CN106699208A - Carbon fiber toughening refractory castable for molten iron desulphurization spray gun and preparation method of carbon fiber toughening refractory castable - Google Patents

Carbon fiber toughening refractory castable for molten iron desulphurization spray gun and preparation method of carbon fiber toughening refractory castable Download PDF

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Publication number
CN106699208A
CN106699208A CN201710010056.9A CN201710010056A CN106699208A CN 106699208 A CN106699208 A CN 106699208A CN 201710010056 A CN201710010056 A CN 201710010056A CN 106699208 A CN106699208 A CN 106699208A
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China
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carbon fiber
spray gun
molten iron
parts
quality
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CN106699208B (en
Inventor
李远兵
欧阳思
李淑静
向若飞
徐娜娜
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Wuhan University of Science and Engineering WUSE
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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
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C1/00—Refining of pig-iron; Cast iron
    • C21C1/02—Dephosphorising or desulfurising
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04—Removing impurities by adding a treating agent
    • C21C7/064—Dephosphorising; Desulfurising

Abstract

The invention relates to carbon fiber toughening refractory castable for a molten iron desulphurization spray gun and a preparation method of the carbon fiber toughening refractory castable. According to the technical scheme, the preparation method comprises the following steps of: firstly, scattering 2-4 parts by mass of high-purity electric smelting mullite powder, 5-10 parts by mass of electric smelting dense corundum fine powder, 2-5 parts by mass of alpha-Al2O3 micro powder, 5-8 parts by mass of rho-Al2O3 micro powder, 3-7 parts by mass of silicon micro-powder, 1-4 parts by mass of silicon carbide powder and 1.5-3 parts by mass of pure calcium aluminate cement and an additive into a flat container, and uniformly mixing; furthermore, scattering 35-48 parts by mass of natural electric smelting mullite, 20-30 parts by mass of andalusite and 3-6 parts by mass of high-purity electric smelting mullite granules into the flat container, and uniformly mixing; further pouring into a stirring machine, and uniformly stirring, thereby obtaining the carbon fiber toughening refractory castable. The carbon fiber toughening refractory castable is low in cost and wide in raw material source, a prepared product is good in thermal shock resistance, the service life of the molten iron desulphurization spray gun can be prolonged, the use temperature of the molten iron desulphurization spray gun can be increased, and the use cost of the molten iron desulphurization spray gun can be lowered.

Description

Molten iron desulfuring spray gun carbon fiber-reinforced castable refractory and preparation method thereof
Technical field
The present invention relates to molten iron injection pretreating spray gun technical field of refractory castable.Specifically related to a kind of desulfurizing iron Spray gun carbon fiber-reinforced castable refractory and preparation method thereof.
Background technology
It, to the deep containers conveying for loading high temperature liquid iron and the instrument of injection pretreating agent, is main that hot metal pretreatment spray gun is The complex structure to be made up of metal gun core and fire proofed wood spray gun lining.Wherein, the Main Function of metal gun core is to ensure spray gun Intensity, rigidity, injection passage it is unimpeded with injection flow field stabilization；Fire proofed wood spray gun lining Main Function be fire resisting, it is heat-insulated, Anti-erosion is washed away with iron-resistant water, prevents metal gun core high temperature deformation, melting loss, oxidation and ablation.Used in the batch (-type) of spray gun During, the high temperature that subject molten iron and slag with the fire proofed wood spray gun of molten iron directly contact lining washes away, mechanical wear, chemical erosion Replace with frequent rapid heat cycle, therefore, fire proofed wood spray gun lining requires there is good high-temperature mechanics intensity, chemerosiveness resistent and heat Shake stability.
Hot metal pretreatment spray gun fire proofed wood spray gun lining is main both at home and abroad at present is poured using Stainless-steel fibre mullite corundum matter Prepared by material feeding, such as：" Commission Office reason ィ Application ヅ ユ Network シ ヨ Application ラ Application ス is given in molten milling "（Clear 61-99614）One kind is disclosed with rich aluminium Electrofused mullite, corundum are the spray gun castable refractory of main raw material(s), by adding carborundum, carbon materials, magnesia powder And magnesium aluminate spinel, improve the erosion-resisting characteristics of castable；By selecting fritting columnar ceramic aggregate, the anti-impact of pouring layer is improved Corrosion energy；By adding steel fibre, castable mechanical property and thermal shock resistance energy are improved, but do not report that its practical application is imitated Really.A kind of pretreating spray gun（Quan Rong, king keeps improvement [J] foreign countries refractory material of power hot metal pretreatment spray guns, 2004,6: 24-28）, it was recently reported that Xin iron companies Wu Chang passes through on the basis of conventional steel fiber enhancing mullite corundum matter castable The means such as the optimization of refractory casting material granularity, increase coarse grain addition, increasing moulding by casting oscillation intensity, improve fire proofed wood spray gun lining Packing and bond strength, and in actual production, make spray gun average life by 8 times/（The min/ of soak time 280 Branch）Bring up to 14.3 times/（Soak time 500min/ branch）." refractory castable for molten iron pretreatment spray gun " （ZL201010167938.4）A kind of refractory castable for molten iron pretreatment spray gun is disclosed, by castable base-material and additive group Into.Wherein castable base-material by 30 ~ 40% sintering zirconium mullite, 10 ~ 20% flint clay, 20 ~ 30% andalusite, 5 ~ 10% Dense alumina fine powder, 2 ~ 5% α-Al2O3Micro mist, 5 ~ 8% ρ-Al2O3Micro mist, 3 ~ 7% silicon powder, 1 ~ 4% carborundum powder, 1.5 ~ 3% pure calcium aluminate cement composition；Described additive is pressed with the gross weight M of described castable base-material as mete-wand Weight by the heat-resistant steel fiber of 1 ~ 5%M, the polypropylene fibre of 0 ~ 0.1%M, the aluctyl of 0 ~ 0.5%M, 0 ~ 0.5%M metallic aluminium The melamine composition of powder, the sodium tripolyphosphate of 0 ~ 0.15%M and 0 ~ 0.5%M；And achieved in actual production extension spray gun make With the certain effect in life-span.
