CN105565291A - Oxidation method for purification process of three-dimensional graphene coated single-particle nano-diamond material - Google Patents
Oxidation method for purification process of three-dimensional graphene coated single-particle nano-diamond material Download PDFInfo
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- CN105565291A CN105565291A CN201410539296.4A CN201410539296A CN105565291A CN 105565291 A CN105565291 A CN 105565291A CN 201410539296 A CN201410539296 A CN 201410539296A CN 105565291 A CN105565291 A CN 105565291A
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Abstract
The invention provides an oxidation method for the purification process of a three-dimensional graphene coated single-particle nano-diamond material. The method is applied to a purification process consisting of magnetic separation, acidification, oxidation, alkalization and heavy liquid separation. In an oxidation process, an oxidizing solution with small oxidizability is employed for oxidation treatment, after oxidation, the oxidized mixed solution is filtered and cleaned by adopting filtration equipment and combining purified water so as to remove amorphous carbon from the mixture, thus providing favorable conditions for subsequent further purification. As the adopted oxidizing solution has small oxidizability, the oxidation method provided by the invention can reduce corrosion damage to oxidation equipment, prolong the service life and save the cost, also effectively removes amorphous carbon from the mixture, and improves the purification rate.
Description
Technical field
The present invention relates to chemical technique technical field, be specifically related to the method for oxidation in the purge process of a kind of three-dimensional grapheme coated single-particle Nano diamond material.
Background technology
Graphene is by individual layer SP
2the cellular two-dirnentional structure of hexagonal lattice of hydbridized carbon atoms composition, its Stability Analysis of Structures, has excellent conductive and heat-conductive characteristic, good mechanical characteristics, thus obtains and study widely.Graphene has been produced out and has been applied in the fields such as energy storage, transparency electrode, thermo-mechanical drive.In order to the potential application of Graphene can be developed further, especially at stored energy conversion aspect, except two-dimensional graphene film, three-dimensional grapheme structure also can prepare, and, three-dimensional grapheme is oxide coated in recent years, the materials such as carbon material start extensively to be studied, such as, the coated single-particle Nano diamond of three-dimensional grapheme, coated due to three-dimensional grapheme, significantly improve the electric conductivity of the Nano diamond material be wrapped by, and combine the good characteristic of Graphene, these mixtures conductivity can significantly increase, in catalysis, electrical condenser, also excellent performance is shown with energy storage aspect, one of the international forward position and focus of physics and semiconductor electronic research field are become.
Usually, the preparation of three-dimensional grapheme coated single-particle Nano diamond material adopts the methods such as dilatometry, after this material of preparation, other impurity is also had in obtained mixing solutions, such as, unsetting carbon, kish impurity or metal ion, sila matter etc., therefore, need to carry out purification process to the mixing solutions of this material, coated for three-dimensional grapheme single-particle Nano diamond is extracted.
Under the purification process of existing three-dimensional grapheme coated single-particle Nano diamond material comprises high-temperature and high-pressure conditions, adopt strong acid and highly basic interrupted oscillation purifying, such as, the mixing solutions of employing nitric acid or sulfuric acid and hydrogen peroxide or chloroazotic acid etc., by separation of repeatedly vibrating, the object filtering to reach purifying.
But employing strong acid, the equipment of highly basic to purifying have strong corrodibility, can shorten the work-ing life of equipment, increase production cost; Further, it is not high that aforesaid method obtains purifying rate, even needs a large amount of filtrations repeatedly, add the production time, thus reduce production efficiency, further increase production cost.
Summary of the invention
In order to overcome above problem, the present invention aims to provide the method for oxidation in the purge process of the coated single-particle Nano diamond of a kind of three-dimensional grapheme, has reached the object improving purifying rate and reduce the corrosion of equipment.
To achieve these goals, technical scheme of the present invention is as follows:
The invention provides the method for oxidation in the purge process of a kind of three-dimensional grapheme coated single-particle Nano diamond material, carry out in purge process to the mixture containing the coated single-particle Nano diamond of three-dimensional grapheme, it is characterized in that, described purge process comprises carries out Magneto separate, acidifying, oxidation, alkalization and heavy-fluid sepn process to described mixture; The method for oxidation of described oxidising process adopts oxidation furnaces and filter plant, and it comprises:
Step 01: the oxidizing solution described mixture after described acidization being placed in oxidation furnaces;
Step 02: at normal temperatures and pressures, carries out oxide treatment to described mixture;
Step 03: after certain oxidization time, is placed in filter plant by the mixing solutions through oxide treatment;
Step 04: adopt pure water and filter plant to carry out filtration cleaning to described mixing solutions, thus by the indefinite form carbon removal in described mixture.
