CN109179386A - A kind of minuent stannic oxide/graphene nano lamella powder and the preparation method and application thereof - Google Patents
A kind of minuent stannic oxide/graphene nano lamella powder and the preparation method and application thereof Download PDFInfo
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- CN109179386A CN109179386A CN201811198112.7A CN201811198112A CN109179386A CN 109179386 A CN109179386 A CN 109179386A CN 201811198112 A CN201811198112 A CN 201811198112A CN 109179386 A CN109179386 A CN 109179386A
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
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Abstract
A kind of minuent stannic oxide/graphene nano lamella powder and the preparation method and application thereof, graphite powder is mixed with oxidant and dispersing aid and grinds the few lamella large scale low degree of oxidation stannic oxide/graphene nano lamella powder of preparation, referred to as low oxidizability stannic oxide/graphene nano lamella powder, the thickness of obtained dry powder-shaped nanometer minuent graphene oxide layer is in 2.35~2.75nm, slice plane is having a size of 1.3~2.5 μm, oxygen content is 8.5~12.8%, and specific surface area is 261~287m2/ g, thermal coefficient is 1326~1852W/ (mK), it is mainly used in the activeness and quietness of cement-based material and improves heating conduction, volume is the 1.5~3.5% of cement powder quality, compression strength, flexural strength and the thermal conductivity ratio control sample of 28 day age cement-based material are respectively increased not less than 39%, 54% and 300%, and impermeabilisation, freeze thawing resistance and the resisting carbonization of concrete have reached best rank.The advantages that preparation method of the invention has material cheap and easy to get, and process route is reasonable, easy to operate, and preparation process is pollution-free, and economic results in society are significant.
Description
Technical field
The present invention relates to a kind of stannic oxide/graphene nano materials, and in particular to it is a kind of using ball-milling method prepared from graphite powder it is low
Spend stannic oxide/graphene nano lamella raw powder's production technology and application.
Technical background
Graphene oxide is a kind of nanoscale sheet layer material, has similar structure and performance, graphite oxide with graphene
Alkene also has big specific surface area, superpower mechanical property, good heating conduction and nano effect, it is made to adsorb, urge
Change, bioanalysis detection, medical carrier, photoelectric material and composite material etc. extensive application.The system of graphene oxide
Preparation Method has tri- kinds of methods of Brodie, Staudenmaier and Hummers, and preparation principle is all for example dense with inorganic strong protonic acid
Strong acid small molecule is inserted into graphite layers by sulfuric acid, fuming nitric aicd etc. fibrous gypsum ink, then with strong oxidizer such as potassium permanganate, chlorine
Sour potassium aoxidizes it.The advantages of most common Hummers method, this method is can to obtain high oxidation degree oxidation stone
Black alkene can regulate and control degree of oxidation and lamella size.But the shortcomings that these methods is low efficiency, pollution is big, generates
The quantity of waste acid water is big, causes the price of graphene oxide very high.Meanwhile different application field is for the structure of graphene oxide
There is different requirements, therefore, research and development high efficiency, low cost, low pollution preparation are suitable for the oxygen that application field requires
Graphite alkene is current research hotspot and there is an urgent need to technologies.
