CN110330320A - A kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon and preparation method thereof - Google Patents

A kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon and preparation method thereof Download PDF

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CN110330320A
CN110330320A CN201910632421.9A CN201910632421A CN110330320A CN 110330320 A CN110330320 A CN 110330320A CN 201910632421 A CN201910632421 A CN 201910632421A CN 110330320 A CN110330320 A CN 110330320A
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carbon
low
ultra
refractory
silicon carbide
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黄军同
张梦
冯志军
胡智辉
李喜宝
闫明格
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Nanchang Hangkong University
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Nanchang Hangkong University
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Abstract

The invention discloses aluminium silicon carbide carbon refractories of a kind of low-carbon Ultra-low carbon and preparation method thereof；Using Al2O3Gathering materials with SiC is aggregate, and crystalline flake graphite, expanded graphite are carbon source, and phenolic resin is bonding agent, additional antioxidant.Wherein: Al2O3Gather materials 75~90wt.%, 3~12wt.% of SiC particulate, 3~6wt.% of phenolic resin, 0.1~4wt.% of carbon raw, 0~1wt.% of nitrate compound, 0.1~3.5wt.% of antioxidant, 0~1wt.% of hard pitch powder.Prepared nitrate alcoholic solution and carbon raw material are poured into phenolic resin be stirred together first, after three rollers grind recirculation gas stripper, obtains micro-nano graphite flake phenolic resin based mixtures, and by Al2O3It is added thereto after particle and SiC particulate are dry-mixed, is eventually adding Al2O3The mixed powder of fine powder, antioxidant and hard pitch composition；After mixing, ageing mixture, compression moulding, solidification to get.The refractory material phosphorus content that the present invention is prepared is low, and has excellent mechanical performance, anti-erosion and thermal shock resistance.

Description

A kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon and preparation method thereof
Technical field
The present invention relates to technical field of refractory materials, and in particular to a kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon And preparation method thereof.
Background technique
Al2O3- SiC-C is the good liner for being mainly used for the molten iron pre-processing device such as fish torpedo type iron mixing vehicle, hot-metal bottle, The erosion that the various desulfurization, dephosphorization, desiliconization agent that use when molten iron pretreatment can be resisted, extends the service life of refractory material. Al2O3Graphite raw material is the critical material of refractory material thermal conductivity with higher and prevention slag infiltration in-SiC-C refractory material, Determine Al2O3The anti-slag and thermal shock resistance of-SiC-C refractory material.At present in Al2O3Ball is used in-SiC-C refractory material more Shape pitch, crystalline flake graphite and new-type carbon black are as carbon source.The wherein antioxygenic property difference and pollution environment of pelletted pitch, and scale Graphite density is small, wetability and bad dispersibility, new-type carbon black then high production cost, be difficult to industrialized production.
But, the higher traditional Al of carbon content2O3There are the following problems for-SiC-C refractory material: (1) carbon content is got over Height, inoxidizability is poor, mechanical strength is lower；(2) high heat conductance caused by high-carbon content will lead to the generation of huge heat loss, make It is larger to obtain temperature drop of the molten iron in transport and preprocessing process, causes the increase of energy consumption and the upset of steel casting process；(3) close A little year graphite are as China's strategic resources, and as exploitation is increasingly stringenter, a large amount of graphite are consumed in high carbon containing refractory In cause the waste of graphite resource；(4) oxidation that avoid these a large amount of graphite/carbons, needs to use a large amount of high price Antioxidant (metal, alloy, carbide), to increase the cost of refractory material.