With the continuous improvement of steel products quality requirement, the continuous progress of hot metal transport technology is pre-processed pure to molten iron The requirement of cleanliness is improved constantly, and molten iron pretreatment temperature is also improved constantly, and molten iron highest pretreatment temperature is led more than 1500 DEG C Molten iron single injection pretreatment time is caused significantly to extend, spray gun use condition drastically deteriorates.Further, since castable under high temperature The middle oxidizable expansion of steel fibre, weakens the interface cohesion of steel fibre and castable matrix, has encouraged the formation of castable crackle With development.Meanwhile, the high-temperature fusion of steel fibre weakens the drawing activeness and quietness effect of steel fibre, resistance to so as to exacerbate spray gun The crackle of fiery material rifle lining is peeled off and erosive wear, and especially when molten iron temperature is more than 1350 DEG C, steel fibre oxidation, corrode are acute Strong, activeness and quietness effect is significantly reduced, and causes spray gun service life drastically to decline.
As can be seen here, the conventional rifle lining castable refractory technology of current spray gun reduces spray gun to iron because adding steel fibre The adaptability of water high temperature, reduces the service life of spray gun, constrains the practical application effect of spray gun, increased desulfurization into This.
The content of the invention
It is contemplated that overcoming prior art defect, it is therefore an objective to provide a kind of with low cost and extensive iron of raw material sources Water desulfuring spray gun is with carbon fiber-reinforced refractory casting preparation method for material.The molten iron desulfuring spray gun prepared with the method is increased with carbon fiber Tough castable refractory good thermal shock stability, can extend molten iron desulfuring spray gun service life, improve molten iron desulfuring spray gun use The use cost of temperature and reduction molten iron desulfuring spray gun.
To achieve the above object, the technical solution adopted in the present invention is：
The molten iron desulfuring spray gun is with the composition and its mass fraction of carbon fiber-reinforced castable refractory：With 35 ~ 48 parts of quality Natural electrofused mullite, the andalusite of 20 ~ 30 parts of quality, high-purity fused mullite particle, 2 ~ 4 parts of quality of 3 ~ 6 parts of quality High-purity fused mullite powder, the electric smelting dense alumina fine powder of 5 ~ 10 parts of quality, the α-Al of 2 ~ 5 parts of quality2O3Micro mist, 5 ~ 8 parts ρ-the Al of quality2O3Micro mist, the silicon powder of 3 ~ 7 parts of quality, the carborundum powder of 1 ~ 4 part of quality, the pure calcium aluminate of 1.5 ~ 3 parts of quality Cement is raw material；With 0.4 ~ 1.7 part of carbon fiber of quality, the silica flour of 0.5 ~ 3 part of quality, 0.05 ~ 0.15 part of quality polypropylene Fiber, 0.04 ~ 0.07 part of carboxymethylcellulose calcium of quality, the defoamer of 0.01 ~ 0.08 part of quality and 0.1 ~ 0.45 part of quality Water reducer is additive.
The carbon fiber is chopped carbon fiber or is chopped carbon fiber and the mixture of carbon fiber powder.
The molten iron desulfuring spray gun is with the preparation method of carbon fiber-reinforced castable refractory：
The first step, according to the molten iron desulfuring spray gun composition and its mass fraction of carbon fiber-reinforced castable refractory, first will High-purity fused mullite powder, electric smelting dense alumina fine powder, α-Al2O3Micro mist, ρ-Al2O3It is micro mist, silicon powder, carborundum powder, pure Aluminous cement, carbon fiber, silica flour, polypropylene fibre, carboxymethylcellulose calcium, defoamer and water reducer point are spread to Flat bottom container It is interior, intersected with rake vertical and horizontal and take off rake 20 ~ 30 minutes.
Second step, according to the molten iron desulfuring spray gun composition and its mass fraction of carbon fiber-reinforced castable refractory, Natural electrofused mullite, andalusite and high-purity fused mullite particle point are spread in the Flat bottom container, with rake longitudinal direction and Lateral cross takes off rake uniformly, pours into mixer, stirs, and obtains final product the carbon fiber-reinforced refractory casting of molten iron desulfuring spray gun Material.
The main chemical compositions of the natural electrofused mullite are：Al2O3It is 66 ~ 75wt%, SiO2It is 20 ~ 28wt%, TiO2 It is 2.5 ~ 3.0wt%.The grain composition of the natural electrofused mullite is：Particle diameter for 3 ~ 5mm account for natural electrofused mullite 28 ~ 35wt%, particle diameter accounts for natural 28 ~ 35wt% of electrofused mullite more than 5mm and less than or equal to 10mm, particle diameter more than 10mm and less than etc. Natural 30 ~ 40wt% of electrofused mullite is accounted in 20mm.
The main chemical compositions of the andalusite are：Al2O3>=58wt%, SiO2It is 20 ~ 28wt%.The andalusite Grade is matched somebody with somebody：Particle diameter accounts for 60 ~ 70wt% of andalusite for 0.15 ~ 1mm, particle diameter more than 1mm and less than or equal to 3mm account for andalusite 30 ~ 40wt%。
The main chemical compositions of the high-purity fused mullite are：Al2O3It is 72 ~ 79wt%, SiO2It is 19 ~ 27wt%.It is described The particle diameter of high-purity fused mullite particle is 0.15 ~ 1mm, the high-purity fused mullite diameter of particle≤0.044mm.
