07 | 江苏卡米特激光智能科技有限公司 | A kind of dedicated laser cutting machine of panel beating |
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