CN109320268A - A kind of graphite erosion-resistant material and graphite material and preparation method - Google Patents
A kind of graphite erosion-resistant material and graphite material and preparation method Download PDFInfo
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- CN109320268A CN109320268A CN201811362283.9A CN201811362283A CN109320268A CN 109320268 A CN109320268 A CN 109320268A CN 201811362283 A CN201811362283 A CN 201811362283A CN 109320268 A CN109320268 A CN 109320268A
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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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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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
- C04B41/5006—Boron compounds
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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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- 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
- 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
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Products (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention proposes a kind of graphite erosion-resistant material and graphite material and preparation methods, comprising: stirs 50 DEG C -80 DEG C of water in blender, and boric acid is added while stirring；After then proceeding to stirring 3 hours；When boric acid after completely dissolution, add a certain amount of glue and a certain amount of suspending agent and continue stirring 5 hours；It is then allowed to stand 12 hours formation resistant to corrosion agent emulsions；Carbon, magnesium, calcium are dried and are crushed to partial size no more than 6 μm；Then these materials are sufficiently mixed to obtain mixture；Lotion is put into blender to be stirred, and mixture is added while stirring；After object to be mixed is all added in lotion；Then repeat stirring, stand, until the viscosity of material reaches 30-90mpa.s, relative density of fluid reaches 1.58-1.88g/cm3, obtain graphite erosion-resistant material.
Description
Technical field
The present invention relates to field of material technology, more particularly, to a kind of graphite erosion-resistant material and graphite material and preparation side
Method.
Background technique
In smelting relevant industries, various containers have been widely used.Graphite has resistance to due to its special crystal structure
Numerous characteristics such as high temperatures, thermal shock resistance, electric conductivity, lubricity, chemical stability, be always military project and modern industry and height,
Newly, indispensable grand strategy resource in sharp technology development, has wide range of applications.In the prior art in order to improve crystal vessel
Thermal conductivity and intensity, usually in processing graphite container selection have high thermal conductivity, low thermal expansion and high elastic modulus stone
Ink material, to improve the thermal shock resistance of crystal vessel.
But in the prevalence of a problem when using this existing crystal vessel: graphite material has at high temperature
It under strong corrosive atmosphere and the industrial and mining condition of corrosivity melt liquid, can quickly be etched, lead to the crystal structure of graphite quilt
It destroys, forms the hole of large area outside in, it is serious chip off-falling slag-off phenomenon finally occur.It will lead to graphite product in this way to shift to an earlier date
The problem of losing due effect, result in waste of resources, increasing production cost.
Summary of the invention
Aiming at the problem that being easily damaged current crystal vessel is easy in high temperature strong corrosion, the embodiment of the present invention is mentioned
Go out a kind of graphite erosion-resistant material and graphite material and preparation method, it is at least part of to solve graphite existing in the prior art
Material problem easy to damage.
To achieve the goals above, the embodiment of the invention provides a kind of graphite erosion-resistant materials, including following parts by weight
Raw material:
Water H2O:4.5-5.2 boric acid H3BO31.2-1.9 nitrogen N:1.8-2.6
Carbon C:2.6-3.8 magnesium Mg:1.3-1.9
Calcium Ca:0.45-0.9 glue: 0.12-0.5 suspending agent: 0.03-0.2.
Meanwhile the embodiment of the invention provides a kind of preparation methods of graphite erosion-resistant material above-mentioned, comprising:
50 DEG C -80 DEG C of water is stirred in blender, and boric acid is added while stirring by step 101；It then proceedes to stir
After 3 hours；When boric acid after completely dissolution, add glue and suspending agent and continue stirring 5 hours；It is then allowed to stand 12 hours and is formed
Resistant to corrosion agent emulsion；
Carbon, magnesium, calcium are dried and are crushed to partial size no more than 6 μm by step 102；Then these materials are sufficiently mixed
Conjunction obtains mixture；
The lotion of step 101 is put into blender and is stirred by step 103, and is added what step 102 obtained while stirring
Mixture；After the mixture of step 102 is all added in lotion；Then repeat stirring, stand, until the viscosity of material
Reach 30-90mpa.s, relative density of fluid reaches 1.58-1.88g/cm3, obtain graphite erosion-resistant material.
Wherein, the stirring container for stirring synthetic material is ceramic vessel or rustless steel container.
In a step 101, boric acid is added while stirring and refers to that addition boric acid 0.5-6kg, addition speed are 0.3-2kg/
min.In step 103, the lotion of step 101 is put into blender and is stirred, and the mixed of step 102 acquisition is added while stirring
Close object；Mixing speed is 150 revs/min, additional amount 0.5-5kg.When lotion is added, whole lotions should be firstly added
60%, after being added to whole dry mash, stirs evenly and remaining 40% lotion is added again.