The Al of the electric smelting dense alumina fine powder2O3Content >=98.6wt%；The particle diameter of electric smelting dense alumina fine powder≤ 0.044mm。
A diameter of 5 ~ 9 μm of the chopped carbon fiber, length is 1 ~ 3mm；Carbon content >=the 95wt% of chopped carbon fiber.
A diameter of 5 ~ 9 μm of the carbon fiber powder, length≤0.282mm；Carbon content >=the 95wt% of carbon fiber powder.
SiC content >=the 97wt% of the carborundum powder；Particle diameter≤the 0.044mm of carborundum powder.
Si contents >=the 98wt% of the silica flour；Particle diameter≤the 0.088mm of silica flour.
The SiO of the silicon powder2Content >=94wt%；Particle diameter≤3 μm of silicon powder.
The length of the polypropylene fibre is 3 ~ 5mm, a diameter of 110 ~ 120 μm；The fusing point of polypropylene fibre is 115 ± 5 ℃。
The water reducer is the mixture of sodium tripolyphosphate and FS20.
Application method of the invention is：Prepared molten iron desulfuring spray gun is poured into carbon fiber-reinforced castable refractory and is stirred 5 ~ 6 parts of water of quality of addition in machine are mixed, 3 ~ 6min is stirred, then poured into spray gun fire proofed wood spray gun liner in pouring mould, vibration moulding, Obtain final product molten iron desulfuring spray gun.
The beneficial effects of the present invention are：
（1）The various raw material that the present invention is used are the conventional raw materials of refractory material, and originating, quite varied and price is relatively low, therefore Low production cost, and the technique that the present invention is sent out involved by preparation method is also relatively simple.
（2）The carbon fiber that the present invention is used is a kind of phosphorus content in the high intensity of more than 95wt%, the tencel of high-modulus Material, its density ratio aluminium is low, but intensity is higher than steel, and with corrosion-resistant, high-modulus, without under creep, non-oxidizing atmosphere Superhigh temperature resistant and fatigue proof characteristic.By the carbon fiber for mixing the chopped carbon fiber and≤0.282mm for adding length to be 1 ~ 3mm Powder, it is to avoid the winding conglomeration caused because fiber is long in carbon fiber dispersion process, it is ensured that chopped carbon fiber and carbon fiber powder It is dispersed, realize the composite strengthening toughening effect of different draw ratio carbon fibers.
（3）The Application of composite that the present invention passes through natural electrofused mullite and high-purity fused mullite, using two kinds of thermal expansions The low mullite performance difference of coefficient and complex effect, improve molten iron desulfuring spray gun with carbon fiber-reinforced castable refractory thermal shock Stability；The excellent high-temperature behavior of high-purity fused mullite extends molten iron desulfuring spray gun with carbon fiber-reinforced castable refractory Sintering range, to adapt to the spray gun performance requirement of blowing desulfurization under the conditions of high temperature liquid iron.It is excellent using gelling property ρ-Al2O3Micro mist is main bonding agent and silicon powder, α-Al2O3Micro mist and pure calcium aluminate cement are auxiliary bonding agent, so as to drop CaO content in low castable, improves molten iron desulfuring spray gun strong with high temperature with the erosion-resisting characteristics of carbon fiber-reinforced castable refractory Degree.Microcrack evolution equation is produced by the high-temperature expansion of andalusite, molten iron desulfuring spray gun is further increased with carbon fiber-reinforced resistance to The thermal shock resistance of fiery castable, have adjusted Linear change rate after high temperature burns.By the use of polypropylene fibre in additive, improve Molten iron desulfuring spray gun is served as a contrast with the explosion-proof performance of carbon fiber-reinforced castable refractory baking process and spray gun fire proofed wood spray gun Globality.
（4）The addition that the present invention passes through silica flour, prevents the high-temperature oxydation ablation of carbon fiber, in the range of silica flour addition, Under the conditions of air atmosphere and 1450 DEG C × 3h be heat-treated after sample under ESEM it is clearly discernible go out residual carbon fiber, So as to the long-acting activeness and quietness that ensure that the carbon fiber-reinforced castable refractory of molten iron desulfuring spray gun is acted on.
（5）The present invention reduces amount of water by sodium tripolyphosphate and the compound use of FS20, improves desulfurizing iron spray The rifle mobile performance of carbon fiber-reinforced castable refractory, workability and the closely knit performance of cast.By carboxymethylcellulose calcium From, improve the wellability and dispersiveness of chopped carbon fiber, overcome the shortcomings of that carbon fiber water infiltration is difficult, reinforced carbon fiber with pour Being tightly combined property and its activeness and quietness effect between material feeding matrix.By the selection of defoamer, it is to avoid in the whipping process that adds water The formation of bubble, reduces amount of water of the molten iron desulfuring spray gun with carbon fiber-reinforced castable refractory, improves mobility, improves Packing and mechanical strength.
（6）Reasonable selection and its weight proportion and the optimization of preparation technology of the present invention by various raw material, realize Being obviously improved for castable thermal shock resistance energy, reaches the mesh for improving molten iron desulfuring spray gun temperature in use and increasing the service life 's.The uniform mixing of various raw materials and additive is ensure that in preparation process, especially the uniform mixing of carbon fiber, anti-blocking The group of twining in fiber blending processes knots.
