CN110511058A - Modified refractory material of a kind of graphene and preparation method thereof - Google Patents
Modified refractory material of a kind of graphene and preparation method thereof Download PDFInfo
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- CN110511058A CN110511058A CN201910935040.8A CN201910935040A CN110511058A CN 110511058 A CN110511058 A CN 110511058A CN 201910935040 A CN201910935040 A CN 201910935040A CN 110511058 A CN110511058 A CN 110511058A
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5001—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with carbon or carbonisable materials
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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Abstract
The invention discloses a kind of preparation methods of the modified refractory material of graphene, using refractory material to be modified and graphene oxide aqueous dispersions as raw material, graphene oxide aqueous dispersions are obtained into the refractory material for being impregnated with graphene oxide into the hole of refractory material by vacuum impregnation, the refractory material for being impregnated with graphene oxide is dried in vacuo later, and carrying out reduction reaction after the drying makes graphene oxide be reduced to graphene, finally carries out the refractory material modified to graphene obtained by drying.Excellent slag corrosion performance resistant to high temperatures can be possessed under conditions of carbon content extremely low (C < 0.1wt%) using refractory material prepared by this method, and be not easy to pollute molten steel.Preparation method of the invention requires the material of refractory material with forming method low, has a wide applicability, and the preparation method simple process, with short production cycle.
Description
Technical field
The present invention relates to a kind of technical field of refractory materials, more particularly, to a kind of modified refractory material of graphene and its system
Preparation Method.
Background technique
Carbon containing sizing refractory material is due to excellent thermal shock resistance and good resistance to slag corrosion, in steel and iron industry
It is widely used, main application range has: 1) blast furnace ironmaking refractory material, such as high temperature furnace bottom, iron tap channel position；
2) liner body of converter, electric furnace and ladle；3) continuous casting critical component, such as the mouth of a river, slide plate, stopper；4) earthenware of smelting metal
Crucible.But traditional carbon containing sizing refractory material carbon content is high, and the precipitation of carbon easily occurs in use, increases molten steel
Carbon pollutes steel.
Unshape refractory because its convenient construction, without high temperature firing and structural integrity it is good, in refractory material total amount
Middle proportion is higher and higher.But due to the non wettability of carbon material and water, so that the preparation of unshape refractory is difficult, and
The resistance to slag corrosion of unshape refractory is lower.
Moreover, no matter carbon containing sizing refractory material or unshape refractory, it is high that receiving is removed in use
Temperature effect is outer, all can be by the erosion of slag, therefore, and the quality of refractory material slag-resistant erosion performance is to influence refractory material to make
With an important quality factor of service life length, and judge a key technical indexes of capabilities of refractory materials superiority and inferiority.Enhancing
The slag-resistant erosion performance of refractory material improves the heat of such Thermal Equipment to the service life for extending furnace lining and its masonry
Efficiency and production efficiency reduce cost, reduce product because polluting caused by refractory material, it is all meaningful for improving product quality
's.
Therefore, it is badly in need of finding a kind of preparation method of refractory material, refractory material is made to possess good slag-resistant aggressivity
Can, while the carbon content of carbon containing sizing refractory material can be made lower, simplify the preparation process of unshape refractory.
Summary of the invention
In view of this, the object of the present invention is to provide modified refractory material of a kind of graphene and preparation method thereof, the preparation
Method is suitable for carbon containing sizing refractory material and amorphous refractory simultaneously.The preparation method make preparation refractory material gather around
Under the premise of having good slag-resistant erosion performance, the carbon content of carbon containing sizing refractory material can be made lower, made unsetting resistance to
The preparation process of fiery material simplifies.
In order to solve the above-mentioned technical problem used technical solution is the present invention: a kind of modified refractory material of graphene
Preparation method leads to graphene oxide aqueous dispersions using refractory material to be modified and graphene oxide aqueous dispersions as raw material
It crosses vacuum impregnation and obtains the refractory material for being impregnated with graphene oxide into the hole of refractory material, oxidation stone will be impregnated with later
The refractory material of black alkene is dried in vacuo, and carrying out reduction reaction after the drying makes graphene oxide be reduced to graphene, most
The refractory material modified to graphene obtained by drying is carried out afterwards.