Preferably, described oxidizing solution comprises: potassium permanganate and the concentration hydrogen peroxide that is less than 40% that sulfuric acid, concentration that concentration is less than 30% are less than 30%.
Preferably, described oxidization time is 1-5 hour.
Preferably, the pore size filter of described filter plant is 10-200 nanometer.
Preferably, described pure electrical conductivity of water is less than 5 μ s/cm.
Preferably, in described step 04, described filtration cleaning process comprises: in described filter plant, add pure water repeatedly filter cleaning to mixing solutions, until namely the pH value of described mixing solutions completes between 3-9 filter cleaning.
Method for oxidation in the purge process of three-dimensional grapheme of the present invention coated single-particle Nano diamond material, be applied in mixture experience Magneto separate, acidifying, oxidation, alkalization and heavy-fluid sepn process, in oxidising process, the less oxidizing solution of oxidisability is adopted to carry out oxide treatment, adopt filter plant after oxidation and in conjunction with pure water, cleaning filtered to the mixing solutions of oxidation, thus the indefinite form carbon can removed in mixture, for follow-up being further purified provides favourable condition; Method for oxidation of the present invention, because the oxidisability of the oxidizing solution adopted is less, can reduces the corrosion damage to oxidation furnaces, extend its work-ing life, save cost; Further, effectively removes the indefinite form carbon in mixture, improve purifying rate.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for oxidation in the purge process of the three-dimensional grapheme coated single-particle Nano diamond material of a preferred embodiment of the present invention
Fig. 2 is the relation of equipment of the method for oxidation of a preferred embodiment of the present invention
Embodiment
For making content of the present invention clearly understandable, below in conjunction with Figure of description, content of the present invention is described further.Certain the present invention is not limited to this specific embodiment, and the general replacement known by those skilled in the art is also encompassed in protection scope of the present invention.
As previously mentioned, existing purification process, need under high-temperature and high-pressure conditions, adopt strong acid and strong base to carry out intermittence vibration to be separated, not only severe corrosion equipment shortens equipment life, increase the process time and increase process costs, and purification effect is also undesirable, often need repeatedly to be separated in large quantities, further increase production cost; The present invention proposes the method for oxidation in the purge process of a kind of three-dimensional grapheme coated single-particle Nano diamond material for this reason, be applied in the purifying comprising experience Magneto separate, acidifying, oxidation, alkalization and heavy-fluid sepn process, its oxidising process, the less oxidizing solution of oxidisability is adopted to carry out oxide treatment, adopt filter plant after oxide treatment and in conjunction with pure water, cleaning filtered to the mixing solutions of oxidation, thus the indefinite form carbon can removed in mixture, for follow-up being further purified provides favourable condition.
In the present invention, being prepared process to three-dimensional grapheme coated single-particle Nano diamond material can specifically comprise:
Step L1: component design; Formula comprises the proportioning of various raw material, and in the present embodiment, filling a prescription is made up of following raw material: trotyl; Hexogen/octogen; Metal.The proportioning of each raw material can need to set according to actual process.Such as, weight percent is the trotyl of 20; Weight percent is the hexogen of 60%, and the metal of 20%.
Step L2: prepare energetic material according to formula;
Concrete, each raw material in formula can be mixed, then compression moulding, is energetic material.Here it should be noted that, energetic material can comprise explosive, priming charge, priming explosive etc.
Step L3: energetic material is loaded in reaction chamber;
Concrete, energetic material can immerse containing in water receptacle, then will be hung in energetic material reactor containing water receptacle;
Step L4: trigger energetic material synthesis three-dimensional grapheme coated single-particle Nano diamond material;
Concrete, the method triggering energetic material has a variety of, and such as detonator triggers.By the high-energy that energetic material produces, uncombined carbon is reacted and forms three-dimensional grapheme coated single-particle Nano diamond material; Meanwhile, inevitably produce the impurity such as unsetting carbon, silicon, metallics, make product be the mixture including three-dimensional grapheme coated single-particle Nano diamond material; Need to carry out purifying to this mixture, to obtain the higher three-dimensional grapheme of purity coated single-particle Nano diamond material.
It should be noted that, the coated single-particle of the three-dimensional grapheme in the present invention Nano diamond material can also adopt existing method, and this can know for those skilled in the art, and the present invention repeats no more this.
The mixture of the present invention to the coated single-particle Nano diamond of the three-dimensional grapheme prepared carries out purifying, and purge process comprises carries out in Magneto separate, acidifying, oxidation, alkalization and heavy-fluid sepn process; Concrete, can comprise and carry out Magneto separate, acidifying, oxidation, alkalization and heavy-fluid sepn process successively, also can comprise and carry out Magneto separate, acidifying, oxidation, alkalization, again acidifying and heavy-fluid sepn process successively; Here acidization can be an acidification process, and may also be repeatedly acidification process, the present invention can be applied in the purge process comprising repeatedly acidification process.