（7）The present invention further extends molten iron on the basis of thermal shock resistance, corrosion resistance and mechanical strength is improved The service life of desulfuring spray gun；Steel fibre is replaced by carbon fiber, molten iron desulfuring spray gun temperature in use is further increased, so that Reduce molten iron desulfuring spray gun and change the frequency repaired with workman, reduce the use cost of molten iron desulfuring spray gun.
The present invention prepare molten iron desulfuring spray gun with carbon fiber-reinforced castable refractory compared with conventional steel fiber castable, Rupture strength of the product of preparation after 110 DEG C × 24h and 1450 DEG C × 3h heat treatments improves 10 ~ 15%, and thermal shock water-cooled number of times is carried High by 50%, maximum operation (service) temperature improves 100 DEG C.
Therefore, extensively, prepared molten iron desulfuring spray gun is with carbon fiber-reinforced for the with low cost and raw material sources of the present invention Castable refractory good thermal shock stability, the service life that molten iron desulfuring spray gun can be extended, the use temperature for improving molten iron desulfuring spray gun The use cost of degree and reduction molten iron desulfuring spray gun.
Brief description of the drawings
Fig. 1 is after a kind of molten iron desulfuring spray gun prepared by the present invention is toasted with carbon fiber-reinforced castable refractory through 110 DEG C × 24h Stereoscan photograph；
Fig. 2 is the scanning after the carbon fiber-reinforced castable refractory of molten iron desulfuring spray gun shown in Fig. 1 is heat-treated through 1450 DEG C × 3h Electromicroscopic photograph.
Specific embodiment
With reference to specific embodiment, the invention will be further described, not to the limitation of its protection domain：
In order to avoid repeating, first that involved raw material in this specific embodiment and additive Unify legislation is as follows, embodiment In repeat no more：
The main chemical compositions of the natural electrofused mullite are：Al2O3It is 66 ~ 75wt%, SiO2It is 20 ~ 28wt%, TiO2For 2.5~3.0wt%.The grain composition of the natural electrofused mullite is：Particle diameter for 3 ~ 5mm account for natural electrofused mullite 28 ~ 35wt%, particle diameter accounts for natural 28 ~ 35wt% of electrofused mullite more than 5mm and less than or equal to 10mm, particle diameter more than 10mm and less than etc. Natural 30 ~ 40wt% of electrofused mullite is accounted in 20mm.
The main chemical compositions of the andalusite are：Al2O3>=58wt%, SiO2It is 20 ~ 28wt%.The andalusite Grade is matched somebody with somebody：Particle diameter accounts for 60 ~ 70wt% of andalusite for 0.15 ~ 1mm, particle diameter more than 1mm and less than or equal to 3mm account for andalusite 30 ~ 40wt%。
The main chemical compositions of the high-purity fused mullite are：Al2O3It is 72 ~ 79wt%, SiO2It is 19 ~ 27wt%.It is described The particle diameter of high-purity fused mullite particle is 0.15 ~ 1mm, the high-purity fused mullite diameter of particle≤0.044mm.
The Al of the electric smelting dense alumina fine powder2O3Content >=98.6wt%；The particle diameter of electric smelting dense alumina fine powder≤ 0.044mm。
A diameter of 5 ~ 9 μm of the chopped carbon fiber, length is 1 ~ 3mm；Carbon content >=the 95wt% of chopped carbon fiber.
A diameter of 5 ~ 9 μm of the carbon fiber powder, length≤0.282mm；Carbon content >=the 95wt% of carbon fiber powder.
SiC content >=the 97wt% of the carborundum powder；Particle diameter≤the 0.044mm of carborundum powder.
Si contents >=the 98wt% of the silica flour；Particle diameter≤the 0.088mm of silica flour.
The SiO of the silicon powder2Content >=94wt%；Particle diameter≤3 μm of silicon powder.
The length of the polypropylene fibre is 3 ~ 5mm, a diameter of 110 ~ 120 μm；The fusing point of polypropylene fibre is 115 ± 5 ℃。
Embodiment 1
A kind of molten iron desulfuring spray gun carbon fiber-reinforced castable refractory and preparation method thereof.Preparation method described in the present embodiment It is：
The molten iron desulfuring spray gun is with the composition and its mass fraction of carbon fiber-reinforced castable refractory：With 35 ~ 39 parts of quality Natural electrofused mullite, the andalusite of 26 ~ 30 parts of quality, high-purity fused mullite particle, 2 ~ 2.5 parts of matter of 3 ~ 4 parts of quality The high-purity fused mullite powder of amount, the electric smelting dense alumina fine powder of 8 ~ 10 parts of quality, the α-Al of 4 ~ 5 parts of quality2O3Micro mist, 7 ~ 8 ρ-the Al of part quality2O3Micro mist, the silicon powder of 5.5 ~ 7 parts of quality, the carborundum powder of 3 ~ 4 parts of quality, the fine aluminium of 2.5 ~ 3 parts of quality Sour calcium cement is raw material, with 0.4 ~ 0.5 part of carbon fiber of quality, the silica flour of 0.5 ~ 1 part of quality, 0.05 ~ 0.08 part of quality it is poly- Tacryl, 0.04 ~ 0.05 part of carboxymethylcellulose calcium of quality, the defoamer and 0.1 ~ 0.17 part of matter of 0.01 ~ 0.02 part of quality The water reducer of amount is additive.