Further, the concentration of the graphene oxide aqueous dispersions is 0.5 ~ 5wt%, is to utilize 1 ~ 10 part of quality
Graphene oxide mixes and uniformly obtained through ultrasonic disperse with the water of 190 ~ 199 parts of quality.
Further, the mass parts ratio of the refractory material to be modified and graphene oxide aqueous dispersions is 1:1.
Further, the reduction reaction is electronation or thermal reduction.
Further, reducing agent used in electronation is any one in sodium borohydride, potassium borohydride or hydrazine hydrate；
The reaction temperature of electronation is 80 ~ 90 DEG C.
Further, thermal reduction is in Ar or N2It is heated to 300 ~ 400 DEG C under atmosphere and keeps the temperature 2h.
Using the modified refractory material of the graphene of above method preparation.
The graphene oxide that the present invention selects is crystalline flake graphite gained, technical maturity, raw material after strong oxidation removing
It is easy to get.
The utility model has the advantages that
As described above, modified refractory material of a kind of graphene of the invention and preparation method thereof, has the advantages that
1, the present invention is modified refractory material by graphene, coats or fills in refractory surface and internal void
There is the graphene not with slag wetting, the channel of slag intrusion refractory material is plugged, so that prepared refractory material is in carbon
Excellent slag corrosion performance resistant to high temperatures can be possessed under conditions of content extremely low (C < 0.1wt%), and be not easy to cause dirt to molten steel
Dye.
2, the present invention is used electronation (using sodium borohydride, potassium borohydride or hydrazine hydrate as reducing agent) or is gone back using heat
Former graphene oxide can be such that the oxygen-containing functional group on graphene oxide removes at a lower temperature and be reduced to graphene and realize also
Former effect, does not need high-temperature process, reduces energy consumption.
3, the present invention is immersed in graphene oxide in the hole of refractory material using vacuum impregnation, since graphene has
Good spreading property only needs a small amount of graphene oxide that good dipping effect can be realized, saves graphene oxide
Dosage, while dip time is shortened, it further reduced production cost.
4, the method that the present invention prepares the modified refractory material of graphene, material and forming method requirement to refractory material
It is low, there is wide applicability, and the preparation method simple process, with short production cycle.
Further specific detailed description is done to the present invention below with reference to embodiment the drawings and specific embodiments.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology to be briefly described, it should be apparent that, the accompanying drawings in the following description is only the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the SEM picture of the modified refractory material of graphene prepared by embodiment 1.
Specific embodiment
A kind of preparation method of the modified refractory material of graphene, with refractory material to be modified and graphene oxide water dispersion
Liquid is raw material, by graphene oxide aqueous dispersions by vacuum impregnation (vacuum degree be 10par) when vacuum impregnation to be modified
Refractory material hole in, the mass parts ratio of refractory material and graphene oxide aqueous dispersions is 1:1, will be impregnated with later
The refractory material of graphene oxide is dried in vacuo, and carrying out reduction reaction after the drying makes graphene oxide be reduced to graphite
Alkene finally carries out the refractory material modified to graphene obtained by drying.The reduction reaction is electronation or thermal reduction.Using
When electronation, reducing agent used in electronation is any one in sodium borohydride, potassium borohydride or hydrazine hydrate；Chemistry is also
Former reaction temperature is 80 ~ 90 DEG C.When using thermal reduction, the reaction temperature of thermal reduction is 300 ~ 400 DEG C.
The concentration of the graphene oxide aqueous dispersions is 0.5 ~ 5wt%, is the graphene oxide using 1 ~ 10 part of quality
Through made from ultrasonic disperse after being mixed with the water of 190 ~ 199 parts of quality.
It is under conditions of carbon content extremely low (C < 0.1wt%) using the modified refractory material of the graphene of above method preparation
Excellent slag corrosion performance resistant to high temperatures can be possessed, and be not easy to pollute molten steel.
Technical scheme in the embodiment of the invention is clearly and completely described combined with specific embodiments below, so that
Those skilled in the art can better understand the present invention and can be practiced, but illustrated embodiment is not as to of the invention
It limits.