Currently, application of the graphene oxide in cement-base composite material is subject to the people's attention, graphene oxide is used
In the knot that the main function of cement-based material is by the template effect regulation hydrolysis product of cement of stannic oxide/graphene nano lamella
Structure and aggregated structure promote cement-based material to form the structure of regular even compact, can be improved the intensity of cement-based material
With toughness can, can reduce or eliminate the crack as caused by structure non-uniform convergent-divergent, leakage the problems such as, this side
Face it is desirable that high oxidation degree graphene oxide (oxygen content be greater than 30%), generally prepared by Hummers method.Cement base
The main problem that material always exists is crack and brittleness, and the main reason for generating crack is to be not easy to distribute by hydration heat of cement
Caused by crack, the thermal coefficient of concrete is the left and right 1.6W/ (mK), and the thermal coefficient 401W/ (mK) of metallic copper, water exists
27 DEG C of thermal coefficient is 0.6084W/ (mK).Graphene is the best Heat Conduction Material of current heating conduction, and thermal coefficient reaches
5300W/ (mK) has been arrived, by the graphene-doped thermal coefficient that concrete can be improved, has improved the dispersion of hydration heat of cement
And eliminate crack caused by the heat of hydration.But graphene is hydrophobic nano material, can not mix and be evenly dispersed into cement base
In body and good uniform dispersion is formed, and stannic oxide/graphene nano lamella has hydrophily, it can be in the mix system of concrete
During standby in incorporation cement matrix.Graphene oxide due in oxidation process to six side's honeycomb crystal structure knots of graphene
Structure produces partial destruction, and the thermal conductivity of graphene oxide decreases compared with graphene thermal conductivity, and oxygen content is 35.21% He
The thermal conductivity of 16.21% graphene oxide membrane is respectively 36W/ (mK) and 373W/ (mK), the reason is that passing through Hummers
Method preparation process, which is its oxidant, produces biggish destruction for the two-dimentional perfect cystal structure of graphene, more on lamella
Oxygen-containing group and small size make its thermal resistance very big.Graphene oxide is in cement-based material for regulating and controlling hydrated product structure
Oxidizability is high, and volume is generally 0.03% or so, and volume is smaller, continuous thermal conducting path cannot be formed, for cement-based material
Thermal coefficient influence it is little.The heating conduction of cement-based material is improved it is necessary to improve the volume of graphene oxide, is passed through
Hummers method prepares graphene oxide, and the problem of environmental pollution and price generated cannot achieve.Therefore, it is necessary to seek
The preparation method of new low degree of oxidation graphene oxide.
Summary of the invention
The purpose of the present invention is to provide it is a kind of it is cheap, generation efficiency is high, pollution-free, be capable of the minuent of mass production
Stannic oxide/graphene nano lamella powder and preparation method and application, is applied to cement-base composite material, is remarkably improved
The density and durability of cement-base composite material microstructure.
In order to achieve the above objectives, the invention patent provides low stannic oxide/graphene nano lamella raw powder's production technology,
90~120 parts of graphite powder, 6~9 parts of grinding aid, 8~12 parts of dispersing aid ball milling in-tank mixing is put by mass fraction to grind
14~16 parts of oxidant, 2~3 parts of oxidation promoter is added after grinding 1 hour in mill, then obtains being low within 20 hours continuing grinding
Spend stannic oxide/graphene nano lamella powder.
The partial size of the graphite powder is 13~15 μm, and carbon content is not less than 99.5%.
The oxidant is that potassium chlorate, potassium peroxydisulfate and potassium bichromate are mixed by mass parts 5:5:6.
The oxidation promoter is brown lead oxide or cobalt trifluoride.
The dispersing aid is powdery polycarboxylic acid water-reducing agent, and solid polycarboxylic acid water reducing agent content is aqueous not less than 99.5%
Rate is not more than 2%, and fineness is that average grain diameter is 35 μm, and water-reducing rate is not less than 30%.
The grinding aid is mixed by silicon powder and steel-making slag powder by the mass ratio of 1:2, and wherein the partial size of silicon powder is 2~10
μm, specific surface area is not less than 3000m2/ kg, dioxide-containing silica are greater than 90%；Steel-making slag powder is the slag of steel mill generation through grinding
Mill gained, partial size are 2~10 μm, and specific surface area is not less than 3000m2/ kg, sulfur trioxide content are not more than 4.0%.
The milling apparatus is high-energy planetary formula ball mill, and ball grinder is stainless cylinder of steel, and abrading-ball is GCr15 exceptional hardness alloy
Abrading-ball, ratio of grinding media to material example be 8:1,300 revs/min of rotational speed of ball-mill.
It is 2.35~2.75nm by minuent stannic oxide/graphene nano lamella powder lamellar spacing made of method made above,
For slice plane having a size of 1.3~2.5 μm, oxygen content is 8.5~12.8%, and specific surface area is 261~287m2/ g, thermal coefficient
For 1326~1852W/ (mK).
By the application of minuent stannic oxide/graphene nano lamella powder made of method made above, prepared by cement-based material
Method, low stannic oxide/graphene nano lamella powder volume are the 1.5~3.5% of cement silty amount, are mixed in mix process low
Degree stannic oxide/graphene nano lamella powder stirs evenly, the compression strength of 28 day age cement-based material, flexural strength and thermally conductive
Coefficient is improved than control sample respectively is not less than 39%, 54% and 300%.
