CN101857195A - Efficient mechanical method for peeling layered compounds - Google Patents
Efficient mechanical method for peeling layered compounds Download PDFInfo
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- CN101857195A CN101857195A CN201010179151A CN201010179151A CN101857195A CN 101857195 A CN101857195 A CN 101857195A CN 201010179151 A CN201010179151 A CN 201010179151A CN 201010179151 A CN201010179151 A CN 201010179151A CN 101857195 A CN101857195 A CN 101857195A
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Abstract
The invention relates to an efficient mechanical method for peeling layered compounds, relating to a method for peeling layered compounds. The invention overcomes the disadvantages of low efficiency for peeling the layered compounds, difficulty in acquiring a large amount of 1 to 10 layers of nanometer slices, easy damage to the lattice of the layered compounds, and the like of the traditional mechanical methods for peeling the layered compounds, such as high-energy ball-milling method, sanding method, and the like. Meanwhile, the invention overcomes the disadvantage of difficult separation of superfine grinding media. In the invention, solid particles and liquid work media (or gas work media) are utilized, and the layered compounds are separated after being mechanically peeled so that the layered compounds are peeled. The invention has the advantages of high grinding efficiency, acquirement of a large amount of 1 to 10 layers of nanometer slices, no change of the lattice of the layered compounds, and easy separation of the grinding media.
Description
Technical field
The present invention relates to the method for peeling layered compounds.
Background technology
Lamellar compound is that a class has the laminated body structure, laminate is passed through coplane or is total to the limit by certain specific structure unit to pile up the compound that forms the particular space structure, each laminate can be regarded a huge planar molecule as, and lamellar compound is formed by the big molecule mutual superposition in these planes exactly.Inorganic layered compounds demonstrates physics, the chemical property of many uniquenesses, and its individual layer or thin layer compound itself and its functional composite material show excellent performance at aspects such as light, electricity, magnetic, catalysis, cause people's special concern.
Lamellar compound of a great variety can be divided into inorganic layered compounds two classes usually: the first kind is that the laminate skeleton does not show electrically typical representative species such as graphite, vanadic anhydride, molybdenum trioxide, hexagonal boron nitride etc.; Second class is that the laminate skeleton is charged, generally electrically charged according to its institute is cationic lamellar compound and anion type laminated compound with it, typical representative species such as hydrotalcite, houghite, polynary sulfide uranyl vanadate, graphite oxide, graphite intercalation compound, montmorillonite, saponite, vermiculite, dolomite etc.Because the ionic lamellar compound easily obtains monolayer material at solution system by intercalation, so study more; The research of the non-electrical inorganic layered compounds that layer structure kept by Van der Waals force is less relatively, but along with the appearance of Graphene this type of research is being become focus in recent years.
To the many methods of having peeled off of lamellar compound, wherein utilizing solvent or chemical reaction to carry out intercalation is main method at present.Though be that the Mechanical Method of representative has research but has following problem by contrast with the high-energy ball milling.
High-energy ball milling (or sand milling) abrasive media particle diameter big (several millimeters-several centimetres), the Impact energy height, graphite can be to amorphous transition, so can do great damage to lamellar compound under the high-energy ball milling effect on existing research surface;
1. if the mode of employing reduction ball milling speed reduces the destruction to lamellar compound, then grinding efficiency is extremely low.This is that its unit volume abrasive media quantity is few because high-energy ball milling abrasive media particle diameter is big, and its number is much smaller than by the number of abrasive particles, and abrasive media is with very low by the bump probability of abrasive grains in mechanical milling process, and grinding efficiency is low.
2. the grinding with graphite is an example, and present result of study shows that general mechanical milling method can obtain the nano flake lamellar compound about 100nm, but is difficult to obtain in enormous quantities 1 layer of lamellar compound to which floor.
So it is generally acknowledged that Mechanical Method such as high-energy ball milling, sand milling are unsuitable for lamellar compound is carried out high efficiency peeling off in enormous quantities.It should be noted that the used abrasive media particle diameter of Mechanical Method such as high-energy ball milling, sand milling more than or equal to 0.3 millimeter, meticulous abrasive media is not used with being separated by abrasive grains because of being difficult to.
Summary of the invention
The invention solves existing machinery method peeling layered compounds exist grinding efficiency low, be difficult to obtain 1 ~ 10 layer a large amount of nano flakes, destroy the lattice of lamellar compound and meticulous shortcomings such as the difficult separation of abrasive media.
The present invention realizes by following proposal:
Scheme one: the method for efficient mechanical peeling layered compounds realizes by following step: with lamellar compound, particle diameter is to carry out mechanical stripping after the solid particle of 1nm ~ 100 μ m and liquid-working-medium mix, splitting time is more than 5 minutes, and liquid-working-medium is that 10 ~ 73mN/m and viscosity are 1 ~ 1 * 10 at the operating temperature lower surface tension force of mechanical stripping
9MPas separates then to remove solid particle and liquid-working-medium; Promptly finished peeling off to lamellar compound; Wherein add dispersant in the mechanical stripping process, dispersant dosage is 0 ~ 20% of a liquid-working-medium.
Scheme two: the method for efficient mechanical peeling layered compounds is undertaken by following step: in airslide disintegrating mill, with gas working dielectric and particle diameter is that the solid particle of 1nm ~ 100 μ m carries out mechanical stripping to lamellar compound, splitting time is removed solid particle then more than 5 minutes; Promptly finished peeling off to lamellar compound.
Solid particle described in above-mentioned two schemes is a magnesium, aluminium, iron, cobalt, nickel, copper, zinc, silver, tin, vanadium, chromium, tungsten, copper alloy, aluminium alloy, kirsite, iron-carbon alloy, magnesium alloy, lithium alloy, boron oxide, silica, zirconia, aluminium oxide, calcium carbonate, magnesia, titanium dioxide, iodine, zinc oxide, tin oxide, di-iron trioxide, tri-iron tetroxide, aluminium nitride, aluminium chloride, titanium nitride, carborundum, sodium fluoride, ammonium fluoride, calcium oxide, carbonic hydroammonium, ammonium bromide, ammonium chromate, ammonium dihydrogen phosphate (ADP), ammonium formate, ammonium acetate, sodium acid carbonate, ammonium hydrogen phosphate, ammonium iodide, ammonium nitrate, ammonium oxalate, ammonium sulfate, ammonium sulfite, ammonium tartrate, ammonium thiocyanate, ammonium acetate, barium iodide, barium nitrate, calcium bromide, calcium iodide, calcium nitrate, calcium nitrite, potassium acetate, potassium bromate, KBr, potash, potassium chlorate, potassium chloride, potassium chromate, potassium bichromate, potassium dihydrogen phosphate, the potassium ferricyanide, potassium ferrocyanide, potassium fluoride, potassium formate, potassium acid sulfate, potassium hydroxide, KI, potassium nitrate, potassium oxalate, potassium sulfate, potassium thiosulfate, lithium acetate, lithium bromide, sodium chloride, lithium chloride, lithium formate, lithium iodide, aluminum nitrate, aluminum sulfate, magnesium acetate, magnesium bromide, magnesium iodide, magnesium sulfate, sodium acetate, sodium carbonate, sodium dihydrogen phosphate, sodium formate, sodium acetate, sodium nitrate, sodium phosphate, sodium sulphate, nickel chloride, nickel nitrate, frerrous chloride, ferrous sulfate, iron chloride, copper chloride, copper nitrate, copper sulphate, zinc sulfate, sucrose, urea, polymer microsphere, a kind of or wherein several mixing in the glass dust.
