CN106379895A - Hydrophilic graphite for refractory castables and preparation method thereof - Google Patents
Hydrophilic graphite for refractory castables and preparation method thereof Download PDFInfo
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62886—Coating the powders or the macroscopic reinforcing agents by wet chemical techniques
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62802—Powder coating materials
- C04B35/62828—Non-oxide ceramics
- C04B35/62839—Carbon
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/447—Phosphates or phosphites, e.g. orthophosphate, hypophosphite
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
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Abstract
The invention relates to a hydrophilic graphite for refractory castables and a preparation method thereof. The technical scheme is as follows: the preparation method comprises the following steps: mixing 0.5-10 parts by mass of graphene oxide and 500 parts by mass of water, and carrying out ultrasonic dispersion for 30-60 minutes to obtain a graphene oxide aqueous dispersion; adding 90-99.5 parts by mass of flake graphite and 0-0.1 part by mass of dispersing agent into the graphene oxide aqueous dispersion, and carrying out ultrasonic dispersion for 30-60 minutes to obtain a graphene-oxide-coated graphite mixed solution; and drying the graphene-oxide-coated graphite mixed solution at 105-110 DEG C for 24-48 hours or drying under freeze conditions for 24-48 hours, thereby obtaining the hydrophilic graphite for refractory castables. The method has the characteristics of simple technique, short production cycle, low cost and small pollution. The prepared hydrophilic graphite for refractory castables has the advantages of favorable dispersity in refractory castables and low water consumption, and can enhance the scouring resistance and thermal shock stability of the refractory castables.
Description
Technical field
The present invention relates to a kind of hydrophilic graphite technical field.More particularly, to a kind of castable refractory with hydrophilic graphite and
Its preparation method.
Background technology
Crystalline flake graphite has the characteristics that to be difficult by molten steel and slag moistening, thermal coefficient of expansion is little and thermal conductivity is high, is drawn
Enter in refractory material, be remarkably improved anti-slag erosion ability and the thermal shock resistance of refractory material.Carbon containing refractory is in steel
Ironworker's industry is used widely, and main range of application has:1)Blast furnace ironmaking refractory material, the such as portion such as Blast Furnace Bottom, iron tap channel
Position;2)The liner body of converter, electric furnace and ladle;3)Continuous casting critical component, the such as mouth of a river, slide plate, stopper etc.;4)Smelting metal
Crucible.
Although crystalline flake graphite is widely applied in shaping refractory product, crystalline flake graphite is nonpolar solid
Material, has natural hydrophobicity, and wettability is excessively poor, is difficult to dispersed, and increased in castable refractory system
The water consumption of castable, is easily caused the castable refractory porosity and rises, structure become loose so that the usability of castable refractory
Can decline.These all hinder application in castable refractory for the crystalline flake graphite, in particular for carbon content be more than 5% resistance to
In fiery castable system.
Content of the invention
It is contemplated that overcoming the deficiencies in the prior art it is therefore intended that providing a kind of process is simple, with short production cycle, cost
The preparation method of the cheap and little hydrophilic graphite of castable refractory water consumption of pollution, prepared castable refractory is with hydrophilic
Property graphite good dispersion and water consumption in castable refractory little, the resistance to slag corrosion of castable refractory can be improved stable with thermal shock
Property.
The technical solution adopted in the present invention is:First by the water of the graphene oxide of 0.5 ~ 10 part of quality and 500 parts of quality
Mixing, ultrasonic disperse 30 ~ 60min, obtain graphene oxide aqueous dispersions;Again by the crystalline flake graphite of 90 ~ 99.5 parts of quality and 0 ~
The dispersant of 0.1 part of quality is added in described graphene oxide aqueous dispersions, and ultrasonic disperse 30 ~ 60min obtains graphite oxide
Alkene wraps up the mixed liquor of graphite;Then the mixed liquor described graphene oxide being wrapped up graphite is dried under the conditions of 105 ~ 110 DEG C
24 ~ 48h or under freezing conditions dry 24 ~ 48h, prepared castable refractory hydrophilic graphite.
