CN110317070A - A kind of preparation method of the impact resistance magnesia carbon brick of resistance to oxygen corrosion - Google Patents
A kind of preparation method of the impact resistance magnesia carbon brick of resistance to oxygen corrosion Download PDFInfo
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- CN110317070A CN110317070A CN201910505793.5A CN201910505793A CN110317070A CN 110317070 A CN110317070 A CN 110317070A CN 201910505793 A CN201910505793 A CN 201910505793A CN 110317070 A CN110317070 A CN 110317070A
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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
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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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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
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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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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- C04B2235/422—Carbon
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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
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- 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
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Abstract
The present invention relates to a kind of preparation methods of impact resistance magnesia carbon brick of resistance to oxygen corrosion, belong to building material technical field.Present invention hot water bath in lye by magnesia stone, dissolve partial impurities, after being mixed with soy meal, microorganism decomposition is carried out using onion Aspergillus, starch and soybean protein in soy meal are decomposed, the cementation in magnesia stone and magnesia carbon brick between each molecule is improved, improves the mechanical strength of magnesia stone, improve the impact strength of magnesia stone, it is difficult to be broken；The present invention carries out energization cell reaction to the fermentation liquid for being mixed with magnesia stone, magnesium ion, which is precipitated, must electronically form magnesium simple substance in cathode, the carbon in magnesia carbon brick is set to be difficult to be oxidized decomposition, it avoids being damaged by corrosion, the aluminium ion being added simultaneously into fermentation liquid must be electronically generated nanometer aluminum simple substance near cathode, meet oxygen preferential oxidation and generate fine and close aluminum oxide film carbon coated in carbon surface by being powered, the corrosion that is decomposed is prevented, is had broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of impact resistance magnesia carbon brick of resistance to oxygen corrosion, belong to building material technical field.
Background technique
Magnesia carbon brick is with high-melting-point alkalinity oxides magnesium (2800 DEG C of fusing point) and to be difficult to be invaded the high-melting-point of profit by clinker
Carbon materials add various non-oxidized substance additives as raw material.The composite fire of not making charcoal being combined into carbonaceous bonding agent
Material.Magnesia carbon brick be mainly used for converter, ac arc furnace, direct current electric arc furnace liner, the positions such as slag line of ladle.Magnesia carbon brick is made
For a kind of composite refractory, efficiently utilize magnesia slag corrosion resistance ability is strong and the high-termal conductivity and low expansion of carbon,
Compensate for the disadvantage of magnesia spalling resistance difference.
China's steel industry yield is huge, annual to reach more than 1,000 ten thousand tons using discarded magnesia carbon brick, the processing of the material
Very big trouble is brought to iron and steel enterprise, by the variation of refractory material bidding mode, the hair integrally contracted with functionality
Exhibition and maturation, it is more and more urgent to refractory material recovery and reusing and recycling technology, it is more and more important.Since used refractory only passes through
Simple break process is crossed, is not finished, its usage amount and use scope is limited, leads to used refractory
Returning utilization rate is lower, causes a large amount of wasting of resources and destroys the sanitation and hygiene of plant area.
Since magnesia carbon brick has excellent thermal shock resistance and preferable resistance to slag, while magnesia resource is very rich, therefore magnesium
Carbon brick has obtained very extensive use in field of metallurgy.But, there is also asking in terms of three during military service for magnesia carbon brick
Topic, first, when magnesia carbon brick encounters oxidizing slag or oxidizing atmosphere will lead to wherein carbon severe oxidation, substantially reduce the property of magnesia carbon brick
Can, reduction service life, second, since the carbon in magnesia carbon brick understands some dissolution during liquid steel refining, lead to molten steel
Carburetting, this does not allow for some steel grades, and third, impact resistance is bad, easy to damage.