Wherein, step 103 specifically includes:
The lotion of step 101 is put into blender to be stirred, and the mixture that step 102 obtains is added while stirring；
Mixture to step 102 is all added in lotion, is sufficiently stirred 8 hours, is then stood 12 hours again；Then it is small that 6 are stirred for
When, then stand 10 hours；Until the viscosity of material reaches 60-100mpa.s, relative density of fluid reaches 1.68-1.98g/
cm3, obtain graphite erosion-resistant material.
Meanwhile the embodiment of the present invention also proposed and a kind of utilize graphite erosion-resistant material above-mentioned manufacture resistant to corrosion graphite
Preparation method, comprising:
Graphite matrix is placed in impregnating autoclave at normal temperature, and graphite erosion-resistant material is added by step 201, then utilizes
Drying compressed air pressurizes to impregnating autoclave, pressure 0.2-2.5Mpa, and pressing time can be 1-8 hours；
Graphite matrix after step 201 processing is sintered by step 202 in heating equipment, and vacuum degree is -3pa
To -1pa, temperature be 300-1000 DEG C, the time is 120-180 hours；
Step 203, the material for obtaining step 202 are passed through nitrogen in atmosphere sintering furnace and carry out high-temperature roasting, and temperature is
1000-1600 DEG C, the time be 180-300 hours, obtain graphite material.
Wherein, impregnating autoclave is general name, may include vacuum tank, pressurized tank, heating tank, pressure cooker, sealing container etc..In step
In rapid 202, heating equipment can be vacuum atmosphere sintering furnace.
Technical solution of the present invention has the advantage that
Above scheme proposes a kind of graphite erosion-resistant material and graphite material and preparation method, can prepare resistance to 1500
The resistant to corrosion graphite composite material of DEG C high temperature.Industrial and mining condition of the product of this new graphite material processing and manufacturing at 1500 DEG C
It is lower try out within 300 days, thorough success is obtained, is domestic 10 times of the same graphite substrate material service life or more, meets or exceeds
Developed country's import graphite material, has broken the technical monopoly of developed country, considerably reduces the production cost of enterprise.
Detailed description of the invention
By with reference to the accompanying drawing to a preferred embodiment of the present invention carry out description, technical solution of the present invention and
Its technical effect will become clearer, and more easily understand.Wherein:
Fig. 1 is the flow diagram of the preparation method of the graphite erosion-resistant material of the embodiment of the present invention.
Specific embodiment
A preferred embodiment of the present invention is described below with reference to appended attached drawing.
To achieve the goals above, the embodiment of the invention provides a kind of graphite erosion-resistant materials, including following parts by weight
Raw material:
Water H2O:4.5-5.2 boric acid H3BO31.2-1.9 nitrogen N:1.8-2.6
Carbon C:2.6-3.8 magnesium Mg:1.3-1.9
Calcium Ca:0.45-0.9 glue: 0.12-0.5 suspending agent: 0.03-0.2.
Meanwhile as shown in Figure 1, the embodiment of the invention provides a kind of preparation sides of graphite erosion-resistant material above-mentioned
Method, comprising:
Meanwhile the embodiment of the invention provides a kind of preparation methods of graphite erosion-resistant material above-mentioned, comprising:
50 DEG C -80 DEG C of water is stirred in blender, and boric acid is added while stirring by step 101；It then proceedes to stir
After 3 hours；When boric acid after completely dissolution, add glue and suspending agent and continue stirring 5 hours；It is then allowed to stand 12 hours and is formed
Resistant to corrosion agent emulsion；
Carbon, magnesium, calcium are dried and are crushed to partial size no more than 6 μm by step 102；Then these materials are sufficiently mixed
Conjunction obtains mixture；
The lotion of step 101 is put into blender and is stirred by step 103, and is added what step 102 obtained while stirring
Mixture；After the mixture of step 102 is all added in lotion；Then repeat stirring, stand, until the viscosity of material
Reach 30-90mpa.s, relative density of fluid reaches 1.58-1.88g/cm3, obtain graphite erosion-resistant material.
Wherein, the stirring container for stirring synthetic material is ceramic vessel or rustless steel container.
In a step 101, boric acid is added while stirring and refers to that addition boric acid 0.5-6kg, addition speed are 0.3-2kg/
min.In step 103, the lotion of step 101 is put into blender and is stirred, and the mixed of step 102 acquisition is added while stirring
Close object；Mixing speed is 150 revs/min, additional amount 0.5-5kg.Specifically, what is be added for the first time is the 60% of whole lotions,
After whole dry mash additions, stirs evenly and remaining 40% lotion is added again.