The C content of described crystalline flake graphite is 95 ~ 99.9wt%, and granularity is 0.045 ~ 0.25mm.
Described graphene oxide is to be obtained using the oxidation of Hummers method.
Described dispersant is one or more of sodium carboxymethyl cellulose, sodium tripolyphosphate and sodium hexameta phosphate.
Due to adopting technique scheme, the present invention compared with prior art has following good effect:
1)The present invention only has several atomic layer level thickness using the graphene oxide that Hummers method is obtained, and has good certainly sprawling
Property, only need a small amount of graphene oxide to can achieve the parcel good to graphite;The addition of micro dispersant improves oxidation stone
The parcel degree to graphite for the black alkene, the hydrophilic of graphite is good.
2)The present invention passes through to control the addition of graphene oxide, using different drying modes, can advantageously control parent
The performance of watersoluble plumbago/price ratio, to meet the use requirement of the castable refractory of multiscale.
3)The present invention can be prepared by castable refractory hydrophilic graphite using graphene oxide, crystalline flake graphite and dispersant
Ink, process is simple, with short production cycle, with low cost;Additionally, due to be not introduced into affect castable refractory performance other raw materials and
Its impurity, the preparation process feature of environmental protection is good.4)The castable refractory hydrophilic graphite that the present invention is obtained can make crystalline flake graphite resistance to
Water consumption that is dispersed in fiery castable, decreasing castable refractory, be easy to improve castable refractory resistance to slag corrosion with
Thermal shock resistance.
Therefore, the present invention have the characteristics that process is simple, with short production cycle, with low cost and pollution little, prepared is resistance to
Fiery castable hydrophilic graphite good dispersion and water consumption in castable refractory is little, and the anti-slag that can improve castable refractory is invaded
Corrosion and thermal shock resistance.
Specific embodiment
With reference to specific embodiment, the invention will be further described, not the restriction to its protection domain.
In this specific embodiment:The C content of described crystalline flake graphite is 95 ~ 99.9wt%;Described graphene oxide is to adopt
The oxidation of Hummers method is obtained.Repeat no more in embodiment.
Embodiment 1
A kind of castable refractory hydrophilic graphite and preparation method thereof.Described preparation method is:Oxidation by 7 ~ 10 parts of quality
Graphene is mixed with the water of 500 parts of quality, ultrasonic disperse 30 ~ 60min, obtains graphene oxide aqueous dispersions;Again by 90 ~ 93 parts
The crystalline flake graphite of quality is added in described graphene oxide aqueous dispersions, and ultrasonic disperse 30 ~ 60min obtains graphene oxide
The mixed liquor of parcel graphite;Then the mixed liquor described graphene oxide being wrapped up graphite dries 24 under the conditions of 105 ~ 110 DEG C ~
48h, prepared castable refractory hydrophilic graphite.
The granularity of crystalline flake graphite described in the present embodiment is 0.045 ~ 0.1mm.
Embodiment 2
A kind of castable refractory hydrophilic graphite and preparation method thereof.Described preparation method is:Oxidation by 7 ~ 10 parts of quality
Graphene is mixed with the water of 500 parts of quality, ultrasonic disperse 30 ~ 60min, obtains graphene oxide aqueous dispersions;Again by 90 ~ 93 parts
The dispersant of the crystalline flake graphite of quality and 0.05 ~ 0.1 part of quality is added in described graphene oxide aqueous dispersions, ultrasonic disperse
30 ~ 60min, obtains the mixed liquor that graphene oxide wraps up graphite;Then described graphene oxide is wrapped up the mixed liquor of graphite
24 ~ 48h, prepared castable refractory hydrophilic graphite is dried under the conditions of 105 ~ 110 DEG C.
In the present embodiment:The granularity of described crystalline flake graphite is 0.045 ~ 0.1mm;Described dispersant is carboxymethyl cellulose
Sodium.
