CN105565291B - Method for oxidation in the purge process of three-dimensional grapheme cladding single-particle Nano diamond material - Google Patents
Method for oxidation in the purge process of three-dimensional grapheme cladding single-particle Nano diamond material Download PDFInfo
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Abstract
The present invention provides the method for oxidation in a kind of purge process of three-dimensional grapheme cladding single-particle Nano diamond material, apply in experience Magneto separate, acidifying, oxidation, alkalization and the purge process of heavy-fluid separation process, in oxidizing process, oxidation processes are carried out using the less oxidizing solution of oxidisability, cleaning is filtered to the mixed solution of oxidation using filter plant and combination pure water after oxidation, so as to remove the indefinite form carbon in mixture, advantage is provided for follow-up being further purified；The method for oxidation of the present invention, since the oxidisability of the oxidizing solution of use is smaller, can reduce the corrosion damage to oxidation furnaces, extend its service life, saved cost；Also, the indefinite form carbon in mixture is effectively removes, improves purifying rate.
Description
Technical field
The present invention relates to chemical process technical field, and in particular to a kind of three-dimensional grapheme coats single-particle Nano diamond
Method for oxidation in the purge process of material.
Background technology
Graphene is by individual layer SP2The cellular two-dimensional structure of hexagonal lattice of hydbridized carbon atoms composition, its stable structure, tool
There are excellent conductive and heat-conductive characteristic, good mechanical property, thus obtained extensive research.Graphene has been prepared out
And apply in fields such as energy storage, transparency electrode, thermo-mechanical drives.Should in order to further develop the potential of graphene
With especially in energy stores conversion aspect, in addition to two-dimensional graphene film, three-dimensional grapheme structure also has been able to prepare
Come, also, the material such as oxide coated, carbon material of three-dimensional grapheme starts to be widely studied in recent years, for example, three-dimensional graphite
Alkene coats single-particle Nano diamond, due to the cladding of three-dimensional grapheme, significantly improves the Nano diamond material being wrapped by
Conductivity, and combine the good characteristic of graphene, the electric conductivity of these compounds can dramatically increase, catalysis,
Excellent performance is also shown in terms of capacitor and energy storage, it has also become the international forward position of physics and semiconductor electronic research field
One of with hot spot.
In general, the methods of preparation of three-dimensional grapheme cladding single-particle Nano diamond material uses dilatometry, is making
After the standby material, also have other impurity in obtained mixed solution, for example, unsetting carbon, kish impurity or gold
Belong to ion, silicon impurities etc., therefore, it is necessary to carry out purification process to the mixed solution of the material, three-dimensional grapheme is coated into simple grain
Sub- Nano diamond extracts.
The purification process of existing three-dimensional grapheme cladding single-particle Nano diamond material includes high-temperature and high-pressure conditions
Under, purified using strong acid and highly basic intermittent oscillation, for example, mixed solution or chloroazotic acid using nitric acid or sulfuric acid and hydrogen peroxide etc.,
By vibrating separation repeatedly, filtering to achieve the purpose that purifying.
However, there is strong corrosivity to the equipment of purifying using strong acid, highly basic, the service life of equipment can be shortened,
Increase production cost；Also, it is not high that the above method obtains purifying rate, or even substantial amounts of repeated filtration is needed, add production
Time, so as to reduce production efficiency, further increases production cost.
The content of the invention
In order to overcome problem above, the present invention is intended to provide a kind of three-dimensional grapheme cladding single-particle Nano diamond is pure
Method for oxidation during change, has achieveed the purpose that to improve purifying rate and has reduced the corrosion to equipment.
To achieve these goals, technical scheme is as follows：
The present invention provides the oxidation in a kind of purge process of three-dimensional grapheme cladding single-particle Nano diamond material
Method, carries out in purge process the mixture containing three-dimensional grapheme cladding single-particle Nano diamond, it is characterised in that institute
Stating purge process includes carrying out Magneto separate, acidifying, oxidation, alkalization and heavy-fluid separation process to the mixture；It is described to aoxidize
The method for oxidation of journey uses oxidation furnaces and filter plant, it includes：
Step 01：The mixture after the acidization is placed in the oxidizing solution of oxidation furnaces；
Step 02：At normal temperatures and pressures, oxidation processes are carried out to the mixture；
Step 03：After certain oxidization time, oxidation-treated mixed solution is placed in filter plant；
Step 04：Filtering cleaning is carried out to the mixed solution using pure water and filter plant, so that by the mixing
Indefinite form carbon removal in thing.
Preferably, the oxidizing solution includes：Sulfuric acid of the concentration less than 30%, concentration are less than 30% permanganic acid
Potassium and concentration are less than 40% hydrogen peroxide.
Preferably, when the oxidization time is 1-5 small.