To improve the oxidation resistance of magnesia carbon brick under the high temperature conditions, key is to control the decarbonization rate of material.At present
A kind of common method is the additive that addition prevents oxidation in magnesia carbon brick, and there are two main classes for common additive, metal or
Alloy fine powder；Nonmetallic fine powder.For example, a kind of magnesia carbon brick of patent, the raw material of the magnesia carbon brick discards magnesium carbon by 30~80 parts by weight
Brick particle, 3~40 parts by weight magnesia particles, 6~12 parts by weight of graphite, 5~15 parts by weight magnesia powders, 3~15 parts by weight micro mists
Additive, 2.2~3.5 parts by weight organic bonds composition.Micro-powder as additive hard pitch powder, aluminium oxide are added in the magnesia carbon brick
It is micro mist, metallic aluminium powder, metallic silicon power, metal magnesium powder, boron nitride powder, any one or more than one to improve in carborundum powder
The oxidation resistance of magnesia carbon brick at high temperature has the disadvantage that metal fine powder such as metallic aluminium powder, metallic silicon power etc. easily occurs
Oxidation, already oxidised metal and the impurity in magnesia and graphite easily occur it is unfavorable react, aoxidize the effect of Shi Huiqi flux, crowd
Well known, in burned-magnesia brick, the silicate mineral of aluminium oxide and high calcium silicon ratio can react to form liquid phase, can be to refractoriness
Apparent influence is generated, under the corrosion function of molten steel, slag and gas, it is easy to lead to the reduction of product service life；In addition
In process of production, it is excessively high that the metal fine powder of addition will cause magnesia carbon brick thermal expansion to the magnesia carbon brick, so that very high stress is generated,
Magnesia carbon brick is caused easily to crack；Rather than the addition of metal fine powder such as boron nitride powder, carborundum powder etc. will affect the anti-of magnesia carbon brick again
Slag；In the preparation process of magnesia carbon brick, be also easy to produce layer split, poor toughness；Slag-resistant erosiveness is poor, and service life is short.
Therefore, it invents a kind of good impact resistance and the good magnesia carbon brick of oxytolerant corrosivity has product to building material technical field
Pole meaning.
Summary of the invention
The technical problems to be solved by the invention: be easily oxidized for carbon in current magnesia carbon brick, shock resistance it is bad
Defect provides a kind of preparation method of impact resistance magnesia carbon brick of resistance to oxygen corrosion.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of impact resistance magnesia carbon brick of resistance to oxygen corrosion the preparation method comprises the following steps:
Pre-mixture is placed in mold, mold is placed in hot press, is 23~25MPa, temperature 200 in compacting pressure
Under conditions of~220 DEG C suppress 60~70min, after compacting put into high temperature furnace in, under argon atmosphere and temperature be 900~
2~3h is calcined under conditions of 1000 DEG C, is discharged after natural cooling up to the impact resistance magnesia carbon brick of resistance to oxygen corrosion；
Pre-mixture the preparation method comprises the following steps:
(1) sulfuric acid solution that fermentation liquid and mass fraction are 30~35% is put into beaker, is made aluminium bar as anode, platinum stick
It is inserted into beaker for cathode, be powered 5~6h under conditions of DC voltage is 40~50V, by the aluminium powder on platinum stick after energization
Scrape investment beaker in, place the beaker in sonic oscillation instrument, supersonic frequency be 35~37kHz under conditions of oscillation 50~
Reaction solution is made in 60min；
(2) by reaction solution and sawdust investment reaction kettle, it is molten that the sodium hydroxide that mass fraction is 18~20% is added dropwise into reaction kettle
Liquid adjusts pH value to 9.8~10.2,30~40min is stood under room temperature, nitrogen is filled with into reaction kettle is increased to air pressure in kettle
1.6~1.8MPa heats reaction kettle, improves temperature in the kettle to 150~160 DEG C, modified filter cake is obtained by filtration after reaction, with distillation
Water cleans filter cake 3~5 times；
(3) it weighs in modified filter cake, graphite, silicon powder, calcium chloride and magnesia particle investment blender, is 150~170 in temperature
DEG C, 30~40min of mixing obtains pre-mixture under conditions of revolving speed is 300~320r/min；
Fermentation liquid the preparation method comprises the following steps:
(1) it weighs in 600~800g magnesia stone investment planetary ball mill, is mixed under conditions of revolving speed is 500~550r/min
35~45min is ground, grinding product is made, the sodium hydroxide solution that grinding product and mass fraction are 35~45% is put into and is burnt
In cup, place the beaker in the water-bath that bath temperature is 60~70 DEG C, mixed serum is made in 2~3h of constant temperature boiling；
(2) will mixed serum put into suction filtration machine in filter obtain filter cake, by filter cake 3~5 times wash with distilled water, weigh filter cake,
In soy meal and distilled water investment three-necked flask, 40~50min system is mixed with the revolving speed of 600~620r/min with blender
Obtain mixed emulsion；
(3) onion Aspergillus bacterium powder is added into three-necked flask, three-necked flask is placed in the greenhouse that temperature is 38~42 DEG C, it is permanent
Temperature stands 8~10 days, is full of nitrogen after standing into three-necked flask, continues constant temperature and stands 3~5 days, is added into three-necked flask
3~4h is mixed with blender with the revolving speed of 700~720r/min in the aluminium chloride crystal powder of mixed emulsion quality 6~8%,
Fermentation liquid is made.