The present invention has prepared few lamella by grinding graphite powder and oxidant, oxidation promoter and dispersing aid mixture
The stannic oxide/graphene nano lamella powder that large scale, two dimensional crystal structure are relatively complete, thermally conductive, electrical conductivity is high has price
It is cheap, generation efficiency is high, pollution-free, can with mass production, can larger amount of incorporation cement-based material, improve cement-based material
Heating conduction, eliminate the crack as caused by the uneven dispersion of hydration heat of cement.
The present invention is promoted under the mechanical force of process of lapping by mixing graphite powder with oxidant and dispersing aid
Physical and chemical changes occur for graphite, obtain few lamella large scale minuent stannic oxide/graphene nano lamella powder, lamellar spacing
In 2.35~2.75nm, planar dimension is 1.3~2.5 μm, while a small amount of carboxyl, hydroxyl and epoxy group are produced on lamella etc.
Chemical group, can be compatible with water phase and be uniformly distributed therein, and is mainly used in activeness and quietness and the increase of cement-based material
The microcrack unevenly generated by aquation heat partition is eliminated in the dispersion of hydration heat of cement.Its advantage is that environmental pollution very little, valence
Lattice are cheap, can largely generate, and can increase the volume in cement matrix, while realizing activeness and quietness and improving cement matrix point
The function of the bulk cement heat of hydration, the material that the invention patent preparation method is related to are easy to get, and process route is reasonable, operation side
Just, the advantages that preparation process is pollution-free, cheap.
Compared with prior art, beneficial effects of the present invention:
(1) efficient to be prepared for few lamella large scale minuent stannic oxide/graphene nano lamella powder, preparation process pollution
Small, the low stannic oxide/graphene nano lamella powder of preparation is cheap with respect to Hummers method, is suitable for prepare with scale and life
It produces, can be applied in cement-based material with biggish volume.
(2) significantly improve the heating conduction of cement-based material, can conduct in time, eliminate hydration heat of cement, eliminate because
Aquation heat accumulation disperses the crack unevenly generated.The thermal conductivity that graphene oxide layer powder obtained by the method for the present invention has had
Can, thermal coefficient is 1326~1852W/ (mK), and the thermal coefficient of concrete, Neng Gouji can be improved after incorporation cement matrix
The heat that time-division bulk cement aquation generates, eliminate due to aquation thermal diffusion it is uneven not in time caused by crack.
(3) have the function of that apparent activeness and quietness, low stannic oxide/graphene nano lamella powder have in cement matrix
There is strong active force between some filling effects and nanometer size effect, with cement matrix, have and promote cement-based material shape
At the ability of uniformly densely structure.It is anti-that active oxygen-containing group on simultaneous oxidation graphene sheet layer can participate in hydrated cementitious
It answers, itself becomes a part in cement matrix and structure, plays the effect of activeness and quietness.
(4) the method for the present invention is pollution-free in production process, prepares graphene oxide sheet from graphite powder using dry ball milling method
Layer powder, the graphite powder and oxidant of addition, oxidation promoter, dispersing aid etc. are completely converted into product, without exhaust gas, waste water,
The generation of waste residue.
(5) graphene oxide of the method for the present invention preparation is cheap, is suitable for large-scale in cement-based material production
It uses.The cost of the graphene oxide prepared by Hummers method is at 300,000 yuan/ton or so, the oxidation of the method for the present invention preparation
The cost of graphene is 1.5 ten thousand yuan/ton or so, if according to 1.5~3.5% incorporations of cement powder amount, every cubic metre of coagulation
Cement amount is calculated according to 450 kilograms in soil, and the cost of the graphene oxide of incorporation Hummers method production is about 2025~4725
Member or so, and the cost for the graphene oxide layer powder for using ball grinding method of the present invention to produce is 101.25~236.25 yuan of left sides
The right side, therefore the price advantage of the method for the present invention is obvious.
Specific embodiment
The present invention is described in detail With reference to embodiment, so that advantage of the invention is easier to by ability
Field technique personnel understand, but the protection scope being not intended to restrict the invention.