Oxidation furnaces and filter plant is adopted in the method for oxidation of its oxidising process; Method for oxidation comprises:
Step 01: the oxidizing solution mixture after acidization being placed in oxidation furnaces;
Step 02: at normal temperatures and pressures, carries out oxide treatment to mixture;
Step 03: after certain oxidization time, is placed in filter plant by the mixing solutions through oxide treatment;
Step 04: adopt pure water and filter plant to carry out filtration cleaning to mixing solutions, thus by the unsetting carbon removal in mixture.
It should be noted that, oxidising process here can be once oxidation process, may also be repeatedly oxide treatment, and method for oxidation of the present invention can be applied in each oxide treatment.
Below with reference to accompanying drawing 1-2 and specific embodiment, the method for oxidation in purifying three-dimensional grapheme of the present invention coated single-particle Nano diamond process is described in further detail.Wherein, Fig. 1 is the schematic flow sheet of the method for oxidation in the purifying three-dimensional grapheme coated single-particle Nano diamond process of a preferred embodiment of the present invention; Fig. 2 is the relation of equipment of the method for oxidation of a preferred embodiment of the present invention.It should be noted that, accompanying drawing all adopt simplify very much form, use non-ratio accurately, and only in order to object that is convenient, that clearly reach aid illustration the present embodiment.
Purge process in the present embodiment comprises:
Magneto separate process, acidifying, oxidation, alkalization and heavy-fluid sepn process are carried out successively to mixture;
Wherein, Magneto separate process can adopt magnetic separator a and automatic control device, and Magneto separate process tentatively can remove the bulk metal impurity in mixture; Acidization can be carried out at normal temperatures and pressures, mixture is placed in acidic solution, and the acid reactant of employing can be weak acid, also can be the strong acid of dilution, such as, sulfurous acid, carbonic acid, hypochlorous acid, the weak acid such as hydrosulphuric acid, or the hydrochloric acid etc. of dilution, this is because the corrodibility of the strong acid of dilution reduces relatively, reduce the corrosion damage to acid equipment to greatest extent; Metallics Impurity removal in mixture can be comprised removal micro-metals by this acidization, such as, and Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu or Zn etc.; Alkalinization can carry out under normal temperature and pressure conditions, and mixture is placed in basic solution, adopt alkaline reactant can for dilution strong base solution, also can be weak caustic solution, such as, NH
3h
2o etc., or the sodium hydroxide of dilution; This alkalinization can by the silicon Impurity removal in mixture.Heavy-fluid sepn process can be centrifugal process, carries out under normal temperature and pressure conditions, adopts high rotating speed centrifugation apparatus, such as, and self-discharging type high speed centrifuge.Rotating speed can be 10000-30000 rev/min, and the time can be 30-300 second, thus is extracted by mixture.Heavy-fluid sepn process can remove the moisture in mixture, reaches the withering object of mixture.
This purge process can also comprise acidization again, then acidization be in order to remove further residual trace metal ion in the mixture comprise the oxidising process of front and continued the K ion, Mn ion etc. that remain.At normal temperatures and pressures, can adopt the strong acid solution of weakly acid soln or dilution, carry out in acidification reaction chamber, the weakly acid soln adopted can be sulfurous acid, carbonic acid, hypochlorous acid, hydrosulphuric acid etc., or the hydrochloric acid of dilution.Such as, the dilute hydrochloric acid that concentration is less than 15%, under normal temperature and pressure conditions, then acidificatoin time is 1-5 hour; And then filter.
In the purge process of the present embodiment, refer to Fig. 1 and 2, the method for oxidation in the present embodiment have employed oxidation furnaces and filter plant, and this method for oxidation specifically comprises:
Step 01: the oxidizing solution mixture after acidization being placed in oxidation furnaces a;
Concrete, mixture is placed in oxidizing solution, and can adopt weakly acid soln, such as oxidizing solution comprises: potassium permanganate and the concentration hydrogen peroxide that is less than 40% that sulfuric acid, concentration that concentration is less than 30% are less than 30%.
As shown in Figure 2, in the present embodiment, there are in oxidation reaction apparatus two oxidizing reaction chamber a, then in the present invention the quantity of oxidizing reaction chamber a is not restricted.
Step 02: at normal temperatures and pressures, carries out oxide treatment to mixture;
Concrete, at normal temperatures and pressures, as shown in Figure 2, oxide treatment is carried out in the oxidizing reaction chamber of oxidation furnaces a here, and here, oxidation furnaces can be acid-resistant reacting kettle, coordinates conductivity meter to use together.
Step 03: after certain oxidization time, is placed in filter plant by the mixing solutions through oxide treatment;
Concrete, the oxidization time in the present embodiment can be 1-5 hour.