The mass ratio for the sulfuric acid solution that fermentation liquid and mass fraction are 30~35% in the preparation method of pre-mixture is 1:
5。
The mass ratio of reaction solution and sawdust is 10:1 in the preparation method of pre-mixture.
In the preparation method of pre-mixture according to parts by weight, the modification filter cake be 13~15 parts, graphite 2.6
~2.8 parts, silicon powder be 0.5~0.7 part, calcium chloride is 1.0~1.2 parts, magnesia particle is 8~10 parts.
The mass ratio for the sodium hydroxide solution that grinding product is 35~45% with mass fraction in the preparation method of fermentation liquid is
1:10。
In the preparation method of fermentation liquid according to parts by weight, the filter cake is 8~10 parts, soy meal is 5~6 parts, steams
Distilled water is 13~15 parts.
The quality for the onion Aspergillus bacterium powder being added in the preparation method of fermentation liquid into three-necked flask is mixed emulsion matter
The 1.5~1.7% of amount.
The quality for the aluminium chloride crystal powder being added in the preparation method of fermentation liquid into three-necked flask is mixed emulsion matter
The 6~8% of amount.
The method have the benefit that:
(1) grinding of magnesia stone is heated boiling first by the present invention in lye, adds soy meal, distilled water is mixed to prepare mixing
Lotion is added onion Aspergillus and is put into greenhouse the obtained fermentation liquid that ferments, and sulfuric acid is added into fermentation liquid and is inserted into electrode energization
Reaction, sonic oscillation are made reaction solution, are then blended under high-temperature and high-pressure conditions reaction solution with sawdust and react, filter after reaction
Modified filter cake is made, finally mixes modified filter cake, silicon powder, magnesia and other auxiliary agents, by hot pressing, high-temperature calcination up to anti-
The impact magnesia carbon brick of resistance to oxygen corrosion, present invention hot water bath in lye by magnesia stone dissolve partial impurities, mix with soy meal
Afterwards, microorganism decomposition is carried out using onion Aspergillus, divides starch and soybean protein in soy meal more efficiently adequately
Solution generates the ingredients such as hydroxyl, carboxyl, amino and other organic group free radicals, not only contributes to reinforce in magnesia carbon brick each point
Bonding degree between son, to improve the structural strength of magnesia carbon brick to a certain extent, moreover it is possible to be bonded and be adsorbed by complex reaction
Magnesium ion in magnesia stone, the introducing of metal ion can reinforce the mechanical strength and toughness of organic fiber to a certain extent, have
Conducive to the mechanical strength for improving magnesia carbon brick, reinforces the impact strength of magnesia carbon brick, can also corrode magnesia stone, make magnesia stone table
The degree of roughness in face increases, and the contact area in magnesia stone and magnesia carbon brick between each molecule is improved, to reinforce between each molecule
Crosslinked action, improve magnesia stone mechanical strength, improve the impact strength of magnesia stone, it is difficult to be broken；
(2) present invention carries out energization cell reaction to the fermentation liquid for being mixed with magnesia stone, and magnesium ion in magnesia stone is precipitated in cathode
Magnesium simple substance must be electronically formed, forms ion cavities in magnesia stone, it is positively charged, there is good reproducibility effect, make magnesium carbon
Carbon in brick is difficult to be oxidized decomposition, avoids being damaged by corrosion, while the aluminium ion being added into fermentation liquid passes through energization, in yin
It nearby extremely must be electronically generated nanometer aluminum simple substance, be scattered in magnesia carbon brick, oxygen preferential oxidation is met in carbon surface and generate densification
Aluminum oxide film carbon coated prevents the corrosion that is decomposed, has broad application prospects.