The present invention utilizes automation to peel off and obtains 1 ~ 10 layer a large amount of nano flake lamellar compounds, and separates easily with abrasive media; Lamellar compound is far longer than the interaction of atom between layer and the layer in the covalent bonding intensity between the atom on the layer plane, and the mass of solid particles of the present invention's use is little, and same movement speed energy is lower, the covalent bond of survivable lamellar compound; The present invention uses a large amount of solid particles, in process of lapping can with collided by the abrasive grains high-frequency, thereby improve grinding efficiency greatly and guaranteed that the lattice of nano flake lamellar compound does not change; The solid particle of huge amount can disperse to be helped to solve the dispersion agglomeration traits of ultra-fine grain by the particle of grinding superfine well.The present invention uses liquid or gas working dielectric to play an important role to peeling off, working media can be peeled off required strength to solid particle and lamellar compound transmission on the one hand, on the other hand, working media has certain peptizaiton to lamellar compound nano thin-layer and solid particle, hinder compound between the stratiform compound nano thin layer, in addition, working media can absorb and conduct the heat that produces in the mechanical stripping process, avoids the overheated lamellar compound nano thin-layer that makes to produce defective.The inventive method is applicable to peeling off of various lamellar compounds; Lamellar compound for example: graphite, vanadic anhydride, molybdenum trioxide, hexagonal boron nitride, metal dithionite thing (MX2, wherein M=Sn, Ti, Zr, Hf, V, Nb, Ta, Mo, W, X=S, Se, Te), Hofmann type compound: Ni (CN)
2NH
3, kaolinite, dickite, pyrophillite, hydrotalcite (LDHs,
M
IIIBe ionic radius and the approaching trivalent metal ion of magnesium ion; A
N-Be anion), houghite (
, M
II=Mg, Fe, Co, Ni, Mn, Zn; M
III=Al, Fe, Cr, Mn, V; A
N-Be anion), polynary sulfide (AMS
2, A=Na, K, M=Cr, V; ACuFeS
2, A=Li, Na, K; Li
2FeS
2, K
2Pt
4S
6), transition metal oxide,
(M
IBe alkali metal ion; M
III=Ti, V, Cr, Mn, Fe, Co, Ni), interlayer is alkali-metal titanate and niobates and niobate-titanate, uranyl vanadate, graphite oxide, graphite intercalation compound, montmorillonite, saponite, vermiculite, dolomite etc.
The specific embodiment
The specific embodiment one: the method for efficient mechanical peeling layered compounds realizes by following step in the present embodiment: with lamellar compound, particle diameter is to carry out mechanical stripping after the solid particle of 1nm ~ 100 μ m and liquid-working-medium mix, splitting time is more than 5 minutes, and liquid-working-medium is that 10 ~ 73mN/m and viscosity are 1 ~ 1 * 10 at the operating temperature lower surface tension force of mechanical stripping
9MPas separates then to remove solid particle and liquid-working-medium; Promptly finished peeling off to lamellar compound; Wherein add dispersant in the mechanical stripping process, dispersant dosage is 0 ~ 20% of a liquid-working-medium.
The described operating temperature of present embodiment promptly will satisfy the equipment requirement will guarantee also that simultaneously liquid-working-medium is in liquid condition in the mechanical stripping process.
The used dispersant of present embodiment can be selected PEI (PEI), softex kw (CTAB), polyacrylic acid (PAA), lauryl sodium sulfate (SDS), dodecyl sodium sulfate (SDBS), commodity dispersant etc. for use, and the commodity dispersant can be selected Disperbyk-163 wetting dispersing agent, Disperbyk-2150 wetting dispersing agent, super dispersant Tilo-3000, super dispersant Tilo-5110, super dispersant Tilo-27000 etc. for use.
Present embodiment is utilized automation to peel off and is obtained 1 ~ 10 layer a large amount of nano flake lamellar compounds, and separates easily with abrasive media; Lamellar compound is far longer than the interaction of atom between layer and the layer in the covalent bonding intensity between the atom on the layer plane, and the mass of solid particles of present embodiment use is little, and same movement speed energy is lower, the covalent bond of survivable lamellar compound; Present embodiment is used a large amount of solid particles, in process of lapping can with collided by the abrasive grains high-frequency, thereby improve grinding efficiency greatly and guaranteed that the lattice of nano flake lamellar compound does not change; The solid particle of huge amount can disperse to help to solve the dispersion agglomeration traits of ultra-fine grain to by the particle of grinding superfine well.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: described solid particle is a magnesium, aluminium, iron, cobalt, nickel, copper, zinc, silver, tin, vanadium, chromium, tungsten, copper alloy, aluminium alloy, kirsite, iron-carbon alloy, magnesium alloy, lithium alloy, boron oxide, silica, zirconia, aluminium oxide, calcium carbonate, magnesia, titanium dioxide, iodine, zinc oxide, tin oxide, di-iron trioxide, tri-iron tetroxide, aluminium nitride, aluminium chloride, titanium nitride, carborundum, sodium fluoride, ammonium fluoride, calcium oxide, carbonic hydroammonium, ammonium bromide, ammonium chromate, ammonium dihydrogen phosphate (ADP), ammonium formate, ammonium acetate, sodium acid carbonate, ammonium hydrogen phosphate, ammonium iodide, ammonium nitrate, ammonium oxalate, ammonium sulfate, ammonium sulfite, ammonium tartrate, ammonium thiocyanate, ammonium acetate, barium iodide, barium nitrate, calcium bromide, calcium iodide, calcium nitrate, calcium nitrite, potassium acetate, potassium bromate, KBr, potash, potassium chlorate, potassium chloride, potassium chromate, potassium bichromate, potassium dihydrogen phosphate, the potassium ferricyanide, potassium ferrocyanide, potassium fluoride, potassium formate, potassium acid sulfate, potassium hydroxide, KI, potassium nitrate, potassium oxalate, potassium sulfate, potassium thiosulfate, lithium acetate, lithium bromide, sodium chloride, lithium chloride, lithium formate, lithium iodide, aluminum nitrate, aluminum sulfate, magnesium acetate, magnesium bromide, magnesium iodide, magnesium sulfate, sodium acetate, sodium carbonate, sodium dihydrogen phosphate, sodium formate, sodium acetate, sodium nitrate, sodium phosphate, sodium sulphate, nickel chloride, nickel nitrate, frerrous chloride, ferrous sulfate, iron chloride, copper chloride, copper nitrate, copper sulphate, zinc sulfate, sucrose, urea, polymer microsphere, a kind of or wherein several mixing in the glass dust.Other step is identical with the specific embodiment one with parameter.
When the present embodiment solid particle is mixture, press between various solid particles arbitrarily than mixing.Above-mentioned solid particle can adopt following method to remove respectively according to its character:
The first kind: can be dissolved in the solid particle of acid, aqueous slkali, for example: Al, Cu, Zn, SnO, ZnO, B
2O
3, SiO
2, NaHCO
3, CaCO
3, CaO etc., can remove by pickling or alkali cleaning;
Second class: room temperature-high temperature (for example 100 ℃) solubility with temperature changes material greatly, for example: carbonic hydroammonium, ammonium dihydrogen phosphate (ADP), ammonium oxalate, potassium dihydrogen phosphate, potassium chloride, potassium ferrocyanide, potassium sulfate, sodium carbonate, sodium dihydrogen phosphate, sodium sulphate, sodium phosphate, sucrose, urea, adopt low-temperature working then to heat up the solid particle dissolving removed;
The 3rd class: the very big material of dissolubility difference in different solvents, for example: most of ionic compounds are (as NaCl, K
2CO
3, KCl, AlCl
3) solubility is big and at ethanol, benzene, CCl in water
4Less Deng solubility in the organic solvent, adopt and in organic working media, to work and the method for after washing is removed;
The 4th class: segregative material under electric field, magnetic field effect, for example: Al
2O
3, CaCO
3, Fe
2O
3, Fe
3O
4, Fe etc., remove by electric field, magnetic field, as removing with static classified filtering equipment or magnetic field separation equipment;
The 5th class: volatile, the distillation of high temperature when heating, decompose the solid particle of removing, as sucrose, I
2, urea, NH
4NO
3, NH
4HCO
3, CH
3COONH
4Deng, adopt the way of high temperature heating to remove;
The 6th class: heavy solid particle, as zirconia, vanadium, chromium, tungsten etc., (telling 20-2 μ m as linear vibrating screen classifying equipoment, gas flow sizing machine removes with thin micro mist, tripod pendulum type batch centrifugal-SS450, multistage grader (step Electronics Co., Ltd. is opened in Shenzhen) to adopt the classification separation equipment.