Various raw materials are used in the following example, unless otherwise mentioned, all use conventional commercial product.Below with reference to specific
Embodiment does further specific detailed description to the present invention, and embodiments of the present invention are not limited thereto.
It should be noted that this preparation method is suitable for all refractory materials (including carbon containing sizing refractory material and indefinite
Type refractory material), part refractory material is only exemplified by embodiment.
Embodiment 1
A kind of preparation method of the modified refractory material of graphene, mainly comprises the steps that the graphite oxide of 1 ~ 5 part of quality first
Alkene is mixed with the water of 199 ~ 195 parts of quality, ultrasonic disperse 2h, and obtaining concentration is 0.5 ~ 2.5wt% graphene oxide aqueous dispersions；
The refractory material of 1 part of quality is immersed in the graphene oxide aqueous dispersions of 1 part of quality again, vacuum impregnation for 24 hours, obtains
It is impregnated with the refractory material of graphene oxide；Then the refractory material for being impregnated with graphene oxide is placed in vacuum oven
It is interior, it is dried in vacuo 48h at 60 DEG C, obtains the dry refractory material for being soaked with graphene oxide；It later will be after the drying
The reducing agent used for refractory material for being soaked with graphene oxide carries out electronation at being 80 DEG C in reaction temperature, after finally restoring again
Refractory material be placed in vacuum oven at 80 DEG C it is dry for 24 hours, the modified refractory material of graphene is made.
Wherein, the refractory material is Al2O3Refractory brick, the reducing agent are sodium borohydride.
Fig. 1 is Al2O3Refractory brick is through the modified SEM photograph of graphene, it can be seen that in refractory surface and stomata
Portion is coated or is filled by the graphene not soaked with slag, plugs the channel of slag intrusion refractory material, makes it have good
Good slag-resistant erosion performance.Compared to unmodified refractory material, scouring area can reduce 20%.
Embodiment 2
A kind of preparation method of the modified refractory material of graphene, mainly comprises the steps that the graphite oxide of 1 ~ 5 part of quality first
Alkene is mixed with the water of 199 ~ 195 parts of quality, ultrasonic disperse 2h, and obtaining concentration is 0.5 ~ 2.5wt% graphene oxide aqueous dispersions；
The refractory material of 1 part of quality is immersed in the graphene oxide aqueous dispersions of 1 part of quality again, vacuum impregnation 36h is obtained
It is impregnated with the refractory material of graphene oxide；Then the refractory material for being impregnated with graphene oxide is placed in vacuum oven
It is interior, it is dried in vacuo at 80 DEG C for 24 hours, obtains the dry refractory material for being soaked with graphene oxide；Later by being soaked with after drying
The reducing agent used for refractory material of graphene oxide carries out electronation at being 90 DEG C in reaction temperature, finally again will be resistance to after reduction
Fiery material is placed in vacuum oven the dry 48h at 60 DEG C, and the modified refractory material of graphene is made.
Wherein, the refractory material is MgO refractory brick, and the reducing agent is potassium borohydride.
Embodiment 3
A kind of preparation method of the modified refractory material of graphene, mainly comprises the steps that the graphite oxide of 1 ~ 5 part of quality first
Alkene is mixed with the water of 199 ~ 195 parts of quality, ultrasonic disperse 2h, and obtaining concentration is 0.5 ~ 2.5wt% graphene oxide aqueous dispersions；
The refractory material of 1 part of quality is immersed in the graphene oxide aqueous dispersions of 1 part of quality again, vacuum impregnation 48h is obtained
It is impregnated with the refractory material of graphene oxide；Then the refractory material for being impregnated with graphene oxide is placed in vacuum oven,
It is dried in vacuo 48h at 60 DEG C, obtains the dry refractory material for being soaked with graphene oxide；Later oxidation will be soaked with after drying
The refractory material of graphene is heat-treated, and finally the refractory material after reduction is placed in vacuum oven again and is done at 80 DEG C
The modified refractory material of graphene is made in dry 36h.
Wherein, the refractory material is Al2O3Refractory casting material, the thermal reduction condition be Ar atmosphere at 300 DEG C
Keep the temperature 2h.