In order to solve the problems, such as that the above refractory material high-carbon content is brought, the carbon content of carbon containing refractory brick must be reduced to suitable When low-level (carbon graphite of < 5wt%, ideal < 3wt%).Especially in recent years, need of the countries in the world for high-quality steel It asks and greatly develops furnace outer refining process and low-carbon carbon containing refractory is promoted to become research emphasis.Mild steel increasing need Also require carbon content in refractory material low as far as possible, if but directly reduce the additional amount of carbon source, and it can make between oxide particle Contact area increase, cause to be sintered between particle at high temperature, increase the elasticity modulus of refractory material, reduce thermal conductivity Rate thus greatly reduces its thermal shock resistance.Meanwhile with the direct reduction of carbon content, more oxides will mutually be on active service It is directly exposed to that there is rodent liquid metal in the process, so that the original excellent corrosion-resistant property of refractory material is deteriorated, drop The integral high temperature performance of low carbon containing refractory.Therefore, novel carbon source is found, the same of the phosphorus content in refractory material is reduced When guarantee that its high-temperature behavior is nowadays Al again2O3One of key subjects in the research of-SiC-C refractory material.
Summary of the invention
Problem to be solved by this invention is: providing aluminium silicon carbide carbon refractory and its preparation of a kind of low-carbon Ultra-low carbon Method, using crystalline flake graphite, expanded graphite as carbon source, phenolic resin as bonding agent, nitrate compound as catalyst, It continuously removes graphite by three-roll grinder to prepare to form micro-nano graphite flake mixture, as Al2O3- SiC-C fire resisting The carbon source of material can guarantee the continuity degree of carbon in material while reducing the phosphorus content of refractory material, guarantee carbon containing fire resisting Material heat-resistant knocking stability energy and corrosion-resistant property.On the other hand, low-carbon Ultra-low carbon Al2O3- SiC-C refractory material is in military service item Under hot environment under part, nitrate energy catalysed phenolic resin part converted in-situ forms carbon nanotube, promotees from microstructure Into the high temperature resistance of material, extend the service life of material, be conducive to the clean steels such as mild steel, ultra-low-carbon steel production and it is secondary The development of refining techniques.
The present invention in order to solve the above problem provided by technical solution are as follows: a kind of aluminum silicon carbide carbon fire resisting of low-carbon Ultra-low carbon Material, raw material components percentage are as follows: Al2O3Gather materials 75~90wt.%, 3~12wt.% of SiC particulate, 3~6wt.% Phenolic resin binder, the carbon raw of 0.1~4wt.%, the nitrate compound of 0~1wt.%, 0.1~3.5wt.% Antioxidant, 0~1wt.% hard pitch powder；The carbon raw is one of crystalline flake graphite, expanded graphite or two Kind mixture；The nitrate compound is one of nickel nitrate, ferric nitrate, cobalt nitrate or two or more.
Preferably, Al described in raw material components2O3Gather materials for electro-corundum, alundum, superfine bauxite, red column The mixed particle of one or both of stone and fine powder composition, main component Al2O3, and SiO2Content be less than 5wt.%. Al2O375~90wt.% of the total ingredient of the Zhan that gathers materials, wherein 15~25wt.% of the total ingredient of the Zhan of 5~3mm of grain graininess, granularity 3 15~25wt.% of the total ingredient of 30~40wt.% of the total ingredient of the Zhan of~1mm, granularity≤1mm Zhan；Al2O3Gather materials fine powder Granularity≤0.088mm, 15~25wt.% of the total ingredient of Zhan.
Preferably, antioxidant described in raw material components be one of metal Al powder, Si powder, boride or several, Partial size≤0.074mm.
