CN109305676A - The minimizing technology of graphitic carbon in a kind of nano diamond ash material being simple and efficient - Google Patents
The minimizing technology of graphitic carbon in a kind of nano diamond ash material being simple and efficient Download PDFInfo
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- CN109305676A CN109305676A CN201811416838.3A CN201811416838A CN109305676A CN 109305676 A CN109305676 A CN 109305676A CN 201811416838 A CN201811416838 A CN 201811416838A CN 109305676 A CN109305676 A CN 109305676A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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Abstract
The invention discloses a kind of minimizing technologies of graphite state carbon in nano diamond ash material, including Nano diamond detonation ash is added into low melting point alkaline medium, are warming up to 400 ~ 500oThe step of nitrite is added in C, under the conditions of 400 ~ 600 DEG C, reacts 0.5 ~ 5 hour, after reaction solution is cooling, is dissolved in water and isolates diamond dust, and filtering washes, is dry, obtaining purified nanotubes diamond product.The present invention is under metal oxide in ash material and the lesser situation of salt, dioxide-containing silica, it can not be after further treatment, high purity product is directly provided, this method has many advantages, such as that simple production process, equipment requirement are lower, product purity is high, production technology safety and environmental protection.
Description
Technical field
The present invention relates to a kind of methods of purification of diamond, are received more particularly to a kind of based on what explosive detonation mode was produced
The minimizing technology of graphite state carbon, belongs to technical field of material in rice diamond ash material.
Background technique
Nano diamond is in Ultraprecise polished, advanced adjustment (lubrication) oil, wear-resistant material additive, wearing face Composite Coatings
Equal fields tool has been widely used.
Detonation Process is artificial synthesized one of the important method of Nano diamond, in detonation ash material impurity, graphite state carbon
Content is maximum, is also most difficult to remove.Mainly there is two class of chemical oxidation and high-temperature air oxidation for the removal of graphite state carbon at present
(" Ultracrystalline Diamond-Sytheses, Properties and Applications ", Willian
Andrew Publishing,NewYork,2006).Chemical oxidation method includes perchloric acid, the concentrated sulfuric acid+nitric acid ,+three oxygen of sulfuric acid
Change the modes such as two chromium, ozone, nitric acid, wherein sulfuric acid+nitric acid has formed commercial scale, but this method is at high temperature under high pressure
(280 DEG C) reactions, it is very high for equipment requirement, and also seriously corroded, product purity be not high.CN1385366A and
CN01114455.6 is disclosed and is carried out oxidative purification method under the conditions of 100-250 DEG C with potassium permanganate+concentrated sulfuric acid, the method for
The removal effect of graphite state carbon is not fairly obvious, while containing heavy metal manganese in waste water, and environmental problem is more.
CN106587046B is disclosed in sulfuric acid medium, removes graphitic carbon with 75-90 DEG C of nitrate, potassium permanganate, hydrogen peroxide processing
Method, test proves that the method is extremely limited to the removal effect of graphitic carbon.CN1400162A is disclosed with the concentrated sulfuric acid+dense nitre
Graphitic carbon is removed under sour fluidized state, the method is poor for the removal effect of graphite state carbon, and technique is for equipment and pipeline etc.
Material is more demanding, otherwise easily causes heavy corrosion.Document " functional material " (2000,31 (1): 56-57) reports utilization
HClO4, H2SO4+K2Cr2O7、H2SO4+KMnO4Three kinds of oxidation treatment methods remove graphitic carbons, although conclusion be three kinds can be effective
Remove graphite state carbon, but perchloric acid boiling process higher cost, H2SO4+K2Cr2O7And H2SO4+KMnO4Two method effects need further
Verifying.Document " New Technologies " (2006 (1): 110-112) and " Northcentral University's journal " (2006,27 (1): 55-58) report
Road air vapour phase oxidation process removes graphitic carbon, and the method operability is poor, while effect is very unsatisfactory.Therefore, it is necessary to right
It is further improved in the minimizing technology of graphitic carbon.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of graphite state carbon in efficiently removal Nano diamond detonation ash material.It should
Method has many advantages, such as that simple production process, production security height, low raw-material cost, product purity are high, and production technology ring
It protects, without toxic gas and heavy metals emission.
