CN105565312A - Acidifying method for three-dimensional graphene-coated single-particle nano-diamond material during purifying - Google Patents
Acidifying method for three-dimensional graphene-coated single-particle nano-diamond material during purifying Download PDFInfo
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- CN105565312A CN105565312A CN201410538311.3A CN201410538311A CN105565312A CN 105565312 A CN105565312 A CN 105565312A CN 201410538311 A CN201410538311 A CN 201410538311A CN 105565312 A CN105565312 A CN 105565312A
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Abstract
The invention provides an acidifying method for a three-dimensional graphene-coated single-particle nano-diamond material during purifying. The acidifying method is applied to magnetic separation, acidifying, oxidation, alkalization and heavy liquid separation of a mixture; during acidifying, an acidic solution with low acidity is used for acidifying; and after acidifying, a filtering device and purified water are cooperatively used for filtering and washing of an acidified mixed solution, so metal particle impurities in the mixture can be removed, and favorable conditions are provided for subsequent further purification. Due to usage of the acidic solution low acidity, the acidifying method provided by the invention can reduce corrosive damage to acidifying equipment, prolongs the service life of the acidifying equipment and saves cost; moreover, after a displacement reaction, the metal particle impurities can be changed into liquid from solids and are then filtered out, so the metal particle impurities in the mixture are effectively removed, and a purifying rate is increased.
Description
Technical field
The present invention relates to chemical technique technical field, be specifically related to the souring method 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 matrix 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, adopt the equipment of strong acid to purifying to have strong corrodibility, the work-ing life of equipment can be shortened, 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 souring method in the purge process of a kind of three-dimensional grapheme coated single-particle Nano diamond material, 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 souring method in the purge process of a kind of three-dimensional grapheme coated single-particle Nano diamond material, 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; Described souring method adopts acidizing unit and filter plant, and it comprises:
Step 01: the acidic solution described mixture through described Magneto separate process being placed in acidizing unit;
Step 02: at normal temperatures and pressures, adopts weak acid to carry out acidification to described mixture;
Step 03: after certain acidificatoin time, is placed in filter plant by the mixing solutions through acidification;
Step 04: adopt pure water and filter plant to carry out filtration cleaning to described mixing solutions, thus the trace metal particle impurities in described mixture is removed.
Preferably, described acidic solution is dilute hydrochloric acid, and the concentration of described dilute hydrochloric acid is 5-25%.
Preferably, described acidificatoin 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.
Souring method 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 acidization, acid less acidic solution is adopted to carry out acidification, adopt filter plant after acidulation and in conjunction with pure water, cleaning filtered to the mixing solutions of acidifying, thus the metallics impurity can removed in mixture, for follow-up being further purified provides favourable condition; Souring method of the present invention, because the acidity of the acidic solution adopted is less, can reduces the corrosion damage to acidizing unit, extend its work-ing life, save cost; Further, through replacement(metathesis)reaction, metallics impurity can be become liquid from solid-state, then be filtered out, effectively removes the metallics impurity in mixture, improve purifying rate.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the souring method 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 be a preferred embodiment of the present invention the relation of equipment of souring method
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 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 souring method in the purge process of a kind of three-dimensional grapheme coated single-particle Nano diamond material for this reason, in experience Magneto separate, acidifying, oxidation, alkalization and heavy-fluid sepn process, its acidization, acid less acidic solution is adopted to carry out acidification, adopt filter plant after acidulation and in conjunction with pure water, cleaning filtered to the mixing solutions of acidifying, thus the metallics impurity 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 energetic material reactor;
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 present invention carries out purifying to the mixture containing the coated single-particle Nano diamond of three-dimensional grapheme prepared, purge process can comprise carries 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; Said souring method is applied in said acidization, adopts acidizing unit and filter plant; Its souring method comprises:
Step 01: the acidic solution mixture after Magneto separate process being placed in acidizing unit;
Step 02: at normal temperatures and pressures, carries out acidification to mixture;
Step 03: after certain acidificatoin time, is placed in filter plant by the mixing solutions through acidification;
Step 04: adopt pure water and filter plant to carry out filtration cleaning to mixing solutions, thus the trace metal particle impurities in mixture is removed.
It should be noted that, acidization here can comprise an acidification, also can comprise repeatedly acidification, and souring method of the present invention can be applied in each acidification process.