Preferably, the boride is B4C or BN or ZrB2Or CaB6。
A kind of preparation method of the aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon, the preparation method includes following step Suddenly,
(1) nitrate compound of 0~1wt.% is first configured to the alcohol that mass percent concentration is 1~30wt.% Solution；
(2) carbon raw material of prepared nitrate alcoholic solution, 0.1~4wt.% are poured into 3~5wt.% together again Phenolic resin in be stirred 2~18min；
(3) mixture in (2) is then added to three-roll grinder from feed roller and carries out the removing of three roller differentials, circulation stripping After 1~20 time, collects to obtain graphite from discharge roller and remove the micro-nano graphite flake to be formed and be dispersed in containing nitrate Mixture in resin；
(4) viscosity of the resin based mixtures obtained for collection in reduction (3) is to increase mobility, by it 40 DEG C~90 The heating of 5~30min is carried out in DEG C water-bath；
(5) by Al2O315~25wt.% of fine powder, the antioxidant of 0.1~3.5wt.%, 0~1wt.% hard pitch powder It is uniformly mixed, obtains mixing fine powders；
(6) by the Al of the total 75~90wt.% of ingredient of Zhan2O3Al in gathering materials2O3Particle and 3~12wt.%SiC particle are put Enter dry-mixed 1~15min in kneading machine (edge runner-wet mill), then be added (4) in heating after resin based mixtures continue mixing 3~ 15min, the Al being eventually adding in (5)2O3Gather materials, the mixed powder that antioxidant and hard pitch are formed continues 4~15min of mixing Pug is made, then ageing mixture 1~for 24 hours；
(7) pug being stranded is added in mold to use combined type friction press or static pressure is waited to be pressed and is made Adobe；
(8) molding adobe is placed in tunnel drying oven after baking-curing to get the low-carbon Ultra-low carbon is arrived Aluminium silicon carbide carbon refractory.
Preferably, the rotating ratio of three roller rates in the step (3) in three-roll grinder is N3 (feed roller): N2 (in Heart roller): for N1 (discharge roller) within 1:1.5:3~1:3:9, the gap between each roll shaft is 0.01~0.2mm.
Preferably, 150~300 DEG C of baking temperature in the step (8), baking time is 8~36h.
Compared with prior art, the invention has the advantages that with Al2O3Gather materials, SiC particulate, carbon raw, antioxidant, height Warm asphalt powder is starting material, and phenolic resin is bonding agent, and nitrate compound is catalyst.The carbon raw is scale One or two kinds of mixtures of graphite, expanded graphite；The nitrate compound be nickel nitrate, ferric nitrate, cobalt nitrate one Kind is two or more.The phenolic resin based micro-nano graphite flake mixture performance being prepared in the present invention is excellent, cost It is lower, it is used for low-carbon Ultra-low carbon Al2O3- SiC-C refractory material, can be on the basis of keeping or improving its comprehensive performance, significantly Reduce the carbon content and thermal conductivity of carbon containing refractory.On the other hand, the low-carbon Ultra-low carbon Al in the present invention2O3- SiC-C fire resisting Effect energy in-situ preparation carbon nanotube or carbon fiber of the material under the hot conditions of military service through catalyst, change from microstructure The high temperature resistance of kind material, extends the service life of material, has significant effect to energy-saving and emission-reduction, and to China's clean steel The development of refining techniques and high temperature industry has important impetus and practical application value.
Specific embodiment
Carry out the embodiment that the present invention will be described in detail below in conjunction with embodiment, whereby to the present invention how application technology hand Section solves technical problem and reaches the realization process of technical effect to fully understand and implement.
Embodiment 1
A kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon and preparation method thereof.3wt.% crystalline flake graphite is poured into It is stirred in 4wt.% phenolic resin, (rotating ratio of three roller rates in three-roll grinder is N3 after recirculation gas stripper 18 times (feed roller): N2 (breast roll): N1 (discharge roller) is 1:2:4, and the gap between feed roller and breast roll is 0.08mm, breast roll Gap between discharge roller is 0.02mm)；It obtains micro-nano graphite flake and is dispersed in mixing in the resin containing nitrate Object is closed, it is heated to 25min in 40 DEG C of water-baths to increase its mobility.Then (wherein by 62wt.% electro-corundum particle The 16wt.% of the total ingredient of Zhan of 5~3mm of grain granularity, the 30wt.% of the total ingredient of the Zhan of 3~1mm of granularity, granularity≤1mm Zhan are total The 16wt.% of ingredient) and the 12wt.%SiC particle resin that is put into dry-mixed 15min in kneading machine (edge runner-wet mill) and is added after heating Based mixtures continue to be kneaded 10min, are eventually adding 17wt.% electro-corundum fine powder partial size (≤0.074mm), 2wt.%Al powder group At mixed powder continue to be kneaded 15min pug and ageing mixture 20h be made.The pug being stranded is added in mold and uses combined type friction Brick machine be pressed be made adobe be placed in tunnel drying oven 36h solidification is toasted at 250 DEG C after to get to institute The aluminum silicon carbide carbon carbon containing refractory for the low-carbon stated.