Preferably, the pore size filter of the filter plant is 10-200 nanometers.
Preferably, the electrical conductivity of the pure water is less than 5 μ s/cm.
Preferably, in the step 04, the filtering cleaning process includes：Pure water pair is added into the filter plant
Mixed solution carries out repeated filtration cleaning, until the pH value of the mixed solution completes filtering cleaning between 3-9.
Method for oxidation in the purge process of the three-dimensional grapheme cladding single-particle Nano diamond material of the present invention, application
It is smaller using oxidisability in oxidizing process in mixture undergoes Magneto separate, acidifying, oxidation, alkalization and heavy-fluid separation process
Oxidizing solution carry out oxidation processes, using filter plant and combine mixed solution of the pure water to oxidation after oxidation
Filtering cleaning, so as to remove the indefinite form carbon in mixture, advantage is provided for follow-up being further purified；This hair
Bright method for oxidation, since the oxidisability of the oxidizing solution of use is smaller, can reduce the corrosion damage to oxidation furnaces, prolong
Its long service life, has saved cost；Also, the indefinite form carbon in mixture is effectively removes, improves purifying rate.
Brief description of the drawings
Fig. 1 is that the three-dimensional grapheme of the preferred embodiment of the present invention coats the purifying of single-particle Nano diamond material
During method for oxidation flow diagram
Fig. 2 is the relation of equipment of the method for oxidation of the preferred embodiment of the present invention
Embodiment
To make present disclosure more clear understandable, below in conjunction with Figure of description, present disclosure is made into one
Walk explanation.Certainly the invention is not limited to the specific embodiment, the general replacement known to those skilled in the art
Cover within the scope of the present invention.
As it was previously stated, existing purification process carries out intermittence using strong acid and strong base and shakes, it is necessary under high-temperature and high-pressure conditions
Separation is swung, not only severe corrosion equipment shortens equipment life, increase process time and increase process costs, and purification effect
It is undesirable, generally require to separate repeatedly in large quantities, further increase production cost；The present invention proposes a kind of three-dimensional stone for this
Method for oxidation in the purge process of black alkene cladding single-particle Nano diamond material, applied to including experience Magneto separate, acidifying,
In the purifying of oxidation, alkalization and heavy-fluid separation process, its oxidizing process, oxygen is carried out using the less oxidizing solution of oxidisability
Change is handled, and cleaning is filtered to the mixed solution of oxidation using filter plant and combination pure water after oxidation processes, so as to
The indefinite form carbon in mixture is removed, advantage is provided for follow-up being further purified.
In the present invention, carrying out preparation process to three-dimensional grapheme cladding single-particle Nano diamond material can specifically wrap
Include：
Step L1：Component design；Being formulated includes the proportioning of various raw materials, in the present embodiment, is formulated and is made of the following raw material：
Trinitrotoluene；Hexogen/octogen；Metal.The proportioning of each raw material can be set according to actual process needs.For example,
Percentage by weight is 20 trinitrotoluene；Percentage by weight is 60% hexogen, and 20% metal.
Step L2：Energetic material is prepared according to formula；
Specifically, each raw material in formula can be uniformly mixed, type is then pressed into, is energetic material.Here need
It is noted that energetic material can include explosive, ignition charge, priming etc..
Step L3：Energetic material is fitted into reaction chamber；
It is hung in specifically, energetic material can be immersed in energetic material reactor containing water container in water container, then will be contained；
Step L4：Trigger energetic material synthesis three-dimensional grapheme cladding single-particle Nano diamond material；
Specifically, the method for triggering energetic material has many kinds, such as detonator triggering.The high energy produced by energetic material
Amount, makes free carbon react to form three-dimensional grapheme cladding single-particle Nano diamond material；Meanwhile inevitably result from not
Shape the impurity such as carbon, silicon, metallic so that product is to include three-dimensional grapheme cladding single-particle Nano diamond material
Mixture；Need to purify the mixture, single-particle Nano diamond is coated to obtain the higher three-dimensional grapheme of purity
Material.
It should be noted that the present invention in three-dimensional grapheme cladding single-particle Nano diamond material can also use it is existing
Method, this could be aware that for those skilled in the art, the present invention this is repeated no more.
The mixture of three-dimensional grapheme cladding single-particle Nano diamond of the present invention to preparing purifies, and purifies
Journey includes carrying out in Magneto separate, acidifying, oxidation, alkalization and heavy-fluid separation process；Specifically, it can include carrying out magnetic point successively
From, acidifying, oxidation, alkalization and heavy-fluid separation process, it can also include carrying out Magneto separate, acidifying, oxidation, alkalization, sour again successively
Change and heavy-fluid separation process；Here acidization can be an acidification process or multiple acidification process,
Present invention could apply in the purge process including multiple acidification process.