The specific embodiment three: what present embodiment was different with the specific embodiment one or two is: the weight ratio 1:0.1 of layered compound and solid particle ~ 10000.
The specific embodiment four: what present embodiment and the specific embodiment three were different is: the weight ratio 1:1 of layered compound and solid particle ~ 2000.Other step is identical with the specific embodiment three with parameter.
The specific embodiment five: what present embodiment and the specific embodiment three were different is: the weight ratio 1:5 of layered compound and solid particle ~ 1000.Other step is identical with the specific embodiment three with parameter.
The specific embodiment six: what present embodiment and the specific embodiment three were different is: the weight ratio 1:10 of layered compound and solid particle ~ 500.Other step is identical with the specific embodiment three with parameter.
The specific embodiment seven: what present embodiment and the specific embodiment three were different is: the weight ratio 1:100 of layered compound and solid particle ~ 200.Other step is identical with the specific embodiment three with parameter.
The specific embodiment eight: what present embodiment was different with one of specific embodiment one to seven is: the weight ratio 1:0.1 of described solid particle and liquid-working-medium ~ 10000.
The specific embodiment nine: what present embodiment and the specific embodiment eight were different is: the weight ratio 1:0.2 of described solid particle and liquid-working-medium ~ 5000.Other step is identical with the specific embodiment eight with parameter.
The specific embodiment ten: what present embodiment and the specific embodiment eight were different is: the weight ratio 1:100 of described solid particle and liquid-working-medium ~ 2000.Other step is identical with the specific embodiment eight with parameter.
The specific embodiment 11: what present embodiment and the specific embodiment eight were different is: the weight ratio 1:200 of described solid particle and liquid-working-medium ~ 500.Other step is identical with the specific embodiment eight with parameter.
The specific embodiment 12: what present embodiment was different with one of specific embodiment one to 11 is: dispersant dosage accounts for 0.01% ~ 15% of liquid-working-medium volume.Other step is identical with one of specific embodiment one to 11 with parameter.
The specific embodiment 13: what present embodiment was different with one of specific embodiment one to 12 is: dispersant dosage accounts for 0.1 ~ 10% of liquid-working-medium volume.Other step is identical with one of specific embodiment one to 12 with parameter.
The specific embodiment 14: what present embodiment was different with one of specific embodiment one to 12 is: dispersant dosage accounts for 1 ~ 8% of liquid-working-medium volume.Other step is identical with one of specific embodiment one to 12 with parameter.
The specific embodiment 15: what present embodiment was different with one of specific embodiment one to 12 is: dispersant dosage accounts for 5% of liquid-working-medium volume.Other step is identical with one of specific embodiment one to 12 with parameter.
The specific embodiment 16: what present embodiment was different with one of specific embodiment one to 15 is: the surface tension 40 ~ 50mN/m of described liquid-working-medium.Other step is identical with one of specific embodiment one to 15 with parameter.
The specific embodiment 17: one of present embodiment and specific embodiment one to 15 are not both: the surface tension 45mN/m of described liquid-working-medium.Other step is identical with one of specific embodiment one to 15 with parameter.
The specific embodiment 18: what present embodiment was different with one of specific embodiment one to 17 is: the viscosity of described liquid-working-medium is 100 ~ 500000mPas.Other step is identical with one of specific embodiment one to 17 with parameter.
The specific embodiment 19: what present embodiment was different with one of specific embodiment one to 17 is: the viscosity of described liquid-working-medium is 1000 ~ 50000mPas.Other step is identical with one of specific embodiment one to 17 with parameter.
The specific embodiment 20: what present embodiment was different with one of specific embodiment one to 17 is: the viscosity of described liquid-working-medium is 5000mPas.Other step is identical with one of specific embodiment one to 17 with parameter.
The specific embodiment 21: what present embodiment was different with one of the specific embodiment and specific embodiment one to 20 is: the particle diameter of described solid particle is 5nm ~ 100nm.Other step is identical with one of specific embodiment one to 15 with parameter.
The specific embodiment 22: what present embodiment and the specific embodiment and the specific embodiment 21 were different is: the particle diameter of described solid particle is 200nm ~ 500nm.Other step is identical with the specific embodiment 21 with parameter.
The specific embodiment 23: what present embodiment and the specific embodiment and the specific embodiment 21 were different is: the particle diameter of described solid particle is 1 μ m ~ 20 μ m.Other step is identical with the specific embodiment 21 with parameter.
The specific embodiment 24: what present embodiment and the specific embodiment and the specific embodiment 21 were different is: the particle diameter of described solid particle is 50 μ m ~ 80 μ m.Other step is identical with the specific embodiment 21 with parameter.
The specific embodiment 25: what present embodiment was different with one of specific embodiment one to 24 is: mechanical stripping is carried out in a kind of or wherein several logotype in employing homogenizer, colloid mill, three-roller, screw extruder, ball mill, pan-milling machine, sand mill, oscillating mill and the ultrasonic device; Described liquid-working-medium is the aqueous solution, the alcoholic solution of alkanes, the alcoholic solution of ketone, the aqueous solution of amine or the alkane solution of aromatic compound of water, alcohols, aromatic compound, ketone, amine, ionic liquid, alkanes, heterocyclic compound, carbon disulfide, carbon tetrachloride, gasoline, vegetable oil, diesel oil, wax, alcohol.Other step is identical with one of specific embodiment one to 24 with parameter.
The specific embodiment 26: what present embodiment and the specific embodiment 25 were different is: described alcohols is ethanol, normal propyl alcohol, n-butanol, ethylene glycol, propane diols, 1,2-butanediol, 1,3-butanediol, 1, a kind of or wherein several mixing in 4-butanediol, glycerine and the isopropyl alcohol.Other step is identical with the specific embodiment 25 with parameter.
When alcohols is mixture in the present embodiment, press between various alcohols arbitrarily than mixing.
The specific embodiment 27: what present embodiment and the specific embodiment 25 were different is: described aromatic compound is benzene, toluene, naphthalene or anthracene.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 28: what present embodiment and the specific embodiment 25 were different is: described ketone is acetone or Ν-methyl pyrrolidone.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 29: what present embodiment and the specific embodiment 25 were different is: described amine is N, dinethylformamide or N, N-dimethylacetylamide.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 30: what present embodiment and the specific embodiment 25 were different is: described ionic liquid is 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole hexafluorophosphate or 1-ethoxy-3-methyl hexafluorophosphate.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 31: what present embodiment and the specific embodiment 25 were different is: described alkanes is n-hexane, octane or decane.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 32: what present embodiment and the specific embodiment 25 were different is: described heterocyclic compound is furans or pyridine.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 33: what present embodiment and the specific embodiment 25 were different is: alcohol is methyl alcohol, ethanol, butanediol, glycerine or isopropyl alcohol in the aqueous solution of described alcohol.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 34: what present embodiment and the specific embodiment 25 were different is: the alcoholic solution of described alkanes is the octanol solution of n-hexane, the decyl alcohol of n-hexane or the decyl alcohol of octadecane.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 35: what present embodiment and the specific embodiment 25 were different is: the alcoholic solution of described ketone is the butanediol solution of acetone or the ethanolic solution of acetone.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 36: what present embodiment and the specific embodiment 25 were different is: the amine in the aqueous solution of described amine is N, dinethylformamide or N, N-dimethylacetylamide.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 37: what present embodiment and the specific embodiment 25 were different is: the hexane solution of the alkane solution benzene of described aromatic compound or the hexane solution of toluene.Other step is identical with the specific embodiment 25 with parameter.
The specific embodiment 38: what present embodiment was different with one of specific embodiment one to 24 is: adopt mill, banbury, homogenizer, colloid mill, three-roller or screw extruder to carry out mechanical stripping, described liquid-working-medium is a macromolecular compound.Other step is identical with one of specific embodiment one to 24 with parameter.
The specific embodiment 39: what present embodiment and the specific embodiment 38 were different is: described macromolecular compound polyacrylate, polyvinyl alcohol, polyethylene glycol, polyvinyl acetate, starch, polybutadiene, poly-butylbenzene diene, epoxy resin, rubber or pitch.Other step is identical with the specific embodiment 38 with parameter.