A kind of preparation-obtained low-carbon Al2O3The technical indicator of-SiC-C fire resistive material product is as follows: carbon content is 5.2%, bulk density 3.12g/cm3, apparent porosity 8.2%, thermal conductivity is 6.2W/ (mK), cold crushing strength 72.6MPa, high temperature break resistant intensity (1400 DEG C of * 3h) 14.5MPa, thermal shock resistance number 16.
Embodiment 2
A kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon and preparation method thereof.First by the nitric acid salinization of 0.8wt.% The alcoholic solution that object compound concentration is 25wt.% is closed, then by prepared nitrate alcoholic solution and 0.5wt.% expanded graphite Pour into 4.8wt.% phenolic resin and be stirred together, after recirculation gas stripper 18 times (three roller rates in three-roll grinder Rotating ratio is N3 (feed roller): N2 (breast roll): N1 (discharge roller) is 1:3:6, and the gap between feed roller and breast roll is 0.1mm, the gap between breast roll and discharge roller are 0.01mm), it obtains micro-nano graphite flake and is dispersed in containing nitrate Resin in mixture, it is heated to 20min in 55 DEG C of water-baths to increase its mobility.Then by 61.6wt.% superfine Bauxite particle be (the total ingredient of the wherein 15wt.% of the total ingredient of the Zhan of 5~3mm of grain graininess, the Zhan of 3~1mm of granularity The 15wt.% of the total ingredient of 31.6wt.%, granularity≤1mm Zhan) and 12wt.%SiC particle be put into dry-mixed 10min in kneading machine And the resin based mixtures being added after heating continue to be kneaded 13min, are eventually adding 16wt.% superfine bauxite fine powder partial size (≤0.074mm), 1.5wt.%Al powder, 1.9wt.%Si powder and 0.9wt.% hard pitch composition mixed powder continue to be kneaded Pug and ageing mixture 18h is made in 10min.The pug being stranded is added in mold and is pressed using combined type friction press Adobe is made and is placed in the aluminium carbonization toasted at 280 DEG C in tunnel drying oven and arrive the Ultra-low carbon after 32h solidifies Silicon-carbon carbon containing refractory.
A kind of preparation-obtained Ultra-low carbon Al2O3The technical indicator of-SiC-C fire resistive material product is as follows: carbon content is 3.9%, bulk density 3.18g/cm3, apparent porosity 6.5%, thermal conductivity is 5.7W/ (mK), cold crushing strength 92.6MPa, high temperature break resistant intensity (1400 DEG C of * 3h) 16.5MPa, thermal shock resistance number 15.