Embodiment 4
A kind of preparation method of the modified refractory material of graphene, mainly comprises the steps that the graphite oxide of 1 ~ 5 part of quality first
Alkene is mixed with the water of 199 ~ 195 parts of quality, ultrasonic disperse 2h, and obtaining concentration is 0.5 ~ 2.5wt% graphene oxide aqueous dispersions；
The refractory material of 1 part of quality is immersed in the graphene oxide aqueous dispersions of 1 part of quality again, vacuum impregnation 48h is obtained
It is impregnated with the refractory material of graphene oxide；Then the refractory material for being impregnated with graphene oxide is placed in vacuum oven,
It is dried in vacuo 48h at 60 DEG C, obtains the dry refractory material for being soaked with graphene oxide；Later oxidation will be soaked with after drying
The refractory material of graphene is heat-treated, and finally the refractory material after reduction is placed in vacuum oven again and is done at 80 DEG C
The modified refractory material of graphene is made in dry 36h.
Wherein, the refractory material is MgO refractory brick, and the thermal reduction condition is to keep the temperature at 400 DEG C in Ar atmosphere
2h。
Embodiment 5
A kind of preparation method of the modified refractory material of graphene, mainly comprises the steps that the oxidation stone of 6 ~ 10 parts of quality first
Black alkene is mixed with the water of 190 ~ 194 parts of quality, ultrasonic disperse 2h, and obtaining concentration is 3.0 ~ 5.0wt% graphene oxide water dispersion
Liquid；The refractory material of 1 part of quality is immersed in the graphene oxide aqueous dispersions of 1 part of quality again, vacuum impregnation for 24 hours,
Obtain the refractory material for being impregnated with graphene oxide；Then the refractory material for being impregnated with graphene oxide vacuum is placed in do
In dry case, it is dried in vacuo 48h at 60 DEG C, obtains the dry refractory material for being soaked with graphene oxide；Later by the drying
The reducing agent used for refractory material for being soaked with graphene oxide afterwards carries out electronation at being 80 DEG C in reaction temperature, finally again will also
Refractory material after original is placed in vacuum oven the dry 36h at 80 DEG C, and the modified refractory material of graphene is made.
Wherein, the refractory material is Al2O3-SiO2Refractory brick, the reducing agent are hydrazine hydrate.
Embodiment 6
A kind of preparation method of the modified refractory material of graphene, mainly comprises the steps that the oxidation stone of 6 ~ 10 parts of quality first
Black alkene is mixed with the water of 190 ~ 194 parts of quality, ultrasonic disperse 2h, and obtaining concentration is 3.0 ~ 5.0wt% graphene oxide water dispersion
Liquid；The refractory material of 1 part of quality is immersed in the graphene oxide aqueous dispersions of 1 part of quality again, vacuum impregnation for 24 hours,
Obtain the refractory material for being impregnated with graphene oxide；Then the refractory material for being impregnated with graphene oxide vacuum is placed in do
In dry case, it is dried in vacuo 48h at 60 DEG C, obtains the dry refractory material for being soaked with graphene oxide；Later by the drying
The reducing agent used for refractory material for being soaked with graphene oxide afterwards carries out electronation at being 80 DEG C in reaction temperature, finally again will also
Refractory material after original is placed in vacuum oven the dry 36h at 80 DEG C, and the modified refractory material of graphene is made.
Wherein, the refractory material is Al2O3- MgO refractory brick, the reducing agent are sodium borohydride.
Embodiment 7
A kind of preparation method of the modified refractory material of graphene, mainly comprises the steps that the oxidation stone of 6 ~ 10 parts of quality first
Black alkene is mixed with the water of 190 ~ 194 parts of quality, ultrasonic disperse 2h, and obtaining concentration is 3.0 ~ 5.0wt% graphene oxide water dispersion
Liquid；The refractory material of 1 part of quality is immersed in the graphene oxide aqueous dispersions of 1 part of quality again, vacuum impregnation 48h,
Obtain the refractory material for being impregnated with graphene oxide；Then the refractory material for being impregnated with graphene oxide vacuum is placed in do
In dry case, it is dried in vacuo 48h at 60 DEG C, obtains the dry refractory material for being soaked with graphene oxide；Later by the drying
The refractory material for being soaked with graphene oxide afterwards is heat-treated, and the refractory material after reduction is finally placed in vacuum oven again
Interior 36h dry at 80 DEG C, is made the modified refractory material of graphene.