Oxidation furnaces and filter plant are used in the method for oxidation of its oxidizing process；Method for oxidation includes：
Step 01：Mixture after acidified process is placed in the oxidizing solution of oxidation furnaces；
Step 02：At normal temperatures and pressures, oxidation processes are carried out to mixture；
Step 03：After certain oxidization time, oxidation-treated mixed solution is placed in filter plant；
Step 04：Filtering cleaning is carried out to mixed solution using pure water and filter plant, thus by mixture not
Shape carbon removal.
It should be noted that oxidizing process here can be once oxidation processing or multiple oxidation processes, this hair
Bright method for oxidation can be applied in each oxidation processes.
Single-particle nanogold is coated to the purifying three-dimensional grapheme of the present invention below with reference to attached drawing 1-2 and specific embodiment
Method for oxidation during hard rock is described in further detail.Wherein, Fig. 1 is the purifying three of the preferred embodiment of the present invention
The flow diagram of method for oxidation during dimension graphene coated single-particle Nano diamond；Fig. 2 be the present invention one compared with
The relation of equipment of the method for oxidation of good embodiment.It should be noted that attached drawing is using very simplified form, using non-accurate
Ratio, and only to it is convenient, clearly achieve the purpose that to aid in illustrating the present embodiment.
Purge process in the present embodiment includes：
Carry out Magneto separate process, acidifying, oxidation, alkalization and heavy-fluid separation process successively to mixture；
Wherein, Magneto separate process can use magnetic separator a and automaton, and Magneto separate process can be preliminary
Remove the bulk metal impurity in mixture；Acidization can carry out at normal temperatures and pressures, and mixture is placed in acid solution
In, the acid reactant used can be weak acid, or diluted strong acid, such as, sulfurous acid, carbonic acid, hypochlorous acid, hydrogen sulphur
The weak acid such as acid, or diluted hydrochloric acid etc., this is because the corrosivity of diluted strong acid is relatively reduced, reduce to acid to greatest extent
The corrosion damage of property equipment；The acidization, which can remove the metallic impurity in mixture, to be included removing trace meter member
Element, for example, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu or Zn etc.；Alkalinization can carry out under normal temperature and pressure conditions, will be mixed
Compound is placed in alkaline solution, and it can be diluted strong base solution to use alkaline reactant, or weak caustic solution, example
Such as, NH3·H2O etc., or diluted sodium hydroxide；The alkalinization can remove the silicon impurities in mixture.Heavy-fluid separated
Journey can be centrifugal process, be carried out under normal temperature and pressure conditions, using high rotating speed centrifugation apparatus, such as, the high rotating speed of self-tipping type from
Scheming.Rotating speed can be 10000-30000 revs/min, and the time can be 30-300 seconds, so that mixture be extracted.Weight
Liquid separation process can remove the moisture in mixture, reach to the withering purpose of mixture.
The purge process can also include acidization, then acidization is to remain in mixture to further remove again
In the remaining K ions of oxidizing process institute of trace metal ion including front and continued, Mn ions etc..It can adopt at normal temperatures and pressures
With weak acid solution or diluted strong acid solution, carried out in acidification reaction chamber, used weak acid solution can be sulfurous acid, carbon
Acid, hypochlorous acid, hydrosulphuric acid etc., or diluted hydrochloric acid.For example, concentration is less than 15% dilute hydrochloric acid, under normal temperature and pressure conditions, then
Acidificatoin time is 1-5 hour；Then refilter.
In the purge process of the present embodiment, please refer to Fig.1 with 2, the method for oxidation in the present embodiment employs oxidation and sets
Standby and filter plant, the method for oxidation specifically include：
Step 01：Mixture after acidified process is placed in the oxidizing solution in oxidation furnaces a；
Specifically, mixture is placed in oxidizing solution, weak acid solution, such as oxidizing solution can be used to include：
Sulfuric acid of the concentration less than 30%, potassium permanganate of the concentration less than 30% and concentration are less than 40% hydrogen peroxide.
As shown in Fig. 2, in the present embodiment, there are two oxidation reaction chamber a in oxidation reaction apparatus, then in the present invention
The quantity of oxidation reaction chamber a is not restricted.
Step 02：At normal temperatures and pressures, oxidation processes are carried out to mixture；
Specifically, at normal temperatures and pressures, as shown in Fig. 2, here oxidation processes in the oxidation reaction chamber of oxidation furnaces a into
OK, here, oxidation furnaces can be acid-resistant reacting kettle, coordinate conductivity gauge to be used together.
Step 03：After certain oxidization time, oxidation-treated mixed solution is placed in filter plant；
Specifically, the oxidization time in the present embodiment can be 1-5 hour.
Step 04：Filtering cleaning is carried out to mixed solution using pure water and filter plant b, thus by mixture not
Sizing carbon removal.