Embodiment 1:
90 parts of graphite powder, 6 parts of grinding aid, 8 parts of dispersing aid are put into mixed grinding in ball grinder by mass fraction, are ground
14 parts of oxidant, 2 parts of oxidation promoter is added in mill after 1 hour, then continuing grinding to obtain within 20 hours lamellar spacing to be 2.35nm,
Slice plane is having a size of 1.3 μm, oxygen content 8.5%, specific surface area 261m2/ g, thermal coefficient are 1326W/ (mK)
Low stannic oxide/graphene nano lamella powder.It the results are shown in Table 1 applied to cement-base composite material.
The partial size of the graphite powder of the present embodiment is 13~15 μm, and carbon content is not less than 99.5%；The oxidant is chlorine
Sour potassium, potassium peroxydisulfate and potassium bichromate are mixed by mass parts 5:5:6；The oxidation promoter is brown lead oxide or borontrifluoride
Cobalt；The dispersing aid is powdery polycarboxylic acid water-reducing agent, and solid polycarboxylic acid water reducing agent content is not less than 99.5%, and moisture content is little
In 2%, fineness is that average grain diameter is 35 μm, and water-reducing rate is not less than 30%；The grinding aid is by silicon powder and steel-making slag powder by 1:2's
Mass ratio is mixed, and wherein the partial size of silicon powder is 2~10 μm, and specific surface area is not less than 3000m2/ kg, dioxide-containing silica are big
In 90%；Steel-making slag powder is the ground gained of slag that steel mill generates, and partial size is 2~10 μm, and specific surface area is not less than 3000m2/
Kg, sulfur trioxide content are not more than 4.0%；The ball milling is high-energy planetary formula ball mill, and ball grinder is stainless cylinder of steel, and abrading-ball is
GCr15 exceptional hardness Alloy Balls In Milling, ratio of grinding media to material example be 8:1,300 revs/min of rotational speed of ball-mill.
Embodiment 2:
100 parts of graphite powder, 8 parts of grinding aid, 10 parts of dispersing aid are put into mixed grinding in ball grinder by mass fraction,
15 parts of oxidant, 2.5 parts of oxidation promoter is added after grinding 1 hour, then exists continuing grinding and obtain lamellar spacing in 20 hours
2.53nm, slice plane is having a size of 1.9 μm, oxygen content 9.6%, specific surface area 275m2/ g, thermal coefficient 1685W/
(mK) low stannic oxide/graphene nano lamella powder.Other are the same as embodiment 1.
It the results are shown in Table 1 applied to cement-base composite material.
Embodiment 3:
120 parts of graphite powder, 9 parts of grinding aid, 12 parts of dispersing aid are put into mixed grinding in ball grinder by mass fraction,
16 parts of oxidant, 3 parts of oxidation promoter is added after grinding 1 hour, then exists continuing grinding and obtain lamellar spacing in 20 hours
2.75nm, slice plane is having a size of 2.5 μm, oxygen content 12.8%, specific surface area 287m2/ g, thermal coefficient are
The low stannic oxide/graphene nano lamella powder of 1852W/ (mK).Other are the same as embodiment 1.
It the results are shown in Table 1 applied to cement-base composite material.
1 embodiment sample application result of table
As can be seen from the results in the table that cement-based material sample prepared by the present invention, the cement-based material tool of 28 day age
There are good heating conduction, compression strength and flexural strength and control sample more to increase significantly, illustrates this patent
The nanoscale graphene sheet layer powder of method preparation has good activeness and quietness for cement matrix and improves thermal conductivity
The effect of energy, the performances such as anti-water penetration, freeze thawing resistance, anti-carbonation have reached best level, illustrate the cement based specimen of preparation
Free from flaw and seepage defect.
Cement-base composite material preparation: P.O42.5 ordinary portland cement, low stannic oxide/graphene nano lamella powder,
Water, solid polycarboxylic acid water reducing agent mass parts ratio be 100:1.5:30:0.3, conserved according to standard method.