Embodiment 3
A kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon and preparation method thereof.First by the nitrate of 0.15wt.% Compound compound concentration is the alcoholic solution of 25wt.%, then by prepared nitrate alcoholic solution and 1.5wt.% scale stone Ink, which is poured into together in 3.5wt.% phenolic resin, to be stirred, (the three roller rates in three-roll grinder after recirculation gas stripper 18 times Rotating ratio be N3 (feed roller): N2 (breast roll): N1 (discharge roller) is 1:3:6, and the gap between feed roller and breast roll is 0.06mm, the gap between breast roll and discharge roller are 0.01mm), it obtains micro-nano graphite flake and is dispersed in containing nitrate Resin in mixture, it is heated to 10min in 80 DEG C of water-baths to increase its mobility.Then 72wt.% is sintered rigid Beautiful particle (36wt.% of the total ingredient of the wherein 18wt.% of the total ingredient of the Zhan of 5~3mm of grain graininess, the Zhan of 3~1mm of granularity, grain The 18wt.% of the total ingredient of degree≤1mm Zhan) and 4.4wt.%SiC particle be put into kneading machine (edge runner-wet mill) dry-mixed 15min and add Enter heating after resin based mixtures continue be kneaded 12min, be eventually adding 18wt.% andalusite fine powder partial size (≤0.074mm), The mixed powder that 0.1wt.%Al powder, 0.1wt.%Si powder, 0.1wt.%BN and 0.15wt.% hard pitch form continues to be kneaded Pug and ageing mixture 22h is made in 13min.The pug being stranded is added in mold and is pressed using combined type friction press Adobe is made and is placed in the aluminium carbonization toasted at 300 DEG C in tunnel drying oven and arrive the Ultra-low carbon after 28h solidifies Silicon-carbon carbon containing refractory.
A kind of preparation-obtained Ultra-low carbon Al2O3The technical indicator of-SiC-C fire resistive material product is as follows: carbon content is 3.1%, bulk density 3.22g/cm3, apparent porosity 5.7%, thermal conductivity is 5.0W/ (mK), cold crushing strength 102.6MPa, high temperature break resistant intensity (1400 DEG C of * 3h) 17.1MPa, thermal shock resistance number 14.
Only highly preferred embodiment of the present invention is described above, but is not to be construed as limiting the scope of the invention.This Invention is not only limited to above embodiments, and specific structure is allowed to vary.All protection models in independent claims of the present invention Interior made various change is enclosed to all fall in the scope of protection of the present invention.

Claims (7)

1. a kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon, it is characterised in that: raw material components percentage are as follows: Al2O3Gather materials 75~90wt.%, 3~12wt.% of SiC particulate, the phenolic resin binder of 3~6wt.%, 0.1~4wt.% Carbon raw, the nitrate compound of 0~1wt.%, 0.1~3.5wt.% antioxidant, 0~1wt.% hard pitch powder； The carbon raw is one or both of crystalline flake graphite, expanded graphite mixture；The nitrate compound is nitre One of sour nickel, ferric nitrate, cobalt nitrate are two or more.
2. a kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon according to claim 1, it is characterised in that: raw material group Al described in point2O3Gather materials for the mixing of one or both of electro-corundum, alundum, superfine bauxite, andalusite Particle and fine powder composition, main component Al2O3, and SiO2Content be less than 5wt.%.Al2O3The 75 of the total ingredient of the Zhan that gathers materials~ 90wt.%, wherein 15~25wt.% of the total ingredient of the Zhan of 5~3mm of grain graininess, the total ingredient of the Zhan of 3~1mm of granularity 30~ 15~25wt.% of the total ingredient of 40wt.%, granularity≤1mm Zhan；Al2O3Gather materials granularity≤0.088mm of fine powder, the total ingredient of Zhan 15~25wt.%.
3. a kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon according to claim 1, it is characterised in that: raw material group Antioxidant described in point is one of metal Al powder, Si powder, boride or several, partial size≤0.074mm.