The molten iron desulfuring spray gun is with the preparation method of carbon fiber-reinforced castable refractory：
The first step, according to the molten iron desulfuring spray gun composition and its mass fraction of carbon fiber-reinforced castable refractory, first will High-purity fused mullite powder, electric smelting dense alumina fine powder, α-Al2O3Micro mist, ρ-Al2O3It is micro mist, silicon powder, carborundum powder, pure Aluminous cement, carbon fiber, silica flour, polypropylene fibre, carboxymethylcellulose calcium, defoamer and water reducer point are spread to Flat bottom container It is interior, intersected with rake vertical and horizontal and take off rake 20 ~ 30 minutes.
Second step, according to the molten iron desulfuring spray gun composition and its mass fraction of carbon fiber-reinforced castable refractory, Natural electrofused mullite, andalusite and high-purity fused mullite particle point are spread in the Flat bottom container, with rake longitudinal direction and Lateral cross takes off rake uniformly, pours into mixer, stirs, and obtains final product the carbon fiber-reinforced refractory casting of molten iron desulfuring spray gun Material.
The carbon fiber is chopped carbon fiber.
The water reducer is the mixture of sodium tripolyphosphate and FS20；Wherein：Sodium tripolyphosphate is 33 ~ 58wt%, and FS20 is 42~67 wt%。
Embodiment 2
A kind of molten iron desulfuring spray gun carbon fiber-reinforced castable refractory and preparation method thereof.Preparation method described in the present embodiment It is：
The molten iron desulfuring spray gun is with the composition and its mass fraction of carbon fiber-reinforced castable refractory：With 39 ~ 44 parts of quality Natural electrofused mullite, the andalusite of 23 ~ 26 parts of quality, high-purity fused mullite particle, 2.5 ~ 3.2 of 4 ~ 4.8 parts of quality The high-purity fused mullite powder of part quality, the electric smelting dense alumina fine powder of 6.5 ~ 8 parts of quality, the α-Al of 3 ~ 4 parts of quality2O3It is micro- ρ-the Al of powder, 6 ~ 7 parts of quality2O3Micro mist, the silicon powder of 4 ~ 5.5 parts of quality, carborundum powder, 2 ~ 2.5 parts of quality of 2 ~ 3 parts of quality Pure calcium aluminate cement be raw material, with 0.5 ~ 0.6 part of carbon fiber of quality, silica flour, 0.08 ~ 0.11 part of matter of 1 ~ 1.5 part of quality The polypropylene fibre of amount, 0.05 ~ 0.06 part of carboxymethylcellulose calcium of quality, the defoamer of 0.02 ~ 0.03 part of quality and 0.17 ~ 0.24 part of water reducer of quality is additive.
The molten iron desulfuring spray gun preparation method of carbon fiber-reinforced castable refractory is with embodiment 1.
The carbon fiber is chopped carbon fiber.
The water reducer is the mixture of sodium tripolyphosphate and FS20；Wherein：Sodium tripolyphosphate is 32 ~ 47wt%, and FS20 is 53~68 wt%。
Embodiment 3
A kind of molten iron desulfuring spray gun carbon fiber-reinforced castable refractory and preparation method thereof.Preparation method described in the present embodiment It is：
The molten iron desulfuring spray gun is with the composition and its mass fraction of carbon fiber-reinforced castable refractory：With 44 ~ 48 parts of quality Natural electrofused mullite, the andalusite of 20 ~ 23 parts of quality, the high-purity fused mullite particle of 4.8 ~ 6 parts of quality, 3.2 ~ 4 parts The high-purity fused mullite powder of quality, the electric smelting dense alumina fine powder of 5 ~ 6.5 parts of quality, the α-Al of 2 ~ 3 parts of quality2O3Micro mist, 5 ~ 6 parts of ρ-Al of quality2O3Micro mist, the silicon powder of 3 ~ 4 parts of quality, the carborundum powder of 1 ~ 2 part of quality, the fine aluminium of 1.5 ~ 2 parts of quality Sour calcium cement is raw material, with 0.6 ~ 0.7 part of carbon fiber of quality, the silica flour of 1.5 ~ 2 parts of quality, 0.11 ~ 0.15 part of quality it is poly- Tacryl, 0.06 ~ 0.07 part of carboxymethylcellulose calcium of quality, the defoamer and 0.24 ~ 0.31 part of matter of 0.03 ~ 0.04 part of quality The water reducer of amount is additive.
The molten iron desulfuring spray gun preparation method of carbon fiber-reinforced castable refractory is with embodiment 1.
The carbon fiber is chopped carbon fiber.
The water reducer is the mixture of sodium tripolyphosphate and FS20；Wherein：Sodium tripolyphosphate is 31 ~ 42wt%, and FS20 is 69~58 wt%。
Embodiment 4
A kind of molten iron desulfuring spray gun carbon fiber-reinforced castable refractory and preparation method thereof.Preparation method described in the present embodiment It is：
The molten iron desulfuring spray gun is with the composition and its mass fraction of carbon fiber-reinforced castable refractory：With 35 ~ 39 parts of quality Natural electrofused mullite, the andalusite of 26 ~ 30 parts of quality, high-purity fused mullite particle, 2 ~ 2.5 parts of matter of 3 ~ 4 parts of quality The high-purity fused mullite powder of amount, the electric smelting dense alumina fine powder of 8 ~ 10 parts of quality, the α-Al of 4 ~ 5 parts of quality2O3Micro mist, 7 ~ 8 ρ-the Al of part quality2O3Micro mist, the silicon powder of 5.5 ~ 7 parts of quality, the carborundum powder of 3 ~ 4 parts of quality, the fine aluminium of 2.5 ~ 3 parts of quality Sour calcium cement is raw material, with 0.8 ~ 1.1 part of carbon fiber of quality, the silica flour of 2 ~ 2.3 parts of quality, 0.05 ~ 0.08 part of quality it is poly- Tacryl, 0.06 ~ 0.07 part of carboxymethylcellulose calcium of quality, the defoamer and 0.21 ~ 0.28 part of matter of 0.04 ~ 0.05 part of quality The water reducer of amount is additive.