Specific embodiment
It weighs in 600~800g magnesia stone investment planetary ball mill, is mixed under conditions of revolving speed is 500~550r/min
35~45min is ground, grinding product is made, the sodium hydroxide solution that grinding product and mass fraction are 35~45% is pressed into quality
Than placing the beaker in the water-bath that bath temperature is 60~70 DEG C, mixing is made in 2~3h of constant temperature boiling in 1:10 investment beaker
Slurries；Above-mentioned mixed serum is put into filter in suction filtration machine and obtains filter cake, by filter cake 3~5 times wash with distilled water, by weight
Number meter weighs in 8~10 parts of filter cakes, 5~6 parts of soy meals and 13~15 parts of distilled water investment three-necked flasks, with blender with 600
The revolving speed of~620r/min is mixed 40~50min and mixed emulsion is made；Mixed emulsion matter is added into above-mentioned three-necked flask
Three-necked flask is placed in the greenhouse that temperature is 38~42 DEG C by the onion Aspergillus bacterium powder of amount 1.5~1.7%, and constant temperature standing 8~
10 days, nitrogen is full of after standing into three-necked flask, continues constant temperature and stands 3~5 days, mixed emulsion matter is added into three-necked flask
The aluminium chloride crystal powder of amount 6~8% is mixed 3~4h with blender with the revolving speed of 700~720r/min, fermentation is made
Liquid；The sulfuric acid solution 1:5 in mass ratio that above-mentioned fermentation liquid and mass fraction are 30~35% is put into beaker, using aluminium bar as
Anode, platinum stick are as in cathode insertion beaker, and be powered 5~6h under conditions of DC voltage is 40~50V, by platinum after energization
Aluminium powder on stick scrapes in investment beaker, places the beaker in sonic oscillation instrument, under conditions of supersonic frequency is 35~37kHz
It vibrates 50~60min and reaction solution is made；Above-mentioned reaction solution and sawdust 10:1 in mass ratio are put into reaction kettle, into reaction kettle
The sodium hydroxide solution that mass fraction is 18~20% is added dropwise and adjusts pH value to 9.8~10.2,30~40min is stood under room temperature, to
Nitrogen is filled in reaction kettle makes air pressure in kettle be increased to 1.6~1.8MPa, heats reaction kettle, improves temperature in the kettle to 150~160
DEG C, modified filter cake is obtained by filtration after reaction, wash with distilled water filter cake 3~5 times；According to parts by weight, it weighs on 13~15 parts
Modified filter cake, 2.6~2.8 parts of graphite, 0.5~0.7 part of silicon powder, 1.0~1.2 parts of calcium chloride and 8~10 parts of magnesia particles are stated to throw
Enter in blender, is 150~170 DEG C in temperature, 30~40min of mixing is obtained pre- under conditions of revolving speed is 300~320r/min
Mixture processed；Above-mentioned pre-mixture is placed in mold, mold is placed in hot press, is 23~25MPa in compacting pressure,
Temperature suppresses 60~70min under conditions of being 200~220 DEG C, puts into high temperature furnace after compacting, under argon atmosphere and warm
Degree calcines 2~3h under conditions of being 900~1000 DEG C, discharged after natural cooling up to the impact resistance magnesia carbon brick of resistance to oxygen corrosion.