The specific embodiment 40: the present embodiment efficient mechanical is peeled off the method for graphite and is finished by following step: the silica that is 7nm with 1 part of crystalline graphite powder, 4 parts of particle diameters and 200 part 1 by weight percentage, the mixing of 3-butanediol is placed in the homogenizer, add polyacrylic acid again, the polyacrylic acid consumption is 1,5% of 3-butanediol volume, peeled off 0.5 ~ 100 hour with 4000 rev/mins speed mechanical, filter, the adding mass percent concentration is 5% HF dissolving SiO
2, washing, filtration; Promptly finished peeling off to graphite.
Present embodiment obtains 1 ~ 10 layer a large amount of Graphenes, and productive rate is more than 92%.
The specific embodiment 41: efficient mechanical is peeled off the method for graphite oxide and is finished by following step: by weight percentage with 1 part of graphite oxide powder, 10 parts of CaCO
3Be placed in the oscillating mill with 100 parts of isopropyl alcohols mixing, add softex kw then, the softex kw consumption is 1% of an isopropyl alcohol volume, and mechanical stripping 0.5 ~ 100 hour filters and obtains graphene oxide and CaCO
3Mixture, add mass percent concentration and be 10% ~ 30% HCl dissolving CaCO
3, washing, filtration; Promptly finished peeling off to graphite oxide.
The present embodiment method is peeled off graphite oxide, obtains graphene oxide, and resulting graphene oxide has individual layer or sandwich construction, and thickness is in 0.5 ~ 5nm scope, and its productive rate is more than 90%.
The specific embodiment 42: the present embodiment efficient mechanical is peeled off the method for hexagonal boron nitride and is finished by following step: one, take by weighing 1 part of hexagonal boron nitride powder, 80 ~ 200 parts of potassium dihydrogen phosphates and 100 ~ 400 parts of water by weight percentage, under 90 ℃ of conditions potassium dihydrogen phosphate is being put into graphite powder after soluble in water then, obtain mixture and place sand mill, add dodecyl sodium sulfate again, the dodecyl sodium sulfate consumption is 0.5% of a water volume; Two, in 0.1 ~ 10 hour said mixture being cooled to 20 ~ 50 ℃ utilizes sand mill to peel off with 1000 ~ 10000 rev/mins speed simultaneously; Three, be warming up to 90 ℃ then, in 0.1 ~ 10 hour, be cooled to 20 ~ 50 ℃ again and utilize sand mill to peel off simultaneously with 1000 ~ 10000 rev/mins speed; Four, the operation of repeating step two and step 3 is 0 ~ 20 time, continued mechanical stripping 0.1 ~ 100 hour, obtain the mixture of Graphene-potassium dihydrogen phosphate-water, add hot mixt to 100 ℃ (purpose is the dissolving phosphoric acid potassium dihydrogen), promptly finished peeling off after filtering, cleaning hexagonal boron nitride.
The whole process of the described method of present embodiment is pollution-free, is the synthetic route of a green.
The present embodiment method is peeled off hexagonal boron nitride, obtains the nano flake hexagonal boron nitride, and resulting nano flake hexagonal boron nitride has individual layer or multilayer (2 ~ 10 layers) structure, and its productive rate is more than 96%.
The specific embodiment 43: the present embodiment efficient mechanical is peeled off LiMnO
2Method finish by following step: by weight percentage with 1 part of LiMnO
2, 10 ~ 500 parts of ZrO
2Be placed in the homogenizer with 500 ~ 5000 parts of ethanol mixing, add polyacrylic acid again, the polyacrylic acid consumption is 3% of an ethanol volume, peels off 0.5 ~ 100 hour with 4000 rev/mins speed, filters the back oven dry then, utilizes the electrostatic separation device separates to go out ZrO
2, promptly finished LiMnO
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake LiMnO
2, productive rate is more than 90%.
The specific embodiment 44: the present embodiment efficient mechanical is peeled off NbSe
2Method finish by following step: by weight percentage with 1 part of NbSe
2, 50 ~ 1000 parts of KCl and 250 ~ 2500 parts of ethanol and 250 ~ 2500 parts of glycerine mix and are placed in the homogenizer, add polyacrylic acid again, the polyacrylic acid consumption is 0.5% of an ethanol volume, peeled off 0.5 ~ 100 hour with 4000 rev/mins speed, filter the back then and add 500 ~ 3000 parts of water (being used to dissolve KCl), filter, water cleans; Promptly finished NbSe
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake NbSe
2, productive rate is more than 90%.
The specific embodiment 45: the present embodiment efficient mechanical is peeled off kaolinic method and is finished by following step: by weight percentage with the Fe of 1 part of kaolin, 150 parts of about 2 μ m of diameter
2O
3Be placed in the oscillating mill with 100 parts of isopropyl alcohols mixing, add softex kw (CTAB) then, the softex kw consumption is 2% of an isopropyl alcohol volume, peels off 0.5 ~ 50 hour, filters the back and removes Fe with magnetic field classified filtering equipment
2O
3Promptly finished and peeled off kaolinic.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake kaolin, and productive rate is more than 90%.
The specific embodiment 44: the present embodiment efficient mechanical is peeled off graphite FeCl
3The method of intercalation compound is finished by following step: by weight percentage with 1 part of graphite FeCl
3The Fe of intercalation compound, 100 parts of about 1 μ m of diameter
2O
3Be placed in the oscillating mill with 200 parts of isopropyl alcohols mixing, add polyacrylic acid (PAA) again, the polyacrylic acid consumption is 1.5% of an isopropyl alcohol volume, peels off 0.5 ~ 100 hour, filters, and washes, removes Fe with the magnetic field separation equipment
2O
3Promptly finished peeling off to graphite intercalation compound.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake graphite FeCl
3Intercalation compound, productive rate is more than 90%.
The specific embodiment 46: the present embodiment efficient mechanical is peeled off the method for graphite and is finished by following step: one, take by weighing 1 part of graphite powder, 200 ~ 2000 parts of urea and 100 ~ 1000 parts of ethanol by weight percentage, put into graphite powder after under 60 ℃ of conditions, adding urea in the ethanol then, obtain mixture and place homogenizer, add polyacrylic acid (PAA) again, the polyacrylic acid consumption is 0.5% of an ethanol volume; Two, in 0.1 ~ 10 hour said mixture being cooled to 20 ℃ utilizes homogenizer to peel off with 1000 ~ 10000 rev/mins speed simultaneously; Three, be warming up to 60 ℃ then, in 0.1 ~ 10 hour, be cooled to 30 ℃ again and utilize sand mill to peel off simultaneously with 1000 ~ 10000 rev/mins speed; Four, the operation of repeating step two and step 3 is 0 ~ 9 time, continued mechanical stripping 0.1 ~ 100 hour, and obtained the mixture of Graphene-urea-ethanol, 35 ℃ ~ 55 ℃ filtrations, in environment heating more than 200 ℃ remaining urea is decomposed rapidly, promptly finished peeling off graphite.
Present embodiment obtains 1 ~ 10 layer a large amount of Graphenes, and thickness is in 0.355 ~ 5nm scope, and conductance is 10
3More than the S/cm, thermal conductivity is more than 2000W/mK, and its productive rate is more than 90%.
The specific embodiment 47: the present embodiment efficient mechanical is peeled off NbSe
2Method finish by following step: by weight percentage with 1 part of NbSe
2, 200 parts of about 200nm of diameter ZrO
2Be placed in the oscillating mill with 150 parts of acetone mixing, add softex kw (CTAB) then, the softex kw consumption is 2% of an acetone volume, peels off 0.5 ~ 100 hour, filter, wash, isolate zirconia powder with centrifuge; Promptly finished NbSe
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake NbSe
2, productive rate is more than 90%.
The specific embodiment 48: the method for present embodiment efficient mechanical peel montmorillonite is finished by following step: by weight percentage with the zirconia powder of 1 part of imvite, 200 parts of about 200nm of diameter and 500 part 1, the mixing of 4-butanediol is placed in the oscillating mill, add polyacrylic acid (PAA) again, the polyacrylic acid consumption is 1,2% of 4-butanediol volume, peeled off 0.5 ~ 100 hour, and filtered, wash, isolate zirconia powder with centrifuge; Promptly finished peeling off to imvite.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake imvites, and productive rate is more than 90%.