Step 04: adopt pure water and filter plant b to carry out filtration cleaning to mixing solutions, thus by the indefinite form carbon removal in mixture.
Concrete, filter plant b can be ceramic membrane, thus ceramic membrane and pure water can be adopted to carry out filtration cleaning to mixing solutions, thus removes indefinite form carbon.Here, the aperture of the filter pore of ceramic membrane b can be 10-200 nanometer, and pure electrical conductivity of water can be less than 5 μ s, and the pH value of the mixing solutions washed is between 3-9; Self-con-tained unit can be adopted to control this process, and the present invention is not restricted this.
In the present embodiment, this filtration cleaning process comprises: in filter plant, add pure water repeatedly filter cleaning to mixing solutions, until namely the pH value of mixing solutions completes between 3-9 filter cleaning.
This oxidising process can by the indefinite form carbon removal in mixture; This is in the process owing to preparing the coated single-particle Nano diamond of three-dimensional grapheme, can form some unsetting carbon, need to be removed; Adopt oxidizing solution, unsetting carbon can be oxidized, generate CO
2gas and discharging from mixing solutions, thus be separated with in the solid-state coated single-particle Nano diamond of three-dimensional grapheme.
Filtering again, can separate comprising single-particle Nano diamond in solid-state three-dimensional grapheme coated single-particle Nano diamond material and some solid matters.Finally by follow-up alkalization, heavy-fluid is separated or the impurity such as silicon, metal ion excludes by alkalization, again acidifying and heavy-fluid sepn process, finally obtains the higher three-dimensional grapheme of purity coated single-particle Nano diamond material.
In sum, by method for oxidation of the present invention, owing to adopting the oxidizing solution that oxidisability is less, the corrosion damage to oxidation furnaces can be reduced, extend its work-ing life, save cost; Further, effectively removes the indefinite form carbon in the mixture after oxidising process, improve purifying rate.
Although the present invention discloses as above with preferred embodiment; right described embodiment is citing for convenience of explanation only; and be not used to limit the present invention; those skilled in the art can do some changes and retouching without departing from the spirit and scope of the present invention, and the protection domain that the present invention advocates should be as the criterion with described in claims.
Claims (6)
1. the method for oxidation in the purge process of the coated single-particle Nano diamond of three-dimensional grapheme, purifying is carried out to the mixture containing the coated single-particle Nano diamond of three-dimensional grapheme, it is characterized in that, described purge process comprises carries out Magneto separate, acidifying, oxidation, alkalization and heavy-fluid sepn process to described mixture; The method for oxidation of described oxidising process adopts oxidation furnaces and filter plant, and it comprises:
Step 01: the oxidizing solution described mixture after described acidization being placed in oxidation furnaces;
Step 02: at normal temperatures and pressures, carries out oxide treatment to described mixture;
Step 03: after certain oxidization time, is placed in filter plant by the mixing solutions through oxide treatment;
Step 04: adopt pure water and filter plant to carry out filtration cleaning to described mixing solutions, thus by the indefinite form carbon removal in described mixture.
2. method for oxidation according to claim 1, is characterized in that, described oxidizing solution comprises: potassium permanganate and the concentration hydrogen peroxide that is less than 40% that sulfuric acid, concentration that concentration is less than 30% are less than 30%.
3. method for oxidation according to claim 1, is characterized in that, described acidificatoin time is 1-5 hour.
4. method for oxidation according to claim 1, is characterized in that, the pore size filter of described filter plant is 10-200 nanometer.
5. method for oxidation according to claim 1, is characterized in that, described pure electrical conductivity of water is less than 5 μ s/cm.
6. method for oxidation according to claim 1, it is characterized in that, in described step 04, described filtration cleaning process comprises: in described filter plant, add pure water repeatedly filter cleaning to mixing solutions, until namely the pH value of described mixing solutions completes between 3-9 filter cleaning.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385366A (en) * | 2001-05-10 | 2002-12-18 | 浣石 | Method for purifying nano diamond |
| CN102616776A (en) * | 2012-04-09 | 2012-08-01 | 江苏金海丰硬质材料科技有限公司 | Purification method of nano diamond ash material |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385366A (en) * | 2001-05-10 | 2002-12-18 | 浣石 | Method for purifying nano diamond |
| CN102616776A (en) * | 2012-04-09 | 2012-08-01 | 江苏金海丰硬质材料科技有限公司 | Purification method of nano diamond ash material |
Non-Patent Citations (2)
| Title |
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| 李和胜 等: ""针对铁基触媒的金刚石提纯工艺研究"", 《金刚石与磨料磨具工程》 * |
| 樊亮 等: ""人造金刚石微粉提纯工艺技术研究"", 《非金属矿》 * |
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