Wherein, the refractory material is Al2O3-SiO2Refractory casting material, the thermal reduction condition be Ar atmosphere in
2h is kept the temperature at 300 DEG C.
Embodiment 8
A kind of preparation method of the modified refractory material of graphene, mainly comprises the steps that the graphene oxide of 6 ~ 10 parts of quality
It is mixed with the water of 190 ~ 194 parts of quality, ultrasonic disperse 2h, obtaining concentration is 3.0 ~ 5.0wt% graphene oxide aqueous dispersions；Again
The refractory material of 1 part of quality is immersed in the graphene oxide aqueous dispersions of 1 part of quality, vacuum impregnation 48h is soaked
Stain has the refractory material of graphene oxide；Then the refractory material for being impregnated with graphene oxide is placed in vacuum oven
It is interior, it is dried in vacuo 48h at 60 DEG C, obtains the dry refractory material for being soaked with graphene oxide；It later will be after the drying
The refractory material for being soaked with graphene oxide is heat-treated, and finally the refractory material after reduction is placed in vacuum oven again
The modified refractory material of graphene is made in dry 36h at 80 DEG C.
Wherein, the refractory material is Al2O3- MgO refractory casting material, the thermal reduction condition are N2In 400 in atmosphere
2h is kept the temperature at DEG C.
The method that the present invention prepares the modified refractory material of graphene, the material and forming method requirement to refractory material are low,
With wide applicability, and it is the preparation method simple process, with short production cycle.
Modified refractory material of a kind of graphene provided by the present invention and preparation method thereof is described in detail above,
Specific case used herein is expounded the principle of the present invention and specific embodiment, and above-described embodiment is only used to help
Assistant solves method and core concept of the invention.It should be pointed out that for those of ordinary skill in the art, it is all according to this
The technical spirit of invention any simple modification, equivalent change and modification to the above embodiments, each fall within guarantor of the invention
It protects in range.
Claims (7)
1. a kind of preparation method of the modified refractory material of graphene, it is characterised in that: with refractory material to be modified and oxidation stone
Black alkene aqueous dispersions are raw material, and graphene oxide aqueous dispersions are impregnated by vacuum impregnation into the hole of refractory material
There is the refractory material of graphene oxide, is later dried in vacuo the refractory material for being impregnated with graphene oxide, and in drying
Carrying out reduction reaction afterwards makes graphene oxide be reduced to graphene, finally carries out the fire proofed wood modified to graphene obtained by drying
Material.
2. a kind of preparation method of the modified refractory material of graphene according to claim 1, it is characterised in that: the oxidation
The concentration of graphene aqueous dispersions is 0.5 ~ 5wt%, is graphene oxide and 190 ~ 199 parts of quality using 1 ~ 10 part of quality
Water mixing and uniformly obtained through ultrasonic disperse.
3. a kind of preparation method of the modified refractory material of graphene according to claim 1, it is characterised in that: described wait change
Property refractory material and graphene oxide aqueous dispersions mass parts ratio be 1:1.
4. a kind of preparation method of the modified refractory material of graphene according to claim 1, it is characterised in that: the reduction
Reaction is electronation or thermal reduction.
5. a kind of preparation method of the modified refractory material of graphene according to claim 4, it is characterised in that: electronation
Reducing agent used is any one in sodium borohydride, potassium borohydride or hydrazine hydrate；The reaction temperature of electronation is 80 ~ 90
℃。
6. a kind of preparation method of the modified refractory material of graphene according to claim 4, it is characterised in that: thermal reduction is
In Ar or N2It is heated to 300 ~ 400 DEG C under atmosphere and keeps the temperature 2h.
7. a kind of modified refractory material of graphene, which is characterized in that it is method system according to claim 1-4
Standby.
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Application publication date: 20191129 |