The specific embodiment 49: the present embodiment efficient mechanical is peeled off the method for Graphene and is finished by following step: 1 part of graphite oxide powder, 5 ~ 50 sodium chloride and 200 parts of PMAs are mixed being placed in the three-roller by weight percentage, add polyacrylic acid then, the polyacrylic acid consumption is 10% ~ 20% of a PMA volume, mechanical stripping 4 ~ 100 hours, dissolve PMA with butyl acetate, filter, water dissolving sodium chloride has promptly been finished peeling off graphite.
Present embodiment obtains 1 ~ 10 layer a large amount of Graphenes, and thickness is in 0.355 ~ 5nm scope, and conductance is 10
3More than the S/cm, thermal conductivity is more than 2000W/mK, and its productive rate is more than 90%.
The specific embodiment 50: the present embodiment efficient mechanical is peeled off MoS
2Method finish by following step: by weight percentage with 1 part of MoS
2, 100 parts of particle diameters are the ZrO of 200nm
2Be placed in the three-roller with 500 parts of PMAs mixing, add polyacrylic acid then, the polyacrylic acid consumption is 10% ~ 20% of a PMA volume, mechanical stripping 4 ~ 50 hours, dissolve PMA with butyl acetate, filter, washing, centrifugation ZrO
2Promptly finished MoS
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake MoS
2, productive rate is more than 90%.
The specific embodiment 51: the method for present embodiment efficient mechanical peel montmorillonite is finished by following step: be the ZrO of 200nm with 1 part of imvite, 150 parts of particle diameters by weight percentage
2With 500 part 1, the mixing of 3-butanediol is placed in the homogenizer, peels off 0.5 ~ 100 hour with 4000 rev/mins speed mechanical, filters washing, the centrifugal ZrO that removes
2Promptly finished peeling off to imvite.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake imvites, and productive rate is more than 92%.
The specific embodiment 52: efficient mechanical is peeled off the method for graphite oxide and is finished by following step: by weight percentage with 1 part of graphite oxide powder, 20-200 part CaCO
3Mixing is placed in the oscillating mill with 100-500 part isopropyl alcohol, and mechanical stripping 0.5 ~ 100 hour filters and obtains graphene oxide and CaCO
3Mixture, add mass percent concentration and be 10% ~ 30% HCl dissolving CaCO
3, washing, filtration; Promptly finished peeling off to graphite oxide.
The present embodiment method is peeled off graphite oxide, obtains graphene oxide, and resulting graphene oxide has individual layer or sandwich construction, and thickness is in 0.355 ~ 5nm scope, and its productive rate is more than 90%.
The specific embodiment 53: the present embodiment efficient mechanical is peeled off the method for graphite and is finished by following step: one, take by weighing 1 part of graphite powder, 80 ~ 200 parts of potassium dihydrogen phosphates and 100 ~ 400 parts of water by weight percentage, under 90 ℃ of conditions potassium dihydrogen phosphate being put into graphite powder after soluble in water, obtain mixture and place sand mill then; Two, in 0.1 ~ 10 hour said mixture being cooled to 20 ~ 50 ℃ utilizes sand mill to peel off with 1000 ~ 10000 rev/mins speed simultaneously; Three, be warming up to 90 ℃ then, in 0.1 ~ 10 hour, be cooled to 20 ~ 50 ℃ again and utilize sand mill to peel off simultaneously with 1000 ~ 10000 rev/mins speed; Four, the operation of repeating step two and step 3 is 0 ~ 20 time, continued mechanical stripping 0.1 ~ 100 hour, obtain the mixture of Graphene-potassium dihydrogen phosphate-water, add hot mixt to 100 ℃ (purpose is the dissolving phosphoric acid potassium dihydrogen), promptly finished peeling off after filtering, cleaning graphite.
The whole process of the described method of present embodiment is pollution-free, is the synthetic route of a green.
The present embodiment method is peeled off graphite, obtains Graphene, and resulting Graphene has individual layer or multilayer (2 ~ 10 layers) structure, and thickness is in 0.355 ~ 5nm scope, and conductance is 10
3More than the S/cm, thermal conductivity is more than 2000W/mK, and its productive rate is more than 90%.
The specific embodiment 54: the present embodiment efficient mechanical is peeled off MoS
2Method finish by following step: by weight percentage with 1 part of MoS
2, 50 ~ 1000 parts of NaCl and 500 ~ 5000 parts of ethanol mix and are placed in the homogenizer, peel off 0.5 ~ 100 hour with 4000 rev/mins speed, filter the back then and add 500 ~ 3000 parts of water (being used to dissolve NaCl), filter, water cleans; Promptly finished MoS
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake MoS
2, productive rate is more than 90%.
The specific embodiment 55: the present embodiment efficient mechanical is peeled off NbSe
2Method finish by following step: by weight percentage with 1 part of NbSe
2, 50 ~ 1000 parts of KCl and 250 ~ 2500 parts of ethanol and 250 ~ 2500 parts of glycerine mix and are placed in the homogenizer, peel off 0.5 ~ 100 hour with 4000 rev/mins speed, filter the back then and add 500 ~ 3000 parts of water (being used to dissolve KCl), filter, water cleans; Promptly finished NbSe
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake NbSe
2, productive rate is more than 90%.
The specific embodiment 56: the present embodiment efficient mechanical is peeled off kaolinic method and is finished by following step: by weight percentage with the Fe of 1 part of kaolin, 150 parts of about 2 μ m of diameter
2O
3Be placed in the oscillating mill with 100 parts of isopropyl alcohols mixing, mechanical stripping 0.5 ~ 100 hour filters the back and removes Fe with magnetic field classified filtering equipment
2O
3Promptly finished and peeled off kaolinic.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake kaolin, and productive rate is more than 90%.
The specific embodiment 57: the present embodiment efficient mechanical is peeled off graphite C uCl
2The method of intercalation compound is finished by following step: by weight percentage with 1 part of graphite C uCl
2The copper powder of intercalation compound, 100 parts of about 1 μ m of diameter and 200 parts of isopropyl alcohols mixing are placed in the oscillating mill, and mechanical stripping 0.5 ~ 100 hour filters, washing, centrifugal removal copper powder; Promptly finished graphite C uCl
2Peeling off of intercalation compound.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake graphite C uCl
2Intercalation compound, productive rate is more than 90%.
The specific embodiment 58: the present embodiment efficient mechanical is peeled off the method for graphite and is finished by following step: one, take by weighing 1 part of graphite powder, 200 ~ 2000 parts of urea and 100 ~ 1000 part 1 by weight percentage, the 3-butanediol, under 60 ℃ of conditions, urea is dissolved in 1 then, put into graphite powder after in the 3-butanediol, obtain mixture and place homogenizer; Two, in 0.1 ~ 10 hour said mixture being cooled to 20 ℃ utilizes homogenizer to peel off with 1000 ~ 10000 rev/mins speed simultaneously; Three, be warming up to 60 ℃ then, in 0.1 ~ 10 hour, be cooled to 30 ℃ again and utilize sand mill to peel off simultaneously with 1000 ~ 10000 rev/mins speed; Four, the operation of repeating step two and step 3 is 0 ~ 9 time, continues mechanical stripping 0.1 ~ 100 hour, obtains Graphene-urea-1, the mixture of 3-butanediol, 35 ℃ ~ 55 ℃ filtrations, in environment heating more than 200 ℃ urea is decomposed rapidly, promptly finished peeling off to graphite.
Present embodiment obtains 1 ~ 10 layer a large amount of Graphenes, and thickness is in 0.355 ~ 5nm scope, and conductance is 10
3More than the S/cm, thermal conductivity is more than 2000W/mK, and its productive rate is more than 90%.