Realizing the object of the invention technical solution is: the minimizing technology of graphite state carbon in nano diamond ash material will be received
Rice diamond detonation ash is added into low melting point alkaline medium, is warming up to 400~500 DEG C, nitrite is added, 400~600
It under the conditions of DEG C, reacts 0.5~5 hour, after reaction solution is cooling, is dissolved in water and isolates diamond dust, filtering, washing, drying,
Obtain purified nanotubes diamond product.
Further, low melting point alkaline medium is sodium hydroxide or potassium hydroxide.
Further, the dosage of low melting point alkaline medium is 2-10 times, preferably 4-8 times of diamond detonation ash quality.
Further, nitrite is sodium nitrite or potassium nitrite, and dosage is the 2- of diamond detonation ash quality
10 times, preferably 4-6 times.
Compared with prior art, the present invention its remarkable advantage is: (1) technique has simple production process, equipment requirement
Lower, the advantages that product purity is high, production technology safety and environmental protection.(2) for metal oxide in ash material and salt, silica
In the lesser situation of content, high purity product directly can not be provided after further treatment.(3) receiving using the production of this technique
Rice diamond be fully able to meet especially Ultraprecise polished related field, advanced adjustment (lubrication) oil, wear-resistant material additive,
The application in the fields such as wearing face Composite Coatings.
Detailed description of the invention
Fig. 1 is the XRD spectra of one product of the embodiment of the present invention and pure graphite powder.
Specific embodiment
The following examples are not intended to limit the scope of the invention to further explanation of the invention.
The present invention using nitrite as oxidant, since nitrite is during heat resolve, 400 DEG C with
Previous step is decomposed, and is avoided two step of nitrate decomposition bring and is difficult to the defect controlled, production technology more safe and feasible.
It is handled in low melting point alkaline medium (sodium hydroxide or potassium hydroxide) using nitrite-oxidizing.Graphitic carbon and Asia
Nitrate reaction forms carbon dioxide, and carbon dioxide is further reacted with alkaline medium, generates carbonate.With alkaline medium hydrogen-oxygen
Change sodium for, it is as follows with the reaction equation of nitrate at high temperature:
3C+4NaNO2+2NaOH→3Na2CO3+2N2↑+H2O↑
3C+4KNO2+2KOH→3K2CO3+2N2↑+H2O↑
It can thus be seen that final product is sodium carbonate+sodium hydroxide under the conditions of selecting with metal medium and oxidant
Or potassium carbonate+potassium hydroxide, remaining is nitrogen and steam.Sodium hydroxide or potassium hydroxide obtain after carbon dioxide treatment
Corresponding carbonate, carbonate can be used as byproduct recycling, and it is a kind of life of green that entire production technology, which does not generate polluter,
Production. art.
Embodiment one:
In 100L stainless steel cauldron, 20kg sodium hydroxide and 4kg detonation ash is added, is warming up to 450 DEG C, 24kg is added
Sodium nitrite, reaction temperature control 450 DEG C~550 DEG C, the reaction time 8 hours.After cooling, enough dissolved hydrogen water sodium oxide molybdenas are added
And sodium carbonate.Filtering, and sufficiently washed to filter liquor and be in neutrality with deionized water.Filtering, drying, obtain canescence product
1.45kg, yield 36.3%.
The XRD spectra of product is shown in Fig. 1, and as seen from Figure 1, the principal character peak of graphite is at 28 °, and product is in 28 ° of nothings
Peak occurs, and shows that graphitic carbon has completely removed in diamond detonation ash.
Embodiment two~six:
Two~embodiment of embodiment, six operating procedure is basically the same as the first embodiment.The difference is that detonation ash adds
Amount, the type of alkaline medium and dosage, the type of nitrite and dosage, reaction control temperature and reaction time.Primary condition
With the results are shown in Table 1.