Example 1
The preparation of fermentation liquid:
It weighs in 600g magnesia stone investment planetary ball mill, mixed grinding 35min under conditions of revolving speed is 500r/min is made
Grinding product puts into the sodium hydroxide solution 1:10 in mass ratio that grinding product and mass fraction are 35% in beaker, by beaker
It is placed in the water-bath that bath temperature is 60 DEG C, mixed serum is made in constant temperature boiling 2h；
Above-mentioned mixed serum is put into filter in suction filtration machine and obtains filter cake, by filter cake 3 times wash with distilled water, in parts by weight
Meter weighs in 8 parts of filter cakes, 5 parts of soy meals and 13 parts of distilled water investment three-necked flasks, mixed with the revolving speed of 600r/min with blender
It closes stirring 40min and mixed emulsion is made；
The onion Aspergillus bacterium powder of mixed emulsion quality 1.5% is added into above-mentioned three-necked flask, three-necked flask, which is placed in temperature, is
In 38 DEG C of greenhouse, constant temperature stands 8 days, is full of nitrogen after standing into three-necked flask, continues constant temperature and stands 3 days, burns to three mouthfuls
The aluminium chloride crystal powder of mixed emulsion quality 6% is added in bottle, 3h, system are mixed with the revolving speed of 700r/min with blender
Obtain fermentation liquid；
The preparation of pre-mixture:
The sulfuric acid solution 1:5 in mass ratio that above-mentioned fermentation liquid and mass fraction are 30% is put into beaker, using aluminium bar as sun
Pole, platinum stick are as in cathode insertion beaker, and be powered 5h under conditions of DC voltage is 40V, by the aluminium on platinum stick after energization
Powder scrapes in investment beaker, places the beaker in sonic oscillation instrument, and 50min system is vibrated under conditions of supersonic frequency is 35kHz
Obtain reaction solution；
By in above-mentioned reaction solution and sawdust 10:1 in mass ratio investment reaction kettle, it is 18% that mass fraction is added dropwise into reaction kettle
Sodium hydroxide solution adjusts pH value to 9.8, stands 30min under room temperature, nitrogen is filled with into reaction kettle is increased to air pressure in kettle
1.6MPa heats reaction kettle, improves temperature in the kettle to 150 DEG C, modified filter cake is obtained by filtration after reaction, wash with distilled water filter cake
3 times；
According to parts by weight, 13 parts of above-mentioned modified filter cakes, 2.6 parts of graphite, 0.5 part of silicon powder, 1.0 parts of calcium chloride and 8 parts of magnesium are weighed
Sand particle is put into blender, is 150 DEG C in temperature, mixing 30min obtains prefabricated mixing under conditions of revolving speed is 300r/min
Object；
The preparation of the impact resistance magnesia carbon brick of resistance to oxygen corrosion:
Above-mentioned pre-mixture is placed in mold, mold is placed in hot press, is 23MPa, temperature 200 in compacting pressure
60min is suppressed under conditions of DEG C, is put into high temperature furnace after compacting, under argon atmosphere and under conditions of temperature is 900 DEG C
2h is calcined, is discharged after natural cooling up to the impact resistance magnesia carbon brick of resistance to oxygen corrosion.
Example 2
The preparation of fermentation liquid:
It weighs in 700g magnesia stone investment planetary ball mill, mixed grinding 40min under conditions of revolving speed is 520r/min is made
Grinding product puts into the sodium hydroxide solution 1:10 in mass ratio that grinding product and mass fraction are 40% in beaker, by beaker
It is placed in the water-bath that bath temperature is 65 DEG C, mixed serum is made in constant temperature boiling 2.5h；
Above-mentioned mixed serum is put into filter in suction filtration machine and obtains filter cake, by filter cake 4 times wash with distilled water, in parts by weight
Meter weighs in 9 parts of filter cakes, 5 parts of soy meals and 14 parts of distilled water investment three-necked flasks, mixed with the revolving speed of 610r/min with blender
It closes stirring 45min and mixed emulsion is made；
The onion Aspergillus bacterium powder of mixed emulsion quality 1.6% is added into above-mentioned three-necked flask, three-necked flask, which is placed in temperature, is
In 40 DEG C of greenhouse, constant temperature stands 9 days, is full of nitrogen after standing into three-necked flask, continues constant temperature and stands 4 days, burns to three mouthfuls
The aluminium chloride crystal powder of mixed emulsion quality 7% is added in bottle, 3.5h is mixed with the revolving speed of 710r/min with blender,
Fermentation liquid is made；
The preparation of pre-mixture:
The sulfuric acid solution 1:5 in mass ratio that above-mentioned fermentation liquid and mass fraction are 32% is put into beaker, using aluminium bar as sun