The specific embodiment 59: the present embodiment efficient mechanical is peeled off NbSe
2Method finish by following step: by weight percentage with 1 part of NbSe
2, the silver powder of 300 parts of about 500nm of diameter and 150 parts of acetone mix and are placed in the oscillating mill, mechanical stripping 0.5 ~ 100 hour, centrifugal, filter; Promptly finished NbSe
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake NbSe
2, productive rate is more than 90%.
The specific embodiment 60: the method for present embodiment efficient mechanical peel montmorillonite is finished by following step: by weight percentage with the zirconia powder of 1 part of imvite, 200 parts of about 200nm of diameter and 500 part 1, the mixing of 4-butanediol is placed in the oscillating mill, mechanical stripping 0.5 ~ 100 hour, filter, wash, remove zirconia powder with centrifuge; Promptly finished peeling off to imvite.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake imvites, and productive rate is more than 90%.
The specific embodiment 61: the present embodiment efficient mechanical is peeled off the method for Graphene and is finished by following step: 1 part of graphite oxide powder, 10-100 sodium chloride and 10-500 part PMA are mixed being placed in the three-roller by weight percentage, mechanical stripping 4 ~ 50 hours, dissolve PMA with butyl acetate, filter, water dissolving sodium chloride has promptly been finished peeling off graphite.
Present embodiment obtains 1 ~ 10 layer a large amount of Graphenes, and thickness is in 0.355 ~ 5nm scope, and conductance is 10
3More than the S/cm, thermal conductivity is more than 2000W/mK, and its productive rate is more than 90%.
The specific embodiment 62: the present embodiment efficient mechanical is peeled off MoS
2Method finish by following step: by weight percentage with 1 part of MoS
2, 80 parts of particle diameters calcium carbonate that is 2 μ m and 300 parts of PMAs mix and are placed in the three-roller, mechanical stripping 4 ~ 100 hours dissolves PMA with butyl acetate, filters, and use diluted hydrochloric acid dissolution calcium carbonate, has promptly finished MoS after the centrifugal and filtration
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake MoS
2, productive rate is more than 90%.
The specific embodiment 63: the method for present embodiment efficient mechanical peeling layered compounds is undertaken by following step: in airslide disintegrating mill, with gas working dielectric and particle diameter is that the solid particle of 1nm ~ 100 μ m carries out mechanical stripping to lamellar compound, splitting time is removed solid particle then more than 5 minutes; Promptly finished peeling off to lamellar compound.
Present embodiment is utilized automation to peel off and is obtained 1 ~ 10 layer a large amount of nano flake lamellar compounds, and separates easily with abrasive media; Lamellar compound is far longer than the interaction of atom between layer and the layer in the covalent bonding intensity between the atom on the layer plane, and the mass of solid particles of present embodiment use is little, and same movement speed energy is lower, the covalent bond of survivable lamellar compound; Present embodiment is used a large amount of solid particles, in process of lapping can with collided by the abrasive grains high-frequency, thereby improve grinding efficiency greatly and guaranteed that the lattice of nano flake lamellar compound does not change; The solid particle of huge amount can disperse to help to solve the dispersion agglomeration traits of ultra-fine grain to by the particle of grinding superfine well.
The specific embodiment 64: what present embodiment and the specific embodiment 63 were different is: described gas working dielectric is air, He, Ne, Ar, N
2, H
2, Cl
2, Br
2, CO, CO
2, CH
4, NH
3, a kind of or wherein several mixing in the benzene vapor.Other step is identical with the specific embodiment 63 with parameter.
The described gas working dielectric of present embodiment is in the gaseous mixture, presses between all gases working media arbitrarily than mixing.
The specific embodiment 65: what present embodiment was different with the specific embodiment 63 or 64 is: described solid particle is a magnesium, aluminium, iron, cobalt, nickel, copper, zinc, silver, tin, vanadium, chromium, tungsten, copper alloy, aluminium alloy, kirsite, iron-carbon alloy, magnesium alloy, lithium alloy, boron oxide, silica, zirconia, aluminium oxide, calcium carbonate, magnesia, titanium dioxide, iodine, zinc oxide, tin oxide, di-iron trioxide, tri-iron tetroxide, aluminium nitride, aluminium chloride, titanium nitride, carborundum, sodium fluoride, ammonium fluoride, calcium oxide, carbonic hydroammonium, ammonium bromide, ammonium chromate, ammonium dihydrogen phosphate (ADP), ammonium formate, ammonium acetate, sodium acid carbonate, ammonium hydrogen phosphate, ammonium iodide, ammonium nitrate, ammonium oxalate, ammonium sulfate, ammonium sulfite, ammonium tartrate, ammonium thiocyanate, ammonium acetate, barium iodide, barium nitrate, calcium bromide, calcium iodide, calcium nitrate, calcium nitrite, potassium acetate, potassium bromate, KBr, potash, potassium chlorate, potassium chloride, potassium chromate, potassium bichromate, potassium dihydrogen phosphate, the potassium ferricyanide, potassium ferrocyanide, potassium fluoride, potassium formate, potassium acid sulfate, potassium hydroxide, KI, potassium nitrate, potassium oxalate, potassium sulfate, potassium thiosulfate, lithium acetate, lithium bromide, sodium chloride, lithium chloride, lithium formate, lithium iodide, aluminum nitrate, aluminum sulfate, magnesium acetate, magnesium bromide, magnesium iodide, magnesium sulfate, sodium acetate, sodium carbonate, sodium dihydrogen phosphate, sodium formate, sodium acetate, sodium nitrate, sodium phosphate, sodium sulphate, nickel chloride, nickel nitrate, frerrous chloride, ferrous sulfate, iron chloride, copper chloride, copper nitrate, copper sulphate, zinc sulfate, sucrose, urea, polymer microsphere, a kind of or wherein several mixing in the glass dust.Other step is identical with the specific embodiment 63 or 64 with parameter.
When the present embodiment solid particle is mixture, press between various solid particles arbitrarily than mixing.Above-mentioned solid particle can adopt following method to remove respectively according to its character:
The first kind: can be dissolved in the solid particle of acid, aqueous slkali, for example: Al, Cu, Zn, SnO, ZnO, B
2O
3, SiO
2, NaHCO
3, CaCO
3, CaO etc., can remove by pickling or alkali cleaning;
Second class: room temperature-high temperature (for example 100 ℃) solubility with temperature changes material greatly, for example: carbonic hydroammonium, ammonium dihydrogen phosphate (ADP), ammonium oxalate, potassium dihydrogen phosphate, potassium chloride, potassium ferrocyanide, potassium sulfate, sodium carbonate, sodium dihydrogen phosphate, sodium sulphate, sodium phosphate, sucrose, urea, adopt low-temperature working then to heat up the solid particle dissolving removed;
The 3rd class: the very big material of dissolubility difference in different solvents, for example: most of ionic compounds are (as NaCl, K
2CO
3, KCl, AlCl
3) solubility is big and at ethanol, benzene, CCl in water
4Less Deng solubility in the organic solvent, adopt and in organic working media, to work and the method for after washing is removed;
The 4th class: segregative material under electric field, magnetic field effect, for example: Al
2O
3, CaCO
3, Fe
2O
3, Fe
3O
4, Fe etc., remove by electric field, magnetic field, as removing with static classified filtering equipment or magnetic field separation equipment;
The 5th class: volatile, the distillation of high temperature when heating, decompose the solid particle of removing, as sucrose, I
2, urea, NH
4NO
3, NH
4HCO
3, CH
3COONH
4Deng, adopt the way of high temperature heating to remove;
The 6th class: heavy solid particle, as zirconia, vanadium, chromium, tungsten etc., (telling 20-2 μ m as linear vibrating screen classifying equipoment, gas flow sizing machine removes with thin micro mist, tripod pendulum type batch centrifugal-SS450, multistage grader (step Electronics Co., Ltd. is opened in Shenzhen) to adopt the classification separation equipment.
Concrete like embodiment 66: what present embodiment was different with one of specific embodiment 63 to 65 is: the weight ratio 1:0.1 of layered compound and solid particle ~ 10000.Other step is identical with one of specific embodiment 63 to 65 with parameter.
The specific embodiment 67: what present embodiment and the specific embodiment 66 were different is: the weight ratio 1:1 of layered compound and solid particle ~ 2000.Other step is identical with the specific embodiment 66 with parameter.