4. a kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon according to claim 3, it is characterised in that: the boron Compound is B4C or BN or ZrB2Or CaB6。
5. a kind of preparation method of the aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon as described in Claims 1-4 is any, Be characterized in that: the preparation method comprises the following steps,
(1) nitrate compound of 0~1wt.% is first configured to the alcoholic solution that mass percent concentration is 1~30wt.%；
(2) carbon raw material of prepared nitrate alcoholic solution, 0.1~4wt.% is poured into the phenol of 3~5wt.% together again 2~18min is stirred in urea formaldehyde；
(3) mixture in (2) is then added to three-roll grinder from feed roller and carries out the removing of three roller differentials, recirculation gas stripper 1 After~20 times, collects to obtain graphite from discharge roller and remove the micro-nano graphite flake to be formed and be dispersed in the resin containing nitrate In mixture；
(4) viscosity of the resin based mixtures obtained for collection in reduction (3) is to increase mobility, by it in 40 DEG C~90 DEG C water The heating of 5~30min is carried out in bath；
(5) by Al2O315~25wt.% of fine powder, the antioxidant of 0.1~3.5wt.%, the mixing of 0~1wt.% hard pitch powder Uniformly, mixing fine powders are obtained；
(6) by the Al of the total 75~90wt.% of ingredient of Zhan2O3Al in gathering materials2O3Particle and 3~12wt.%SiC particle are put into mixing Dry-mixed 1~15min in machine (edge runner-wet mill) is then added the resin based mixtures in (4) after heating and continues 3~15min of mixing, most The Al in (5) is added afterwards2O3Gather materials, the mixed powder that antioxidant and hard pitch are formed continues 4~15min of mixing pug is made, Then ageing mixture 1~for 24 hours；
(7) pug being stranded is added in mold to use combined type friction press or static pressure is waited to be pressed and brick is made Base；
(8) molding adobe is placed in tunnel drying oven after baking-curing to the aluminium carbon for arriving the low-carbon Ultra-low carbon SiClx carbon refractory.
6. a kind of preparation method of the aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon according to claim 5, feature Be: the rotating ratio of three roller rates in the step (3) in three-roll grinder is N3 (feed roller): N2 (breast roll): N1 is (out Expect roller) within 1:1.5:3~1:3:9, the gap between each roll shaft is 0.01~0.2mm.
7. a kind of preparation method of the aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon according to claim 5, feature Be: 150~300 DEG C of baking temperature in the step (8), baking time is 8~36h.
CN201910632421.9A 2019-07-13 2019-07-13 A kind of aluminium silicon carbide carbon refractory of low-carbon Ultra-low carbon and preparation method thereof Pending CN110330320A (en)

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CN111777417A (en) * 2020-07-29 2020-10-16 攀钢冶金材料有限责任公司 Silicon carbide-carbon ramming mass for blast furnace slag high-temperature carbonization electric furnace and preparation method thereof
CN112390650A (en) * 2020-11-17 2021-02-23 宜兴瑞泰耐火材料工程有限公司 High-density high-oxidation-resistance silicon carbide brick for incinerator and preparation process thereof
CN112390650B (en) * 2020-11-17 2022-08-19 宜兴瑞泰耐火材料工程有限公司 High-density high-oxidation-resistance silicon carbide brick for incinerator and preparation process thereof
CN113981336A (en) * 2021-09-30 2022-01-28 深圳市联域光电股份有限公司 Aluminum alloy composite heat dissipation material containing carbide/graphene sandwich structure for LED lamp and preparation method thereof
CN113981336B (en) * 2021-09-30 2022-11-22 深圳市联域光电股份有限公司 Aluminum alloy composite heat dissipation material containing carbide/graphene sandwich structure for LED lamp and preparation method thereof
CN115637158A (en) * 2022-12-23 2023-01-24 华北理工大学 Expanded graphite/carbon nanotube composite material and preparation method and application thereof
CN115925397A (en) * 2022-12-30 2023-04-07 江苏集萃安泰创明先进能源材料研究院有限公司 Stopper rod body, stopper rod and preparation method thereof
CN115925397B (en) * 2022-12-30 2024-01-23 江苏集萃安泰创明先进能源材料研究院有限公司 Stopper rod body, stopper rod and preparation method of stopper rod
CN117383949A (en) * 2023-11-10 2024-01-12 江苏君耀耐磨耐火材料有限公司 Preparation method of carbon nanofiber toughened refractory material
CN117383949B (en) * 2023-11-10 2024-04-02 江苏君耀耐磨耐火材料有限公司 Preparation method of carbon nanofiber toughened refractory material
CN117466645A (en) * 2023-12-27 2024-01-30 之江实验室 Aluminum silicide whisker and preparation method thereof

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