As in cathode insertion beaker, be powered 5.5h under conditions of DC voltage is 45V, will be on platinum stick after energization for pole, platinum stick
Aluminium powder scrapes in investment beaker, places the beaker in sonic oscillation instrument, vibrates 55min under conditions of supersonic frequency is 36kHz
Reaction solution is made；
By in above-mentioned reaction solution and sawdust 10:1 in mass ratio investment reaction kettle, it is 19% that mass fraction is added dropwise into reaction kettle
Sodium hydroxide solution adjusts pH value to 10.0, stands 35min under room temperature, nitrogen is filled with into reaction kettle is increased to air pressure in kettle
1.7MPa heats reaction kettle, improves temperature in the kettle to 155 DEG C, modified filter cake is obtained by filtration after reaction, wash with distilled water filter cake
4 times；
According to parts by weight, 14 parts of above-mentioned modified filter cakes, 2.7 parts of graphite, 0.6 part of silicon powder, 1.1 parts of calcium chloride and 9 parts of magnesium are weighed
Sand particle is put into blender, is 160 DEG C in temperature, mixing 35min obtains prefabricated mixing under conditions of revolving speed is 310r/min
Object；
The preparation of the impact resistance magnesia carbon brick of resistance to oxygen corrosion:
Above-mentioned pre-mixture is placed in mold, mold is placed in hot press, is 24MPa, temperature 210 in compacting pressure
65min is suppressed under conditions of DEG C, is put into high temperature furnace after compacting, under argon atmosphere and under conditions of temperature is 950 DEG C
2.5h is calcined, is discharged after natural cooling up to the impact resistance magnesia carbon brick of resistance to oxygen corrosion.
Example 3
The preparation of fermentation liquid:
It weighs in 800g magnesia stone investment planetary ball mill, mixed grinding 45min under conditions of revolving speed is 550r/min is made
Grinding product puts into the sodium hydroxide solution 1:10 in mass ratio that grinding product and mass fraction are 45% in beaker, by beaker
It is placed in the water-bath that bath temperature is 70 DEG C, mixed serum is made in constant temperature boiling 3h；
Above-mentioned mixed serum is put into filter in suction filtration machine and obtains filter cake, by filter cake 5 times wash with distilled water, in parts by weight
Meter weighs in 10 parts of filter cakes, 6 parts of soy meals and 15 parts of distilled water investment three-necked flasks, with blender with the revolving speed of 620r/min
50min is mixed, mixed emulsion is made；
The onion Aspergillus bacterium powder of mixed emulsion quality 1.7% is added into above-mentioned three-necked flask, three-necked flask, which is placed in temperature, is
In 42 DEG C of greenhouse, constant temperature stands 10 days, is full of nitrogen after standing into three-necked flask, continues constant temperature and stands 5 days, burns to three mouthfuls
The aluminium chloride crystal powder of mixed emulsion quality 8% is added in bottle, 4h, system are mixed with the revolving speed of 720r/min with blender
Obtain fermentation liquid；
The preparation of pre-mixture:
The sulfuric acid solution 1:5 in mass ratio that above-mentioned fermentation liquid and mass fraction are 35% is put into beaker, using aluminium bar as sun
Pole, platinum stick are as in cathode insertion beaker, and be powered 6h under conditions of DC voltage is 50V, by the aluminium on platinum stick after energization
Powder scrapes in investment beaker, places the beaker in sonic oscillation instrument, and 60min system is vibrated under conditions of supersonic frequency is 37kHz
Obtain reaction solution；
By in above-mentioned reaction solution and sawdust 10:1 in mass ratio investment reaction kettle, it is 20% that mass fraction is added dropwise into reaction kettle
Sodium hydroxide solution adjusts pH value to 10.2, stands 40min under room temperature, nitrogen is filled with into reaction kettle is increased to air pressure in kettle
1.8MPa heats reaction kettle, improves temperature in the kettle to 160 DEG C, modified filter cake is obtained by filtration after reaction, wash with distilled water filter cake
5 times；
According to parts by weight, 15 parts of above-mentioned modified filter cakes, 2.8 parts of graphite, 0.7 part of silicon powder, 1.2 parts of calcium chloride and 10 parts of magnesium are weighed
Sand particle is put into blender, is 170 DEG C in temperature, mixing 40min obtains prefabricated mixing under conditions of revolving speed is 320r/min
Object；
The preparation of the impact resistance magnesia carbon brick of resistance to oxygen corrosion:
Above-mentioned pre-mixture is placed in mold, mold is placed in hot press, is 25MPa, temperature 220 in compacting pressure
70min is suppressed under conditions of DEG C, is put into high temperature furnace after compacting, under argon atmosphere and under conditions of temperature is 1000 DEG C
3h is calcined, is discharged after natural cooling up to the impact resistance magnesia carbon brick of resistance to oxygen corrosion.