Wherein, step 103 specifically includes:
The lotion of step 101 is put into blender to be stirred, and the mixture that step 102 obtains is added while stirring；
Mixture to step 102 is all added in lotion, is sufficiently stirred 8 hours, is then stood 12 hours again；Then it is small that 6 are stirred for
When, then stand 10 hours；Until the viscosity of material reaches 60-100mpa.s, relative density of fluid reaches 1.68-1.98g/
cm3, obtain graphite erosion-resistant material.
Meanwhile the embodiment of the present invention also proposed and a kind of manufacture impermeable graphite using graphite erosion-resistant material above-mentioned
Preparation method, comprising:
Graphite matrix is placed in impregnating autoclave at normal temperature, and graphite erosion-resistant material is added by step 201, then utilizes
Drying compressed air pressurizes to impregnating autoclave, pressure 0.2-2.5Mpa, and pressing time can be 1-8 hours；
Graphite matrix after step 201 processing is sintered by step 202 in heating equipment, and vacuum degree is -3pa
To -1pa, temperature be 300-1000 DEG C, the time is 120-180 hours；
Step 203, the material for obtaining step 202 are passed through nitrogen in atmosphere sintering furnace and carry out high-temperature roasting, and temperature is
1000-1600 DEG C, the time be 180-300 hours, obtain graphite material.
Wherein, impregnating autoclave is general name, may include vacuum tank, pressurized tank, heating tank, pressure cooker, sealing container etc..In step
In rapid 202, heating equipment can be vacuum atmosphere sintering furnace.
Specifically, the present invention relates to resistance to 1500 DEG C of high temperature resistants resistant to corrosion graphite composite material and its preparation processes.Stone
Ink has numerous spies such as heat-resisting quantity, thermal shock resistance, electric conductivity, lubricity, chemical stability due to its special crystal structure
Property, it is always indispensable grand strategy resource in military project and modern industry and height, new, point technology development, has a wide range of application
It is general.But China's technical level is low, and production technology falls behind relatively, mid and low-end products can only be produced, and high-end graphite produces
Product especially have the graphite products of specific function, it is still necessary to from developed country's import.Graphite material has the following problems: in height
Under the lower industrial and mining condition with vigorous erosion atmosphere and corrosivity melt liquid of temperature, the crystal knot of graphite is quickly etched, destroyed
Structure causes the hole of large area outside in, and chip off-falling slag-off phenomenon is serious, and graphite product is forced to lose due effect in advance,
It results in waste of resources, increases production cost.
In order to solve the above technical problems, the present invention provides a kind of resistance to 1500 DEG C of high-temperature anti-corrosions special graphite new material, institute
Special graphite new material is stated, by percentage to the quality, including such as the following group:
The present invention also provides a kind of preparation process of 1500 DEG C of high temperature resistant anti-erosion special graphite new materials, the anti-erosions
The preparation process of special graphite new material, includes the following steps:
Prepare graphite anti-erosion agent technique
50-80 DEG C of distilled water is poured into stainless steel or ceramic stirrer, a certain amount of H is slowly added into3BO3, then carry out
It mixes slowly 3 hours (in order to avoid spillage), works as H3BO3All after dissolution, glue and suspending agent are added, is further continued for stirring 5 hours,
Stop stirring, after standing 12 hours, the lotion of graphite anti-erosion agent is made.
By the main component of graphite anti-erosion agent, dried respectively, crush (6 microns of granularity or less), mix in proportion,
Stirring etc..It after dry powder blend is uniform, pours into the blender of lotion, is stirred when pouring into.When lotion is by whole dry powder blend material
After wet, be sufficiently stirred 8 hours, stand 12 hours, be further continued for stirring 6 hours, stands 10 hours.Then painting -4# glasss is used
When relative density of fluid reaches 1.58-1.88g/cm3, graphite anti-erosion agent is made in measurement, viscosity 15-45mpa.s.
Impregnation technology
Graphite substrate material is put into impregnating autoclave, under normal temperature conditions, prepared graphite is resisted by self-priming water pump and is invaded
Erosion agent liquid is drawn into impregnating autoclave, is then pressurizeed by filtered dry compressed gas to impregnating autoclave, pressure 0.2-
2.5Mpa completes the impregnation technique to graphite substrate material under normal temperature state.
Roasting technique
It will be put into vacuum atmosphere sintering furnace by the good graphite substrate material of graphite anti-erosion agent impregnation, in vacuum degree
Under the conditions of reaching -3pa to -1pa, into the sintering for crossing 300-1000 DEG C, 120-180 hours.Then, under the conditions of nitrogen protection,
It is new to prepare a kind of 1500 DEG C of high temperature resistant anti-erosion special graphites for the high-temperature roasting for carrying out 1000-1600 DEG C, 180-300 hours
Material.