The specific embodiment 68: what present embodiment and the specific embodiment 66 were different is: the weight ratio 1:5 of layered compound and solid particle ~ 1000.Other step is identical with the specific embodiment 66 with parameter.
The specific embodiment 69: what present embodiment and the specific embodiment 66 were different is: the weight ratio 1:10 of layered compound and solid particle ~ 500.Other step is identical with the specific embodiment 66 with parameter.
The specific embodiment 70: what present embodiment and the specific embodiment 66 were different is: the weight ratio 1:100 of layered compound and solid particle ~ 200.Other step is identical with the specific embodiment 66 with parameter.
The specific embodiment 71: what present embodiment was different with one of the specific embodiment and specific embodiment 63 to 70 is: the particle diameter of described solid particle is 5nm ~ 100nm.Other step is identical with one of specific embodiment 63 to 70 with parameter.
The specific embodiment 72: what present embodiment and the specific embodiment and the specific embodiment 71 were different is: the particle diameter of described solid particle is 200nm ~ 500nm.Other step is identical with the specific embodiment 71 with parameter.
The specific embodiment 73: what present embodiment and the specific embodiment and the specific embodiment 71 were different is: the particle diameter of described solid particle is 1 μ m ~ 20 μ m.Other step is identical with the specific embodiment 71 with parameter.
The specific embodiment 74: what present embodiment and the specific embodiment and the specific embodiment 71 were different is: the particle diameter of described solid particle is 50 μ m ~ 80 μ m.Other step is identical with the specific embodiment 71 with parameter.
The specific embodiment 75: the present embodiment efficient mechanical is peeled off the method for Graphene and is finished by following step: in airslide disintegrating mill, the silica that with nitrogen and particle diameter is 7nm carries out mechanical stripping to 1 part of graphite powder, silica and graphite powder mass ratio are 4 ~ 10:1, and the adding mass percent concentration is 5% HF dissolving SiO
2, filter; Promptly finished peeling off to graphite.
Present embodiment obtains 1 ~ 10 layer a large amount of Graphenes, and thickness is in 0.355 ~ 5nm scope, and conductance is 10
3More than the S/cm, thermal conductivity is more than 2000W/mK, and its productive rate is more than 90%.
The specific embodiment 76: the method for present embodiment efficient mechanical peel montmorillonite is finished by following step: in airflow milling, be the Fe of 7nm ~ 1 μ m with nitrogen and particle diameter
2O
3Imvite was carried out mechanical stripping 0.1 ~ 20 hour, Fe
2O
3With the imvite mass ratio be 40 ~ 1000:1, utilize static classified filtering equipment or magnetic field separation equipment to remove Fe then
2O
3Promptly finished peeling off to imvite.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake imvites, and productive rate is more than 90%.
The specific embodiment 77: the present embodiment efficient mechanical is peeled off the method for graphite oxide and is finished by following step: in airflow milling, be the Fe of 5 μ m with nitrogen and particle diameter
2O
3The graphite oxide powder was carried out mechanical stripping 0.1 ~ 20 hour, Fe
2O
3With graphite oxide powder mass ratio be 400:1, utilize the magnetic field separation equipment to remove Fe then
2O
3Promptly finished peeling off to graphite oxide.
Present embodiment obtains 1 ~ 10 layer a large amount of graphene oxides, and thickness is in 0.355 ~ 5nm scope, and its productive rate is more than 90%.
The specific embodiment 78: the present embodiment efficient mechanical is peeled off the method for graphite oxide and is finished by following step: in airflow milling, with argon gas and urea graphite oxide was carried out mechanical stripping 0.1 ~ 20 hour, urea and graphite oxide mass ratio are 200 ~ 2000:1, washing, filtration add heat abstraction residual urine element then under 160 ~ 200 ℃ of conditions; Promptly finished peeling off to graphite oxide.
Present embodiment obtains 1 ~ 10 layer a large amount of graphite oxide nano flakes, and productive rate is more than 90%.
The specific embodiment 79: the present embodiment efficient mechanical is peeled off MoS
2Method finish by following step: in airflow milling, with air and the CaCO of humidity more than 90%
3To MoS
2Carried out mechanical stripping 0.1 ~ 20 hour, CaCO
3And MoS
2Mass ratio is 200 ~ 2000:1, and mass percent concentration is 10% ~ 30% HCl dissolving CaCO then
3, washing, filtration; Promptly finished MoS
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake MoS
2, productive rate is more than 90%.
The AAA specific embodiment 80: the present embodiment efficient mechanical is peeled off NbSe
2Method finish by following step: in airflow milling, with helium and potassium dihydrogen phosphate to NbSe
2Carried out mechanical stripping 0.1 ~ 20 hour, potassium dihydrogen phosphate and NbSe
2Mass ratio is 200 ~ 2000:1, and heating is 100 ℃ after the adding suitable quantity of water, filters the back and cleans; Promptly finished NbSe
2Peel off.
The AAA present embodiment obtains 1 ~ 10 layer a large amount of nano flake NbSe
2, productive rate is more than 90%.
The specific embodiment 81: the present embodiment efficient mechanical is peeled off the method for hexagonal boron nitride and is finished by following step: in airflow milling, with nitrogen and sucrose hexagonal boron nitride was carried out mechanical stripping 0.1 ~ 20 hour, sucrose and hexagonal boron nitride mass ratio are 500 ~ 1000:1, be heated to 100 ℃ after adding water, filter the back and clean; Promptly finished peeling off to hexagonal boron nitride.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake hexagonal boron nitrides, and productive rate is more than 90%.
The specific embodiment 82: the present embodiment efficient mechanical is peeled off kaolin (Al
2Si
2O
5(OH)
4) method finish by following step: in airflow milling, with nitrogen and NaCl kaolin was carried out mechanical stripping 0.5 ~ 20 hour, NaCl and kaolin mass ratio are 500 ~ 1000:1, add 500 ~ 3000 parts of water (being used to dissolve NaCl), filter, water cleans 3 ~ 5 times; Promptly finished and peeled off kaolinic.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake kaolin, and productive rate is more than 90%.
The specific embodiment 82: the method for present embodiment efficient mechanical peel montmorillonite is finished by following step: in airflow milling, with nitrogen and KCl imvite was carried out mechanical stripping 0.5 ~ 20 hour, KCl and imvite mass ratio are 500 ~ 1000:1, add 500 ~ 3000 parts of water (being used to dissolve KCl), filter, water cleans 3 ~ 5 times; Promptly finished peeling off to imvite.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake imvites, and productive rate is more than 90%.
The specific embodiment 82: the present embodiment efficient mechanical is peeled off the method for graphite oxide and is finished by following step: in airflow milling, with nitrogen and Al
2O
3The graphite oxide powder was carried out mechanical stripping 0.5 ~ 20 hour, Al
2O
3With the graphite powder mass ratio be 50 ~ 1000:1, utilize static classified filtering equipment to remove Al
2O
3Promptly finished peeling off to graphite oxide.
Present embodiment obtains 1 ~ 10 layer a large amount of graphene oxides, and thickness is in 0.5 ~ 5nm scope, and its productive rate is more than 90%.
The specific embodiment 83: the present embodiment efficient mechanical is peeled off the method for hexagonal boron nitride and is finished by following step: in airflow milling, with argon gas and iron powder hexagonal boron nitride was carried out mechanical stripping 0.5 ~ 20 hour, iron powder and hexagonal boron nitride mass ratio are 10 ~ 2000:1, remove iron powder with the magnetic field separation equipment; Promptly finished peeling off to hexagonal boron nitride.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake hexagonal boron nitrides, and productive rate is more than 90%.
The specific embodiment 84: the present embodiment efficient mechanical is peeled off the method for hexagonal boron nitride and is finished by following step: in airflow milling, with nitrogen and urea hexagonal boron nitride was carried out mechanical stripping 0.5 ~ 20 hour, urea and hexagonal boron nitride mass ratio are 10 ~ 1000:1, peeling off hexagonal boron nitride promptly finished in washing, filtration.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake hexagonal boron nitrides, and productive rate is more than 90%.