The molten iron desulfuring spray gun preparation method of carbon fiber-reinforced castable refractory is with embodiment 1.
The carbon fiber is the mixture of chopped carbon fiber and carbon fiber powder；Wherein：Carbon fiber powder is 44 ~ 60wt%, is chopped Carbon fiber is 40 ~ 56wt%.
The water reducer is the mixture of sodium tripolyphosphate and FS20；Wherein：Sodium tripolyphosphate is 42 ~ 56.5wt%, FS20 It is 43.5 ~ 58 wt%.
Embodiment 5
A kind of molten iron desulfuring spray gun carbon fiber-reinforced castable refractory and preparation method thereof.Preparation method described in the present embodiment It is：
The molten iron desulfuring spray gun is with the composition and its mass fraction of carbon fiber-reinforced castable refractory：With 39 ~ 44 parts of quality Natural electrofused mullite, the andalusite of 23 ~ 26 parts of quality, high-purity fused mullite particle, 2.5 ~ 3.2 of 4 ~ 4.8 parts of quality The high-purity fused mullite powder of part quality, the electric smelting dense alumina fine powder of 6.5 ~ 8 parts of quality, the α-Al of 3 ~ 4 parts of quality2O3It is micro- ρ-the Al of powder, 6 ~ 7 parts of quality2O3Micro mist, the silicon powder of 4 ~ 5.5 parts of quality, carborundum powder, 2 ~ 2.5 parts of quality of 2 ~ 3 parts of quality Pure calcium aluminate cement be raw material, with 1.1 ~ 1.4 parts of carbon fibers of quality, the silica flour of 2.3 ~ 2.6 parts of quality, 0.08 ~ 0.11 part The polypropylene fibre of quality, 0.06 ~ 0.07 part of carboxymethylcellulose calcium of quality, the defoamer of 0.05 ~ 0.06 part of quality and 0.28 ~ 0.35 part of water reducer of quality is additive.
The molten iron desulfuring spray gun preparation method of carbon fiber-reinforced castable refractory is with embodiment 1.
The carbon fiber is the mixture of chopped carbon fiber and carbon fiber powder；Wherein：Carbon fiber powder is 50 ~ 61.5wt%, short Carbon fiber is cut for 38.5 ~ 50wt%.
The water reducer is the mixture of sodium tripolyphosphate and FS20；Wherein：Sodium tripolyphosphate is 39 ~ 50wt%, and FS20 is 50~61wt%。
Embodiment 6
A kind of molten iron desulfuring spray gun carbon fiber-reinforced castable refractory and preparation method thereof.Preparation method described in the present embodiment It is：
The molten iron desulfuring spray gun is with the composition and its mass fraction of carbon fiber-reinforced castable refractory：With 44 ~ 48 parts of quality Natural electrofused mullite, the andalusite of 20 ~ 23 parts of quality, the high-purity fused mullite particle of 4.8 ~ 6 parts of quality, 3.2 ~ 4 parts The high-purity fused mullite powder of quality, the electric smelting dense alumina fine powder of 5 ~ 6.5 parts of quality, the α-Al of 2 ~ 3 parts of quality2O3Micro mist, 5 ~ 6 parts of ρ-Al of quality2O3Micro mist, the silicon powder of 3 ~ 4 parts of quality, the carborundum powder of 1 ~ 2 part of quality, the fine aluminium of 1.5 ~ 2 parts of quality Sour calcium cement is raw material, with 1.4 ~ 1.7 parts of carbon fibers of quality, the silica flour of 2.6 ~ 3 parts of quality, 0.11 ~ 0.15 part of quality it is poly- Tacryl, 0.06 ~ 0.07 part of carboxymethylcellulose calcium of quality, the defoamer and 0.35 ~ 0.45 part of matter of 0.06 ~ 0.08 part of quality The water reducer of amount is additive.
The molten iron desulfuring spray gun preparation method of carbon fiber-reinforced castable refractory is with embodiment 1.
The carbon fiber is the mixture of chopped carbon fiber and carbon fiber powder；Wherein：Carbon fiber powder is 53 ~ 62.5wt%, short Carbon fiber is cut for 37.5 ~ 47wt%.
The water reducer is the mixture of sodium tripolyphosphate and FS20；Wherein：Sodium tripolyphosphate is 37.5 ~ 50wt%, FS20 It is 50 ~ 53.5wt%.
The application method of this specific embodiment is：Prepared molten iron desulfuring spray gun is fallen with carbon fiber-reinforced castable refractory Enter 5 ~ 6 parts of water of quality of addition in mixer, stir 3 ~ 6min, then pour into spray gun fire proofed wood spray gun liner in pouring mould, vibrate Shaping, obtains final product molten iron desulfuring spray gun.
The beneficial effect of this specific embodiment is：
（1）The various raw material that this specific embodiment is used are the conventional raw materials of refractory material, quite varied and valency of originating Lattice are relatively low, therefore low production cost, and the technique that this specific embodiment is sent out involved by preparation method is also relatively simple.
（2）The carbon fiber that this specific embodiment is used is high intensity, high-modulus of a kind of phosphorus content in more than 95wt% New fiber materials, its density ratio aluminium is low, but intensity is higher than steel, and with corrosion-resistant, high-modulus, without creep, non-oxygen Change superhigh temperature resistant and fatigue proof characteristic under environment.By mixing the chopped carbon fiber for adding length for 1 ~ 3mm and≤0.282mm Carbon fiber powder, it is to avoid the winding conglomeration caused because fiber is long in carbon fiber dispersion process, it is ensured that chopped carbon fiber with Carbon fiber powder it is dispersed, realize the composite strengthening toughening effect of different draw ratio carbon fibers.