1 embodiment primary condition of table and result
aGraphite carbon removal situation in XRD the case where 28 ° or so peaks according to judging.
Claims (7)
1. the minimizing technology of graphite state carbon in nano diamond ash material, which is characterized in that by Nano diamond detonation ash be added to
In low melting point alkaline medium, it is warming up to 400 ~ 500oNitrite is added in C, and under the conditions of 400 ~ 600 DEG C, reaction 0.5 ~ 5 is small
When, it after reaction solution is cooling, is dissolved in water and isolates diamond dust, filtering, washing, drying obtain purified nanotubes diamond product.
2. the method as described in claim 1, which is characterized in that low melting point alkaline medium is sodium hydroxide or potassium hydroxide.
3. method according to claim 1 or 2, which is characterized in that the dosage of low melting point alkaline medium is diamond detonation ash
2-10 times of quality.
4. method according to claim 1 or 2, which is characterized in that the dosage of low melting point alkaline medium is diamond detonation ash
4-8 times of quality.
5. the method as described in claim 1, which is characterized in that nitrite is sodium nitrite or potassium nitrite.
6. method as claimed in claim 1 or 5, which is characterized in that nitrite dosage is the 2- of diamond detonation ash quality
10 times.
7. method as claimed in claim 1 or 5, which is characterized in that nitrite dosage is the 4-6 of diamond detonation ash quality
Times.
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| CN201811416838.3A CN109305676B (en) | 2018-11-26 | 2018-11-26 | Simple and efficient method for removing graphite carbon in nano diamond ash |
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| CN201811416838.3A CN109305676B (en) | 2018-11-26 | 2018-11-26 | Simple and efficient method for removing graphite carbon in nano diamond ash |
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| CN109305676B CN109305676B (en) | 2021-08-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479202A (en) * | 2020-11-30 | 2021-03-12 | 上海征世科技有限公司 | Artificial diamond purification process |
| CN112479201A (en) * | 2020-11-30 | 2021-03-12 | 上海征世科技有限公司 | Artificial diamond purification method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033065A (en) * | 2007-04-13 | 2007-09-12 | 中国地质大学（武汉） | Method of purifying environment-friendly type ultra-fine diamond |
| WO2008123801A1 (en) * | 2007-04-10 | 2008-10-16 | 'new Diamonds Of Siberia, Ltd.' | Diamond cleaning method |
| CN102616777A (en) * | 2012-04-09 | 2012-08-01 | 江苏金海丰硬质材料科技有限公司 | Method for removing graphite carbon in nanometer diamond ash prepared by detonation technique |
| CN104495836A (en) * | 2014-11-26 | 2015-04-08 | 河南晶锐超硬材料有限公司 | Method for processing diamond micropowder |
| 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 |
-
2018
- 2018-11-26 CN CN201811416838.3A patent/CN109305676B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008123801A1 (en) * | 2007-04-10 | 2008-10-16 | 'new Diamonds Of Siberia, Ltd.' | Diamond cleaning method |
| CN101033065A (en) * | 2007-04-13 | 2007-09-12 | 中国地质大学（武汉） | Method of purifying environment-friendly type ultra-fine diamond |
| CN102616777A (en) * | 2012-04-09 | 2012-08-01 | 江苏金海丰硬质材料科技有限公司 | Method for removing graphite carbon in nanometer diamond ash prepared by detonation technique |
| CN104495836A (en) * | 2014-11-26 | 2015-04-08 | 河南晶锐超硬材料有限公司 | Method for processing diamond micropowder |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112479202A (en) * | 2020-11-30 | 2021-03-12 | 上海征世科技有限公司 | Artificial diamond purification process |
| CN112479201A (en) * | 2020-11-30 | 2021-03-12 | 上海征世科技有限公司 | Artificial diamond purification method |
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| CN109305676B (en) | 2021-08-03 |
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