Comparative example 1: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking fermentation liquid.
Comparative example 2: it is essentially identical with the preparation method of example 2, it has only the difference is that lacking pre-mixture.
Comparative example 3: the impact resistance magnesia carbon brick of resistance to oxygen corrosion of Liaoning company production.
Oxytolerant erosion test: the magnesia carbon brick in example 1~3 and comparative example is placed under the conditions of 1400 DEG C of temperature and is kept the temperature
2h carries out oxidation test in air atmosphere, measures decarburized layer area.
Flexural strength and compressive resistance test are detected by GBT22589-2008 magnesia carbon brick standard.
Anti-thermal shock test；Magnesia carbon brick in example 1~3 and comparative example is placed under the conditions of 1200 DEG C of temperature and is kept the temperature
0.5h carries out thermal shock test, measures remaining flexural strength conservation rate.
1 magnesia carbon brick performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | All than drawing 2 | Comparative example 3 |
| Decarburized layer area (%) | 9 | 9 | 8 | 11 | 15 | 10 |
| Flexural strength (MPa) | 18.9 | 19.0 | 19.2 | 12.3 | 14.8 | 14.9 |
| Compressive resistance (MPa) | 50 | 51 | 52 | 30 | 40 | 41 |
| Remaining flexural strength conservation rate (%) | 93 | 93 | 94 | 80 | 86 | 87 |
Good, the decarburized layer according to the above-mentioned detection data impact resistance magnesia carbon brick of resistance to oxygen corrosion oxytolerant corrosivity produced by the present invention
Area is small, and flexural strength and compressive resistance are high, and after thermal shock test, remaining High anti bending strength, shock resistance is good, has wide
Application prospect.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of the impact resistance magnesia carbon brick of resistance to oxygen corrosion, it is characterised in that specific preparation step are as follows:
Pre-mixture is placed in mold, mold is placed in hot press, is 23~25MPa, temperature 200 in compacting pressure
Under conditions of~220 DEG C suppress 60~70min, after compacting put into high temperature furnace in, under argon atmosphere and temperature be 900~
2~3h is calcined under conditions of 1000 DEG C, is discharged after natural cooling up to the impact resistance magnesia carbon brick of resistance to oxygen corrosion；
The specific preparation step of the pre-mixture are as follows:
(1) sulfuric acid solution that fermentation liquid and mass fraction are 30~35% is put into beaker, is made aluminium bar as anode, platinum stick
It is inserted into beaker for cathode, be powered 5~6h under conditions of DC voltage is 40~50V, by the aluminium powder on platinum stick after energization
Scrape investment beaker in, place the beaker in sonic oscillation instrument, supersonic frequency be 35~37kHz under conditions of oscillation 50~
Reaction solution is made in 60min；
(2) by reaction solution and sawdust investment reaction kettle, it is molten that the sodium hydroxide that mass fraction is 18~20% is added dropwise into reaction kettle
Liquid adjusts pH value to 9.8~10.2,30~40min is stood under room temperature, nitrogen is filled with into reaction kettle is increased to air pressure in kettle
1.6~1.8MPa heats reaction kettle, improves temperature in the kettle to 150~160 DEG C, modified filter cake is obtained by filtration after reaction, with distillation
Water cleans filter cake 3~5 times；
(3) it weighs in modified filter cake, graphite, silicon powder, calcium chloride and magnesia particle investment blender, is 150~170 in temperature
DEG C, 30~40min of mixing obtains pre-mixture under conditions of revolving speed is 300~320r/min；
The specific preparation step of the fermentation liquid are as follows:
(1) it weighs in 600~800g magnesia stone investment planetary ball mill, is mixed under conditions of revolving speed is 500~550r/min
35~45min is ground, grinding product is made, the sodium hydroxide solution that grinding product and mass fraction are 35~45% is put into and is burnt
In cup, place the beaker in the water-bath that bath temperature is 60~70 DEG C, mixed serum is made in 2~3h of constant temperature boiling；
(2) will mixed serum put into suction filtration machine in filter obtain filter cake, by filter cake 3~5 times wash with distilled water, weigh filter cake,
In soy meal and distilled water investment three-necked flask, 40~50min system is mixed with the revolving speed of 600~620r/min with blender
Obtain mixed emulsion；
(3) onion Aspergillus bacterium powder is added into three-necked flask, three-necked flask is placed in the greenhouse that temperature is 38~42 DEG C, it is permanent
Temperature stands 8~10 days, is full of nitrogen after standing into three-necked flask, continues constant temperature and stands 3~5 days, is added into three-necked flask
3~4h is mixed with blender with the revolving speed of 700~720r/min in the aluminium chloride crystal powder of mixed emulsion quality 6~8%,
Fermentation liquid is made.