（3）The Application of composite that this specific embodiment passes through natural electrofused mullite and high-purity fused mullite, using two The low mullite performance difference of thermal coefficient of expansion and complex effect are planted, molten iron desulfuring spray gun is improve and is poured with carbon fiber-reinforced fire resisting Material feeding thermal shock resistance；The excellent high-temperature behavior of high-purity fused mullite extends the carbon fiber-reinforced fire resisting of molten iron desulfuring spray gun The sintering range of castable, to adapt to the spray gun performance requirement of blowing desulfurization under the conditions of high temperature liquid iron.Using gelling ρ-the Al of function admirable2O3Micro mist is main bonding agent and silicon powder, α-Al2O3Micro mist and pure calcium aluminate cement are secondary combined Agent, so as to reduce CaO content in castable, improves the erosion-resisting characteristics of the carbon fiber-reinforced castable refractory of molten iron desulfuring spray gun With elevated temperature strength.Microcrack evolution equation is produced by the high-temperature expansion of andalusite, molten iron desulfuring spray gun carbon is further increased fine The thermal shock resistance of toughness reinforcing castable refractory is tieed up, Linear change rate after high temperature burns is have adjusted.By polypropylene fibre in additive Use, improve the explosion-proof performance and spray gun fire proofed wood of the carbon fiber-reinforced castable refractory baking process of molten iron desulfuring spray gun The globality of spray gun lining.
（4）The addition that this specific embodiment passes through silica flour, prevents the high-temperature oxydation ablation of carbon fiber, in silica flour addition In the range of, be heat-treated under the conditions of air atmosphere and 1450 DEG C × 3h after sample under ESEM it is clearly discernible go out residual Carbon fiber, so as to the long-acting activeness and quietness that ensure that the carbon fiber-reinforced castable refractory of molten iron desulfuring spray gun is acted on.
（5）This specific embodiment reduces amount of water by sodium tripolyphosphate and the compound use of FS20, improves iron The water desulfuring spray gun mobile performance of carbon fiber-reinforced castable refractory, workability and the closely knit performance of cast.By carboxymethyl The selection of cellulose, improves the wellability and dispersiveness of chopped carbon fiber, overcomes the shortcomings of that carbon fiber water infiltration is difficult, strengthens carbon Being tightly combined property and its activeness and quietness effect between fiber and castable matrix.By the selection of defoamer, it is to avoid add water and stir The formation of bubble during mixing, reduces amount of water of the molten iron desulfuring spray gun with carbon fiber-reinforced castable refractory, improves stream Dynamic property, improves packing and mechanical strength.
（6）This specific embodiment is excellent by the reasonable selection and its weight proportion of various raw material and preparation technology's Change, realize being obviously improved for castable thermal shock resistance energy, reach raising molten iron desulfuring spray gun temperature in use and extension is used The purpose in life-span.The uniform mixing of various raw materials and additive is ensure that in preparation process, especially carbon fiber is uniform mixed Close, prevent the group of twining in carbon fiber mixed process from knotting.
（7）This specific embodiment is further prolonged on the basis of thermal shock resistance, corrosion resistance and mechanical strength is improved The service life of molten iron desulfuring spray gun is grown；Steel fibre is replaced by carbon fiber, molten iron desulfuring spray gun is further increased and is used Temperature, the frequency repaired with workman is changed so as to reduce molten iron desulfuring spray gun, reduces the use cost of molten iron desulfuring spray gun.
Molten iron desulfuring spray gun prepared by this specific embodiment is poured with carbon fiber-reinforced castable refractory and conventional steel fiber Material feeding is compared, and the rupture strength of the product of preparation after 110 DEG C × 24h and 1450 DEG C × 3h heat treatments improves 10 ~ 15%, thermal shock Water-cooled number of times improves 50%, and maximum operation (service) temperature improves 100 DEG C.
Fig. 1 be embodiment 1 prepare a kind of molten iron desulfuring spray gun with carbon fiber-reinforced castable refractory through 110 DEG C × 24h Stereoscan photograph after baking, Fig. 2 is the carbon fiber-reinforced castable refractory sample of molten iron desulfuring spray gun shown in Fig. 1 through 1450 DEG C × 3h heat treatment after stereoscan photograph, in Fig. 1 and Fig. 2：1 represents carbon fiber；2 represent that carbon fiber oxidized residual is elongated micro- Hole.Chopped carbon fiber is can be seen that by Fig. 1 and Fig. 2 to be uniformly distributed in castable, and combined closely with castable matrix, it is high The part elongated micropore of chopped carbon fiber oxidized residual after warm treatment, and be uniformly distributed in castable matrix.By various originals The reasonable selection and its weight proportion of material and the optimization of preparation technology, realize being obviously improved for castable thermal shock resistance energy Reach the purpose for improving molten iron desulfuring spray gun temperature in use and increasing the service life.
Therefore, the molten iron desulfuring spray gun carbon that this specific embodiment is with low cost and raw material sources are extensive, prepared Fiber reinforced castable refractory good thermal shock stability, can extend the service life of molten iron desulfuring spray gun, improve molten iron desulfuring spray gun Temperature in use and reduce molten iron desulfuring spray gun use cost.