Below with reference to accompanying drawing 1-2 and specific embodiment, the souring method 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 souring method 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 souring method 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.
In the present embodiment, carry out purifying to the mixture containing three-dimensional grapheme coated single-particle Nano diamond material prepared, purge process 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; Oxidising process can be carried out under normal temperature and pressure conditions, and mixture is placed in oxidizing solution, and the oxidizing solution of employing can carry out redox reaction for sulfuric acid, potassium permanganate or hydrogen peroxide etc.; This oxidising process can by the unsetting carbon removal in mixture; 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.
After Magneto separate process, refer to Fig. 1 and 2, the souring method in the present embodiment, have employed acidizing unit and filter plant, this souring method specifically comprises:
Step 01: the acidic solution mixture after Magneto separate process being placed in acidizing unit a;
Concrete, mixture, after Magneto separate, excludes bulk metal, after this, mixture is placed in acidic solution, can be the strong acid solution of weak acid or dilution, such as, and the hydrochloric acid of dilution, sulfurous acid, carbonic acid, hypochlorous acid, hydrosulphuric acid etc.;
Step 02: at normal temperatures and pressures, carries out acidification to mixture;
Concrete, at normal temperatures and pressures, as shown in Figure 2, acidification is carried out in the acidification reaction chamber of acidizing unit a here, and the acidic solution adopted is dilute hydrochloric acid, and the concentration of dilute hydrochloric acid can be 5-25%.Here, acidizing unit can be acid-resistant reacting kettle, coordinates conductivity meter to use together.
Step 03: after certain acidificatoin time, is placed in filter plant by the mixing solutions through acidification;
Concrete, the acidificatoin 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 the trace metal particle impurities in mixture is removed.
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 metallics impurity.Here, the aperture of the filter pore of ceramic membrane c 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.
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.; This is due in acidization, acidic solution can with metallics impurity generation replacement(metathesis)reaction, be chloride soln by metallics impurity conversion, and be no longer solid-state, be convenient to carry out filtering separation with in the solid-state coated single-particle Nano diamond of three-dimensional grapheme.
In sum, by souring method of the present invention, owing to adopting acid less acidic solution, the corrosion damage to acidizing unit can be reduced, extend its work-ing life, save cost; Further, through replacement(metathesis)reaction, metallics impurity can be become liquid from solid-state, then be filtered out, effectively removes the metallics impurity in mixture, 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 souring method in the purge process of a purifying three-dimensional grapheme coated single-particle Nano diamond material, 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; Described souring method adopts acidizing unit and filter plant, and it comprises:
Step 01: the acidic solution described mixture through described Magneto separate process being placed in acidizing unit;
Step 02: at normal temperatures and pressures, carries out acidification to described mixture;
Step 03: after certain acidificatoin time, is placed in filter plant by the mixing solutions through acidification;
Step 04: adopt pure water and filter plant to carry out filtration cleaning to described mixing solutions, thus the trace metal particle impurities in described mixture is removed.
2. souring method according to claim 1, is characterized in that, in described step 01, described acidic solution is dilute hydrochloric acid, and the concentration of described dilute hydrochloric acid is 5-25%.
3. souring method according to claim 1, is characterized in that, described acidificatoin time is 1-5 hour.
4. souring method according to claim 1, is characterized in that, the pore size filter of described filter plant is 10-200 nanometer.
5. souring method according to claim 1, is characterized in that, described pure electrical conductivity of water is less than 5 μ s/cm.
6. souring method 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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Cited By (1)
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| CN108264441A (en) * | 2018-04-24 | 2018-07-10 | 中国工程物理研究院化工材料研究所 | A kind of octogen of graphene oxide cladding and preparation method thereof |
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| US20140004031A1 (en) * | 2012-06-28 | 2014-01-02 | Arizona Board Of Regents On Behalf Of The University Of Arizona | Method of purifying nanodiamond powder and purified nanodiamond powder |
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| CN101208462A (en) * | 2005-06-29 | 2008-06-25 | 日本化药株式会社 | Process for producing fine diamond and fine diamond |
| CN101641286A (en) * | 2007-02-09 | 2010-02-03 | 石塚博 | Diamond micropowder powder and capture method thereof, and the diamond slurries that disperseed this diamond micropowder powder |
| CN102906019A (en) * | 2010-04-14 | 2013-01-30 | 贝克休斯公司 | Method of preparing polycrystalline diamond from derivatized nanodiamond |
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