2. a kind of preparation method of impact resistance magnesia carbon brick of resistance to oxygen corrosion according to claim 1, it is characterised in that: prefabricated
The mass ratio for the sulfuric acid solution that fermentation liquid described in the specific preparation step (1) of mixture is 30~35% with mass fraction is
1:5。
3. a kind of preparation method of impact resistance magnesia carbon brick of resistance to oxygen corrosion according to claim 1, it is characterised in that: prefabricated
The mass ratio of reaction solution described in the specific preparation step (2) of mixture and sawdust is 10:1.
4. a kind of preparation method of impact resistance magnesia carbon brick of resistance to oxygen corrosion according to claim 1, it is characterised in that: prefabricated
In the specific preparation step (3) of mixture preferably according to parts by weight, the modification filter cake is 13~15 parts, graphite is
2.6~2.8 parts, silicon powder be 0.5~0.7 part, calcium chloride is 1.0~1.2 parts, magnesia particle is 8~10 parts.
5. a kind of preparation method of impact resistance magnesia carbon brick of resistance to oxygen corrosion according to claim 1, it is characterised in that: fermentation
The mass ratio for the sodium hydroxide solution that grinding product described in the specific preparation step (1) of liquid and mass fraction are 35~45%
For 1:10.
6. a kind of preparation method of impact resistance magnesia carbon brick of resistance to oxygen corrosion according to claim 1, it is characterised in that: fermentation
In the specific preparation step (2) of liquid preferably according to parts by weight, the filter cake is 8~10 parts, soy meal is 5~6 parts, steams
Distilled water is 13~15 parts.
7. a kind of preparation method of impact resistance magnesia carbon brick of resistance to oxygen corrosion according to claim 1, it is characterised in that: fermentation
The quality for the onion Aspergillus bacterium powder being added described in the specific preparation step (3) of liquid into three-necked flask is mixed emulsion matter
The 1.5~1.7% of amount.
8. a kind of preparation method of impact resistance magnesia carbon brick of resistance to oxygen corrosion according to claim 1, it is characterised in that: fermentation
The quality for the aluminium chloride crystal powder being added described in the specific preparation step (3) of liquid into three-necked flask is mixed emulsion matter
The 6~8% of amount.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111682211A (en) * | 2020-05-29 | 2020-09-18 | 华南理工大学 | Soybean protein based double-crosslinking self-healing supermolecule sulfur anode aqueous binder and preparation method and application thereof |
| CN117285344A (en) * | 2023-09-21 | 2023-12-26 | 株洲火炬安泰新材料有限公司 | IGZO target material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104870398A (en) * | 2013-01-16 | 2015-08-26 | 黑崎播磨株式会社 | Magnesia-carbon brick |
-
2019
- 2019-06-12 CN CN201910505793.5A patent/CN110317070A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104870398A (en) * | 2013-01-16 | 2015-08-26 | 黑崎播磨株式会社 | Magnesia-carbon brick |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111682211A (en) * | 2020-05-29 | 2020-09-18 | 华南理工大学 | Soybean protein based double-crosslinking self-healing supermolecule sulfur anode aqueous binder and preparation method and application thereof |
| CN117285344A (en) * | 2023-09-21 | 2023-12-26 | 株洲火炬安泰新材料有限公司 | IGZO target material and preparation method thereof |
| CN117285344B (en) * | 2023-09-21 | 2024-04-16 | 株洲火炬安泰新材料有限公司 | IGZO target material and preparation method thereof |
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