The specific embodiment 85: this enforcement efficient mechanical is peeled off NbSe
2Method finish by following step: in airflow milling, with nitrogen and Al
2O
3To NbSe
2Carried out mechanical stripping 0.5 ~ 20 hour, Al
2O
3And NbSe
2Mass ratio is 50 ~ 1000:1, removes Al with the static grader
2O
3Powder; Promptly finished NbSe
2Peel off.
Present embodiment obtains 1 ~ 10 layer a large amount of nano flake NbSe
2, productive rate is more than 90%.
The specific embodiment 86: this enforcement efficient mechanical is peeled off the method for graphite and is finished by following step: in airflow milling, with air and the zirconia powder of humidity more than 90% the Graphene powder was carried out mechanical stripping 0.5 ~ 20 hour, zirconia powder and graphite powder mass ratio are 50 ~ 1000:1, remove zirconia powder with the flow separation machine; Promptly finished peeling off to graphite.
Present embodiment obtains 1 ~ 10 layer a large amount of Graphenes, and thickness is in 0.355 ~ 5nm scope, and conductance is 10
3More than the S/cm, productive rate is more than 90%.
Claims (11)
1. the method for efficient mechanical peeling layered compounds, the method that it is characterized in that the efficient mechanical peeling layered compounds realizes by following step: with lamellar compound, particle diameter is to carry out mechanical stripping after the solid particle of 1nm ~ 100 μ m and liquid-working-medium mix, splitting time is more than 5 minutes, and liquid-working-medium is that 10 ~ 73mN/m and viscosity are 1 ~ 1 * 10 at the operating temperature lower surface tension force of mechanical stripping
9MPas separates then and removes solid particle and liquid-working-medium; Promptly finished peeling off to lamellar compound; Wherein add dispersant in the mechanical stripping process, dispersant dosage is 0 ~ 20% of a liquid-working-medium.
2. the method for efficient mechanical peeling layered compounds according to claim 1 is characterized in that described solid particle is a magnesium, aluminium, iron, cobalt, nickel, copper, zinc, silver, tin, vanadium, chromium, tungsten, copper alloy, aluminium alloy, kirsite, iron-carbon alloy, magnesium alloy, lithium alloy, boron oxide, silica, zirconia, aluminium oxide, calcium carbonate, magnesia, titanium dioxide, iodine, zinc oxide, tin oxide, di-iron trioxide, tri-iron tetroxide, aluminium nitride, aluminium chloride, titanium nitride, carborundum, sodium fluoride, ammonium fluoride, calcium oxide, carbonic hydroammonium, ammonium bromide, ammonium chromate, ammonium dihydrogen phosphate (ADP), ammonium formate, ammonium acetate, ammonium acetate, sodium acid carbonate, ammonium hydrogen phosphate, ammonium iodide, ammonium nitrate, ammonium oxalate, ammonium sulfate, ammonium sulfite, ammonium tartrate, ammonium thiocyanate, ammonium acetate, barium iodide, barium nitrate, calcium bromide, calcium iodide, calcium nitrate, calcium nitrite, potassium acetate, potassium bromate, KBr, potash, potassium chlorate, potassium chloride, potassium chromate, potassium bichromate, potassium dihydrogen phosphate, the potassium ferricyanide, potassium ferrocyanide, potassium fluoride, potassium formate, potassium acid sulfate, potassium hydroxide, KI, potassium nitrate, potassium oxalate, potassium sulfate, potassium thiosulfate, lithium acetate, lithium bromide, sodium chloride, lithium chloride, lithium formate, lithium iodide, aluminum nitrate, aluminum sulfate, magnesium acetate, magnesium bromide, magnesium iodide, magnesium sulfate, sodium acetate, sodium carbonate, sodium dihydrogen phosphate, sodium formate, sodium acetate, sodium nitrate, sodium phosphate, sodium sulphate, nickel chloride, nickel nitrate, frerrous chloride, ferrous sulfate, iron chloride, copper chloride, copper nitrate, copper sulphate, zinc sulfate, sucrose, urea, polymer microsphere, a kind of or wherein several mixing of glass dust.
3. want the method for 2 described efficient mechanical peeling layered compounds according to right, it is characterized in that weight ratio 1:0.1 ~ 10000 of layered compound and solid particle, the weight ratio 1:0.1 of described solid particle and liquid-working-medium ~ 10000.
4. want the method for 3 described efficient mechanical peeling layered compounds according to right, it is characterized in that the surface tension 40 ~ 50mN/m of described liquid-working-medium.
5. want the method for 4 described efficient mechanical peeling layered compounds according to right, the viscosity that it is characterized in that described liquid-working-medium is 100 ~ 500000mPas.
6. according to the method for the described efficient mechanical peeling layered compounds of each claim of claim 1-5, it is characterized in that adopting in homogenizer, colloid mill, three-roller, screw extruder, ball mill, pan-milling machine, sand mill, oscillating mill and the ultrasonic device a kind of or wherein several logotype to carry out mechanical stripping; Described liquid-working-medium is the aqueous solution, the alcoholic solution of alkanes, the alcoholic solution of ketone, the aqueous solution of amine or the alkane solution of aromatic compound of water, alcohols, aromatic compound, ketone, amine, ionic liquid, alkanes, heterocyclic compound, carbon disulfide, carbon tetrachloride, gasoline, vegetable oil, diesel oil, wax, alcohol.
7. according to the method for the described efficient mechanical peeling layered compounds of claim 6, it is characterized in that described alcohols is ethanol, normal propyl alcohol, n-butanol, ethylene glycol, propane diols, 1,2-butanediol, 1,3-butanediol, 1, a kind of or wherein several mixing in 4-butanediol, glycerine and the isopropyl alcohol; Described aromatic compound is benzene, toluene, naphthalene or anthracene; Described ketone is acetone or Ν-methyl pyrrolidone; Described amine is N-NMF, N, dinethylformamide or N, N-DEF; Described ionic liquid is 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole hexafluorophosphate or 1-ethoxy-3-methyl hexafluorophosphate; Described alkanes is n-hexane, octane or decane; Described heterocyclic compound is furans or pyridine; Alcohol is methyl alcohol, ethanol, glycerine, butanediol or isopropyl alcohol in the aqueous solution of described alcohol; The alcoholic solution of described alkanes is the octanol solution of n-hexane, the decyl alcohol solution of n-hexane or the decyl alcohol solution of octadecane; The alcoholic solution of described ketone is the butanediol solution of acetone or the ethanolic solution of acetone; Amine in the aqueous solution of described amine is N-NMF solution or N, dinethylformamide solution; The alkane solution of described aromatic compound is the hexane solution of benzene or the hexane solution of toluene.
8. according to the method for the described efficient mechanical peeling layered compounds of each claim of claim 1-5, it is characterized in that adopting mill, banbury, homogenizer, colloid mill, three-roller or screw extruder to carry out mechanical stripping, described liquid-working-medium is a macromolecular compound.
9. the method for described according to Claim 8 efficient mechanical peeling layered compounds is characterized in that described macromolecular compound polyacrylate, polyvinyl alcohol, polyethylene glycol, polyvinyl acetate, starch, polybutadiene, poly-butylbenzene diene, epoxy resin, rubber or pitch.
10. the method for efficient mechanical peeling layered compounds, the method that it is characterized in that the efficient mechanical peeling layered compounds is undertaken by following step: in airslide disintegrating mill, with gas working dielectric and particle diameter is that the solid particle of 1nm ~ 100 μ m carries out mechanical stripping to lamellar compound, splitting time is removed solid particle then more than 5 minutes; Promptly finished peeling off to lamellar compound.
11., it is characterized in that described gas working dielectric is air, He, Ne, Ar, N according to the method for the described efficient mechanical peeling layered compounds of claim 10
2, H
2, Cl
2, Br
2, CO, CO
2, CH
4, NH
3, a kind of or wherein several mixing in the benzene vapor.
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|---|---|---|---|
| CN201010179151A CN101857195A (en) | 2010-05-21 | 2010-05-21 | Efficient mechanical method for peeling layered compounds |
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