Specifically, filter plant b can be ceramic membrane, so as to be carried out using ceramic membrane and pure water to mixed solution
Filtering cleaning, so as to remove indefinite form carbon.Here, the aperture of the filter hole of ceramic membrane b can be 10-200 nanometers, pure water
Electrical conductivity can be less than 5 μ s, and the pH value for the mixed solution washed is between 3-9；This mistake can be controlled using self-con-tained unit
Journey, the invention is not limited in this regard.
In the present embodiment, which includes：Pure water is added into filter plant to carry out anti-mixed solution
Multiple filtering cleaning, until the pH value of mixed solution completes filtering cleaning between 3-9.
The oxidizing process can be by the indefinite form carbon removal in mixture；This is because prepare three-dimensional grapheme cladding simple grain
During sub- Nano diamond, some unsetting carbon can be formed, it is necessary to remove it；, can will not using oxidizing solution
Setting carbon is aoxidized, and generates CO2Gas and discharged from mixed solution so that with solid three-dimensional grapheme coat simple grain
Sub- Nano diamond phase separation.
Filtered again, can will be in solid three-dimensional grapheme cladding single-particle Nano diamond material and some solid-states
Material is separated including single-particle Nano diamond.Most separate through follow-up alkalization, heavy-fluid or alkalization, be acidified again and again afterwards
Liquid separation process excludes the impurity such as silicon, metal ion, finally obtains the higher three-dimensional grapheme cladding single-particle of purity and receives
Rice diamond.
In conclusion by the method for oxidation of the present invention, due to using the less oxidizing solution of oxidisability, can reduce
To the corrosion damage of oxidation furnaces, extend its service life, saved cost；Also, after effectively removes oxidized process
Mixture in indefinite form carbon, improve purifying rate.
Although the present invention is disclosed as above with preferred embodiment, the right embodiment illustrate only for the purposes of explanation and
, the present invention is not limited to, if those skilled in the art can make without departing from the spirit and scope of the present invention
Dry changes and retouches, and the protection domain that the present invention is advocated should be subject to described in claims.
Claims (8)
- A kind of 1. method for oxidation in purge process of three-dimensional grapheme cladding single-particle Nano diamond, to containing three-dimensional graphite The mixture of alkene cladding single-particle Nano diamond is purified, wherein, the mixture further includes unsetting carbon, kish Impurity or metal ion and silicon impurities；It is characterized in that, the purge process includes tentatively removing the mixture successively Except the Magneto separate process of the bulk metal impurity in mixture, using the acidization of weak acid or diluted strong acid, oxidizing process, Using the alkalinization and heavy-fluid separation process of weak base or diluted highly basic, the acidization is by the residual in the mixture Metal impurities or metal ion remove；The acidization and the alkalinization carry out at normal temperatures and pressures, described to aoxidize The method for oxidation of journey uses oxidation furnaces and filter plant, it includes：Step 01：The mixture after the acidization is placed in the oxidizing solution of oxidation furnaces；Wherein, it is described Oxidizing solution is the less weak oxide solution of oxidisability；Step 02：At normal temperatures and pressures, oxidation processes are carried out to the mixture；Step 03：After certain oxidization time, oxidation-treated mixed solution is placed in filter plant；Step 04：Filtering cleaning is carried out to the mixed solution using pure water and filter plant, so that by the mixture Indefinite form carbon removal.
- 2. method for oxidation according to claim 1, it is characterised in that the oxidizing solution includes：Concentration is less than 30% potassium permanganate of sulfuric acid, concentration less than 30% and concentration are less than 40% hydrogen peroxide.
- 3. method for oxidation according to claim 1, it is characterised in that when the acidificatoin time is 1-5 small.
- 4. method for oxidation according to claim 1, it is characterised in that the kish impurity or metal ion for Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu or Zn.
- 5. method for oxidation according to claim 1, it is characterised in that also comprising acidified again after the oxidizing process Journey, then acidization further remove the trace metal ion remained after oxidizing process in the mixture.
- 6. method for oxidation according to claim 1, it is characterised in that the pore size filter of the filter plant is received for 10-200 Rice.
- 7. method for oxidation according to claim 1, it is characterised in that the electrical conductivity of the pure water is less than 5 μ s/cm.
- 8. method for oxidation according to claim 1, it is characterised in that in the step 04, the filtering cleaning process bag Include：Pure water is added into the filter plant repeated filtration cleaning is carried out to mixed solution, until the pH of the mixed solution Value completes filtering cleaning between 3-9.
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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 |
|---|
| "人造金刚石微粉提纯工艺技术研究";樊亮 等;《非金属矿》;20040731;第27卷(第4期);第32-34页 * |
| "针对铁基触媒的金刚石提纯工艺研究";李和胜 等;《金刚石与磨料磨具工程》;20061031(第5期);第62-65页 * |
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