For person of ordinary skill in the field, with the development of technology, present inventive concept can be in different ways
It realizes.Embodiments of the present invention are not limited in embodiments described above, and can carry out within the scope of the claims
Variation.
Claims (5)
1. a kind of graphite erosion-resistant material, the raw material including following parts by weight:
Water H2O:4.5-5.2 boric acid H3BO31.2-1.9 nitrogen N:1.8-2.6
Carbon C:2.6-3.8 magnesium Mg:1.3-1.9
Calcium Ca:0.45-0.9 glue: 0.12-0.5 suspending agent: 0.03-0.2.
2. a kind of preparation method using graphite erosion-resistant material as described in claim 1 characterized by comprising
50 DEG C -80 DEG C of water is stirred in blender, and boric acid is added while stirring by step 101；It is small to then proceed to stirring 3
Shi Hou；When boric acid after completely dissolution, add glue and suspending agent and continue stirring 5 hours；It is resistance to be then allowed to stand formation in 12 hours
Corrode agent emulsion；
Carbon, magnesium, calcium are dried and are crushed to partial size no more than 6 μm by step 102；Then these materials are sufficiently mixed
To mixture；
The lotion of step 101 is put into blender and is stirred by step 103, and the mixing that step 102 obtains is added while stirring
Object；After the mixture of step 102 is all added in lotion；Then repeat stirring, stand, until the viscosity of material reaches
30-90mpa.s, relative density of fluid reach 1.58-1.88g/cm3, obtain graphite erosion-resistant material.
3. the preparation method of graphite erosion-resistant material according to claim 2, which is characterized in that stirring container is that ceramics hold
Device or rustless steel container.
4. the preparation method of graphite erosion-resistant material according to claim 2, which is characterized in that step 103 specifically includes:
The lotion of step 101 is put into blender to be stirred, and the mixture that step 102 obtains is added while stirring；To step
Rapid 102 mixture is all added in lotion, is sufficiently stirred 8 hours, is then stood 12 hours again；Then it is stirred for 6 hours, then
Stand 10 hours；Until the viscosity of material reaches 60-100mpa.s, relative density of fluid reaches 1.68-1.98g/cm3, obtain
Graphite erosion-resistant material.
5. a kind of preparation side using graphite erosion-resistant material according to any one of claims 1-4 manufacture resistant to corrosion graphite
Method, comprising:
Graphite matrix is placed in impregnating autoclave at normal temperature, and graphite erosion-resistant material is added by step 201, then utilizes drying
Compressed air pressurizes to impregnating autoclave, pressure 0.2-2.5Mpa, and pressing time can be 1-8 hours；
Step 202, by step 201 processing after graphite matrix be sintered in heating equipment, vacuum degree be -3pa to -
1pa, temperature are 300-1000 DEG C, the time is 120-180 hours；
Step 203, the material for obtaining step 202 are passed through nitrogen in atmosphere sintering furnace and carry out high-temperature roasting, and temperature is
1000-1600 DEG C, the time be 180-300 hours, obtain graphite material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811362283.9A CN109320268A (en) | 2018-11-15 | 2018-11-15 | A kind of graphite erosion-resistant material and graphite material and preparation method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811362283.9A CN109320268A (en) | 2018-11-15 | 2018-11-15 | A kind of graphite erosion-resistant material and graphite material and preparation method |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177097A (en) * | 2014-08-12 | 2014-12-03 | 杨清泉 | Special graphite carbon sleeved roller for corrosion-resistant and abrasion-resistant continuous annealing line and manufacturing process thereof |
| CN107721427A (en) * | 2017-11-27 | 2018-02-23 | 安阳市佰士特异型石墨制品有限责任公司 | A kind of new-energy automobile power battery special combination graphite crucible and its manufacturing process |
-
2018
- 2018-11-15 CN CN201811362283.9A patent/CN109320268A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177097A (en) * | 2014-08-12 | 2014-12-03 | 杨清泉 | Special graphite carbon sleeved roller for corrosion-resistant and abrasion-resistant continuous annealing line and manufacturing process thereof |
| CN107721427A (en) * | 2017-11-27 | 2018-02-23 | 安阳市佰士特异型石墨制品有限责任公司 | A kind of new-energy automobile power battery special combination graphite crucible and its manufacturing process |
Non-Patent Citations (2)
| Title |
|---|
| 戴金辉等: "《无机非金属材料概论》", 31 July 2018, 哈尔滨工业大学出版社 * |
| 黄伯云 主编: "《中国战略性新兴产业 新材料 碳/碳复合材料》", 31 December 2017, 中国铁道出版社 * |
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