Embodiment 3
A kind of castable refractory hydrophilic graphite and preparation method thereof.Described preparation method is:Oxidation stone by 5 ~ 8 parts of quality
Black alkene is mixed with the water of 500 parts of quality, ultrasonic disperse 30 ~ 60min, obtains graphene oxide aqueous dispersions;Again by 92 ~ 95 parts of matter
The dispersant of the crystalline flake graphite of amount and 0.05 ~ 0.1 part of quality is added in described graphene oxide aqueous dispersions, ultrasonic disperse 30
~ 60min, obtains the mixed liquor that graphene oxide wraps up graphite;Then the mixed liquor described graphene oxide being wrapped up graphite exists
24 ~ 48h, prepared castable refractory hydrophilic graphite are dried under freezing conditions.
In the present embodiment:The granularity of described crystalline flake graphite is 0.1 ~ 0.15mm;Described dispersant is sodium tripolyphosphate.
Embodiment 4
A kind of castable refractory hydrophilic graphite and preparation method thereof.Described preparation method is:Oxidation stone by 5 ~ 8 parts of quality
Black alkene is mixed with the water of 500 parts of quality, ultrasonic disperse 30 ~ 60min, obtains graphene oxide aqueous dispersions;Again by 92 ~ 95 parts of matter
The crystalline flake graphite of amount is added in described graphene oxide aqueous dispersions, and ultrasonic disperse 30 ~ 60min obtains graphene oxide bag
Wrap up in the mixed liquor of graphite;Then the mixed liquor described graphene oxide being wrapped up graphite is dried 24 ~ 48h, system under freezing conditions
Obtain castable refractory hydrophilic graphite.
The granularity of crystalline flake graphite described in the present embodiment is 0.1 ~ 0.15mm.
Embodiment 5
A kind of castable refractory hydrophilic graphite and preparation method thereof.Described preparation method is:Oxidation stone by 3 ~ 6 parts of quality
Black alkene is mixed with the water of 500 parts of quality, ultrasonic disperse 30 ~ 60min, obtains graphene oxide aqueous dispersions;Again by 94 ~ 97 parts of matter
The dispersant of the crystalline flake graphite of amount and 0.05 ~ 0.1 part of quality is added in described graphene oxide aqueous dispersions, ultrasonic disperse 30
~ 60min, obtains the mixed liquor that graphene oxide wraps up graphite;Then the mixed liquor described graphene oxide being wrapped up graphite exists
24 ~ 48h, prepared castable refractory hydrophilic graphite is dried under the conditions of 105 ~ 110 DEG C.
In the present embodiment:The granularity of described crystalline flake graphite is 0.15 ~ 0.2mm;Described dispersant is sodium hexameta phosphate.
Embodiment 6
A kind of castable refractory hydrophilic graphite and preparation method thereof.
The present embodiment removes the mixing beyond the region of objective existence that described dispersant is sodium carboxymethyl cellulose and sodium tripolyphosphate, and remaining is with enforcement
Example 5.
Embodiment 7
A kind of castable refractory hydrophilic graphite and preparation method thereof.Described preparation method is:Oxidation by 0.5 ~ 4 part of quality
Graphene is mixed with the water of 500 parts of quality, ultrasonic disperse 30 ~ 60min, obtains graphene oxide aqueous dispersions;Again by 96 ~ 99.5
Part crystalline flake graphite of quality and the dispersant of 0.05 ~ 0.1 part of quality are added in described graphene oxide aqueous dispersions, ultrasonic point
Dissipate 30 ~ 60min, obtain the mixed liquor that graphene oxide wraps up graphite;Then described graphene oxide is wrapped up the mixing of graphite
Liquid is dried 24 ~ 48h, prepared castable refractory hydrophilic graphite under freezing conditions.
In the present embodiment:The granularity of described crystalline flake graphite is 0.2 ~ 0.25mm;Described dispersant is sodium tripolyphosphate and six
The mixture of Polymeric sodium metaphosphate..
Embodiment 8
A kind of castable refractory hydrophilic graphite and preparation method thereof.
Dispersant described in the present embodiment is the mixture of sodium carboxymethyl cellulose, sodium tripolyphosphate and sodium hexameta phosphate.
This specific embodiment compared with prior art has following good effect:
1)This specific embodiment only has several atomic layer level thickness using the graphene oxide that Hummers method is obtained, and has good
From spreadability, only need an a small amount of graphene oxide to can achieve the parcel good to graphite;The addition of micro dispersant improves
The parcel degree to graphite for the graphene oxide, the hydrophilic of graphite is good.