Detection method: " Technology of Steady State Thermal Resistance of Thermal Insulating Material and measurement in relation to characteristic are anti-according to GB10294-1988 for thermal coefficient
Guarded hot plate method " it is tested.Compression strength and flexural strength are according to GB50107-2010 " Standard for inspection and assessment of strength of concrete "
Method carries out.Water resistant permeability is carried out according to GB/T50082-2009 method, sample sizeOsmotic pressure
Power 3.5MPa, pressing time 48h.Freezing and thawing performance according to JTG E30-2005, " test by highway engineering cement and cement concrete
Regulation " it carries out, using the anti-freezing property for being rapidly frozen testing machine measurement concrete, a Frozen-thawed cycled lasts 2~5h, freeze thawing temperature
- 18 DEG C of degree, specimen size 100mm × 100mm × 500mm.Sample be carbonized according to GB/T50082-2009 method " normal concrete
Long-term behaviour and endurance quality test method standard " it is tested, specimen size 100mm × 100mm × 100mm.
Claims (9)
1. a kind of minuent stannic oxide/graphene nano lamella raw powder's production technology, it is characterised in that: press mass fraction for graphite powder
90~120 parts, 6~9 parts of grinding aid, 8~12 parts of dispersing aid be put into mixed grinding in ball grinder, grinding is added after 1 hour
Then 14~16 parts of oxidant, 2~3 parts of oxidation promoter obtain being low stannic oxide/graphene nano piece continuing grinding for 20 hours
Layer powder.
2. minuent stannic oxide/graphene nano lamella raw powder's production technology according to claim 1, it is characterised in that: described
The partial size of graphite powder is 13~15 μm, and carbon content is not less than 99.5%.
3. minuent stannic oxide/graphene nano lamella raw powder's production technology according to claim 1, it is characterised in that: described
Oxidant be potassium chlorate, potassium peroxydisulfate and potassium bichromate be mixed by mass parts 5:5:6.
4. minuent stannic oxide/graphene nano lamella raw powder's production technology according to claim 1, it is characterised in that: described
Oxidation promoter is brown lead oxide or cobalt trifluoride.
5. minuent stannic oxide/graphene nano lamella raw powder's production technology according to claim 1, it is characterised in that: described
Dispersing aid is powdery polycarboxylic acid water-reducing agent, and solid polycarboxylic acid water reducing agent content is not less than 99.5%, and moisture content is not more than 2%,
Fineness is that average grain diameter is 35 μm, and water-reducing rate is not less than 30%.
6. minuent stannic oxide/graphene nano lamella raw powder's production technology according to claim 1, it is characterised in that: described
Grinding aid is mixed by silicon powder and steel-making slag powder by the mass ratio of 1:2, and wherein the partial size of silicon powder is 2~10 μm, specific surface area
Not less than 3000m2/ kg, dioxide-containing silica are greater than 90%；Steel-making slag powder is the ground gained of slag that steel mill generates, partial size
It is 2~10 μm, specific surface area is not less than 3000m2/ kg, sulfur trioxide content are not more than 4.0%.
7. minuent stannic oxide/graphene nano lamella raw powder's production technology according to claim 1, it is characterised in that: described
Milling apparatus is high-energy planetary formula ball mill, and ball grinder is stainless cylinder of steel, and abrading-ball is GCr15 exceptional hardness Alloy Balls In Milling, ratio of grinding media to material
Example be 8:1,300 revs/min of rotational speed of ball-mill.
8. minuent stannic oxide/graphene nano lamella powder, feature made of a kind of preparation method as described in claim 1 exist
In: low stannic oxide/graphene nano lamella powder lamellar spacing be 2.35~2.75nm, slice plane having a size of 1.3~2.5 μm,
Oxygen content is 8.5~12.8%, and specific surface area is 261~287m2/ g, thermal coefficient are 1326~1852W/ (mK).
9. the application of minuent stannic oxide/graphene nano lamella powder, is pressed made of a kind of preparation method as described in claim 1
Cement matrix preparation method for material, the volume of low stannic oxide/graphene nano lamella powder are the 1.5~3.5% of cement silty amount,
Low stannic oxide/graphene nano lamella powder is mixed after mixing evenly with cement powder in mixed concrete, 28 day age water
Compression strength, flexural strength and the thermal coefficient of cement-based material are improved than control sample respectively is not less than 39%, 54% and
300%.
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