Claims (13)

1. a kind of molten iron desulfuring spray gun preparation method of carbon fiber-reinforced castable refractory, it is characterised in that the desulfurizing iron Spray gun is with the composition and its mass fraction of carbon fiber-reinforced castable refractory：With 35 ~ 48 parts of natural electrofused mullites of quality, 20 ~ 30 parts of andalusites of quality, the high-purity fused mullite particle of 3 ~ 6 parts of quality, the high-purity fused mullite powder of 2 ~ 4 parts of quality Body, the electric smelting dense alumina fine powder of 5 ~ 10 parts of quality, the α-Al of 2 ~ 5 parts of quality2O3ρ-the Al of micro mist, 5 ~ 8 parts of quality2O3Micro mist, 3 ~ 7 parts of silicon powders of quality, the carborundum powder of 1 ~ 4 part of quality, the pure calcium aluminate cement of 1.5 ~ 3 parts of quality are raw material, with 0.4 ~ 1.7 parts of carbon fibers of quality, the silica flour of 0.5 ~ 3 part of quality, the polypropylene fibre of 0.05 ~ 0.15 part of quality, 0.04 ~ 0.07 part of matter The carboxymethylcellulose calcium of amount, the defoamer and 0.1 ~ 0.45 part of water reducer of quality of 0.01 ~ 0.08 part of quality are additive；
The carbon fiber is chopped carbon fiber or is chopped carbon fiber and the mixture of carbon fiber powder；
The molten iron desulfuring spray gun is with the preparation method of carbon fiber-reinforced castable refractory：
The first step, according to the molten iron desulfuring spray gun composition and its mass fraction of carbon fiber-reinforced castable refractory, first will High-purity fused mullite powder, electric smelting dense alumina fine powder, α-Al2O3Micro mist, ρ-Al2O3It is micro mist, silicon powder, carborundum powder, pure Aluminous cement, carbon fiber, silica flour, polypropylene fibre, carboxymethylcellulose calcium, defoamer and water reducer point are spread to Flat bottom container It is interior, intersected with rake vertical and horizontal and take off rake 20 ~ 30 minutes；
Second step, according to the molten iron desulfuring spray gun composition and its mass fraction of carbon fiber-reinforced castable refractory, Natural electrofused mullite, andalusite and high-purity fused mullite particle point are spread in the Flat bottom container, with rake longitudinal direction and Lateral cross takes off rake uniformly, pours into mixer, stirs, and obtains final product the carbon fiber-reinforced refractory casting of molten iron desulfuring spray gun Material.
2. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature The main chemical compositions for being the natural electrofused mullite are：Al2O3It is 66 ~ 75wt%, SiO2It is 20 ~ 28wt%, TiO2For 2.5~3.0wt%；
The grain composition of the natural electrofused mullite is：Particle diameter natural 28 ~ 35wt% of electrofused mullite for 3 ~ 5mm is accounted for, particle diameter is big Natural 28 ~ 35wt% of electrofused mullite is accounted in 5mm and less than or equal to 10mm, particle diameter is accounted for naturally more than 10mm and less than or equal to 20mm 30 ~ 40wt% of electrofused mullite.
3. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature The main chemical compositions for being the andalusite are：Al2O3>=58wt%, SiO2It is 20 ~ 28wt%；
The grain composition of the andalusite is：Particle diameter accounts for 60 ~ 70wt% of andalusite for 0.15 ~ 1mm, particle diameter more than 1mm and less than etc. 30 ~ 40wt% of andalusite is accounted in 3mm.
4. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature The main chemical compositions for being the high-purity fused mullite are：Al2O3It is 72 ~ 79wt%, SiO2It is 19 ~ 27wt%；
The particle diameter of the high-purity fused mullite particle be 0.15 ~ 1mm, the high-purity fused mullite diameter of particle≤ 0.044mm。
5. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature It is the Al of the electric smelting dense alumina fine powder2O3Content >=98.6wt%；Particle diameter≤the 0.044mm of electric smelting dense alumina fine powder.
6. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature It is a diameter of 5 ~ 9 μm of the chopped carbon fiber, length is 1 ~ 3mm；Carbon content >=the 95wt% of chopped carbon fiber.
7. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature It is a diameter of 5 ~ 9 μm of the carbon fiber powder, length≤0.282mm；Carbon content >=the 95wt% of carbon fiber powder.
8. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature It is the SiC content >=97wt% of the carborundum powder；Particle diameter≤the 0.044mm of carborundum powder.
9. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature It is the Si contents >=98wt% of the silica flour；Particle diameter≤the 0.088mm of silica flour.
10. the molten iron desulfuring spray gun according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature It is the SiO of the silicon powder2Content >=94wt%；Particle diameter≤3 μm of silicon powder.
The 11. molten iron desulfuring spray guns according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature It is that the length of the polypropylene fibre is 3 ~ 5mm, a diameter of 110 ~ 120 μm；The fusing point of polypropylene fibre is 115 ± 5 DEG C.
The 12. molten iron desulfuring spray guns according to claim 1 preparation method of carbon fiber-reinforced castable refractory, its feature It is that the water reducer is sodium tripolyphosphate and the mixture of FS20.
A kind of 13. carbon fiber-reinforced castable refractories of molten iron desulfuring spray gun, it is characterised in that the molten iron desulfuring spray gun carbon Fiber reinforced castable refractory is molten iron desulfuring spray gun according to any one of claim 1 ~ 12 with carbon fiber-reinforced The carbon fiber-reinforced castable refractory of molten iron desulfuring spray gun prepared by the preparation method of castable refractory.
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CN116217251A (en) * 2023-02-28 2023-06-06 中铸新材工业（江苏）有限公司 Low-density low-heat-storage ceramic fiber castable for aluminum industry and preparation method thereof
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