2)This specific embodiment is passed through to control the addition of graphene oxide, using different drying modes, can facilitate
Ground controls the performance/price ratio of hydrophilic graphite, to meet the use requirement of the castable refractory of multiscale.
3)This specific embodiment can be prepared by castable refractory parent using graphene oxide, crystalline flake graphite and dispersant
Watersoluble plumbago, process is simple, with short production cycle, with low cost;Additionally, due to be not introduced into affect castable refractory performance other
Raw material and its impurity, the preparation process feature of environmental protection is good.4)The castable refractory hydrophilic graphite energy that this specific embodiment is obtained
Make the water consumption that crystalline flake graphite is dispersed in castable refractory, decrease castable refractory, be easy to improve castable refractory
Resistance to slag corrosion and thermal shock resistance.
Therefore, this specific embodiment has the characteristics that process is simple, with short production cycle, with low cost and little, the institute of pollution
Good dispersion and water consumption in castable refractory are little with hydrophilic graphite for the castable refractory of preparation, can improve castable refractory
Resistance to slag corrosion and thermal shock resistance.
Claims (5)
1. a kind of castable refractory with the preparation method of hydrophilic graphite it is characterised in that first by the oxidation stone of 0.5 ~ 10 part of quality
Black alkene is mixed with the water of 500 parts of quality, ultrasonic disperse 30 ~ 60min, obtains graphene oxide aqueous dispersions;Again by 90 ~ 99.5 parts
The dispersant of the crystalline flake graphite of quality and 0 ~ 0.1 part of quality is added in described graphene oxide aqueous dispersions, and ultrasonic disperse 30 ~
60min, obtains the mixed liquor that graphene oxide wraps up graphite;Then the mixed liquor described graphene oxide being wrapped up graphite exists
Dry 24 ~ 48h under the conditions of 105 ~ 110 DEG C or 24 ~ 48h, prepared castable refractory hydrophilic graphite are dried under freezing conditions.
2. castable refractory according to claim 1 with the preparation method of hydrophilic graphite it is characterised in that described scale
The C content of graphite is 95 ~ 99.9wt%, and granularity is 0.045 ~ 0.25mm.
3. castable refractory according to claim 1 with the preparation method of hydrophilic graphite it is characterised in that described oxidation
Graphene is to be obtained using the oxidation of Hummers method.
4. castable refractory according to claim 1 with the preparation method of hydrophilic graphite it is characterised in that described dispersion
Agent is one or more of sodium carboxymethyl cellulose, sodium tripolyphosphate and sodium hexameta phosphate.
5. a kind of castable refractory hydrophilic graphite is it is characterised in that described castable refractory hydrophilic graphite is according to power
Profit requires the castable refractory parent prepared by preparation method of castable refractory hydrophilic graphite any one of 1 ~ 4
Watersoluble plumbago.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110627059A (en) * | 2019-10-13 | 2019-12-31 | 武汉善达化工有限公司 | Dispersible graphite powder and preparation method thereof |
CN113443853A (en) * | 2021-07-05 | 2021-09-28 | 宜兴必方陶瓷科技有限公司 | Preparation method of hydrophilic graphite for carbon-containing refractory material |
CN116867753A (en) * | 2021-04-07 | 2023-10-10 | 杰富意钢铁株式会社 | Castable refractory |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110627059A (en) * | 2019-10-13 | 2019-12-31 | 武汉善达化工有限公司 | Dispersible graphite powder and preparation method thereof |
CN110627059B (en) * | 2019-10-13 | 2022-03-11 | 武汉善达化工有限公司 | Dispersible graphite powder and preparation method thereof |
CN116867753A (en) * | 2021-04-07 | 2023-10-10 | 杰富意钢铁株式会社 | Castable refractory |
CN113443853A (en) * | 2021-07-05 | 2021-09-28 | 宜兴必方陶瓷科技有限公司 | Preparation method of hydrophilic graphite for carbon-containing refractory material |
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