CN106145971B - A kind of cracking resistance magnesia carbon brick and preparation method thereof - Google Patents

A kind of cracking resistance magnesia carbon brick and preparation method thereof Download PDF

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CN106145971B
CN106145971B CN201610530487.3A CN201610530487A CN106145971B CN 106145971 B CN106145971 B CN 106145971B CN 201610530487 A CN201610530487 A CN 201610530487A CN 106145971 B CN106145971 B CN 106145971B
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magnesia
carbon brick
cracking resistance
magnesia carbon
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张刚
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Changzhou Suzhou Refractory and Metallurgical Refractories Co., Ltd.
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Changzhou Suzhou Refractory And Metallurgical Refractories Co Ltd
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    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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Abstract

The invention discloses a kind of cracking resistance magnesia carbon bricks, are made of the component of following parts by weight: 75~80 parts of magnesia, 7~10 parts of basalt particles, 5~10 parts of cupric sulfate pentahydrates, 0.3~0.5 part of hexa, 15~18 parts of graphite, 3~5 parts of ceramic particle Al4SiC4, 3~5 parts of bonding agents.Cracking resistance magnesia carbon brick of the invention can effectively avoid brick body layer from splitting, and substantially reduce carbon loss vector, improve the resistance to slag and antioxygenic property of magnesia carbon brick, improve service life, brick body quality and excellent performance.The present invention also provides a kind of cracking resistance magnesia carbon brick preparation methods, and processing step is simple, strong operability, and to equipment without particular/special requirement, preparation cost is low, are suitble to industrialized production.

Description

A kind of cracking resistance magnesia carbon brick and preparation method thereof
Technical field
The present invention relates to technical field of refractory materials, more particularly, to a kind of cracking resistance magnesia carbon brick and preparation method thereof.
Background technique
Magnesia carbon brick is because having good thermal shock resistance and resistance to slag corrosion, so being widely used in ferrous metallurgical industry. Product strength is caused to reduce since carbon is oxidizable, corrosion resistance decline makes magnesia carbon brick lose the upper hand.To improve magnesia carbon brick in height Oxidation resistance under the conditions of temperature, key are to control the decarbonization rate of material.A kind of currently used method is in magnesia carbon brick Middle addition prevents the additive of oxidation, and there are two main classes for common additive, (1) metal or alloy fine powder；(2) nonmetallic thin Powder.
For example, application publication number CN101747065A, the Chinese patent of data of publication of application 2010.06.23 discloses one kind Magnesia carbon brick, the raw material of the magnesia carbon brick is by 30-80 parts by weight waste magnesia carbon bricks particle, 3-40 parts by weight magnesia particle, 6-12 weight Part graphite, 5-15 parts by weight magnesia powder, 3-15 parts by weight micro-powder as additive, 2.2-3.5 parts by weight organic bond composition.The magnesium Micro-powder as additive (hard pitch powder, alumina powder, metallic aluminium powder, metallic silicon power, metal magnesium powder, boron nitride are added in carbon brick It is any one or more than one in powder, carborundum powder) to improve the oxidation resistance of magnesia carbon brick at high temperature, there are following Insufficient: (1) metal fine powder (such as metallic aluminium powder, metallic silicon power) easily aoxidizes, in already oxidised metal and magnesia and graphite Impurity easily occur unfavorable reaction, aoxidize the effect of Shi Huiqi flux, it is well known that in burned-magnesia brick, aluminium oxide and high The silicate mineral of calcium silicon ratio can react to form liquid phase, and apparent influence can be generated on refractoriness, gentle in molten steel, slag Under the corrosion function of body, it is easy to lead to the reduction of product service life；In addition the magnesia carbon brick in process of production, the metal of addition Micro mist will cause magnesia carbon brick thermal expansion it is excessively high, to generate very high stress, magnesia carbon brick is caused easily to crack；Rather than metal fine powder The addition of (such as boron nitride powder, carborundum powder) will affect the resistance to slag of magnesia carbon brick again；(2) in the preparation process of magnesia carbon brick, Be also easy to produce layer split, poor toughness.
Summary of the invention
The present invention is to provide a kind of formula conjunction to solve above-mentioned technical problem present in the magnesia carbon brick of the prior art Natural sciences can effectively avoid brick body layer from splitting, improve service life, the cracking resistance magnesia carbon brick of brick body quality and excellent performance.
The present invention also provides a kind of cracking resistance magnesia carbon brick preparation methods, and processing step is simple, strong operability, at low cost, It is suitble to industrialized production.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of cracking resistance magnesia carbon brick of the invention, the cracking resistance magnesia carbon brick are made of the component of following parts by weight: 75~80 parts Magnesia, 7~10 parts of basalt particles, 5~10 parts of cupric sulfate pentahydrates, 0.3~0.5 part of hexa, 15~18 parts of graphite, 3~5 parts of ceramic particle Al4SiC4, 3~5 parts of bonding agents.The present invention defect existing for existing magnesia carbon brick formula, to its into It has gone re-optimization improvement, has especially been added to basalt particle, cupric sulfate pentahydrate and ceramic particle Al4SiC4, wherein basalt Particle can make the crackle formed in brick body shift and diverge, and inhibit long crack to generate and change direction, while preventing brick body The diffusion of internal fissure, from the thermal shock resistance that can effectively improve magnesia carbon brick, the combination water in cupric sulfate pentahydrate loses under the high temperature conditions After going, volume reduces, so that generating short space around copper sulphate, which can effectively offset the thermal expansion of magnesia carbon brick, reduces Internal stress, thus effectively magnesia carbon brick is avoided to crack, ceramic particle Al4SiC4Relative to conventional additives (such as metallic aluminium powder, metal Silicon powder etc.), the carbon being oxidized can be restored, while being added to supplementary carbon source in magnesia carbon brick for the carbon of itself as free carbon, separately Outer Al4SiC4Decompose the Al generated2O3, SiC reacts with MgO and ultimately generates magnesium aluminate spinel and forsterite in brick body surface shape At protective layer to prevent from further aoxidizing, carbon loss vector can be substantially reduced, the resistance to slag of magnesia carbon brick is improved, it can be improved and use the longevity Life.
Preferably, the magnesia is mixed by the different-grain diameter magnesia of following parts by weight: 20~25 parts of 3~5mm's Magnesia, the magnesia of 25~30 parts of 1~2mm, the magnesia of 10~15 parts of 0.3~0.5mm, the magnesia of 5~8 parts of 0.05~0.08mm. The size distribution of magnesia is very crucial, and the specific surface area of the particle of small particle is larger, can make with the more air of people when being added The generation probability that layer is split increases；And the less layer that equally will also result in of large-size particles as framework material is split, therefore the present invention By the particle size range and additional amount of strict control magnesia particle, to guarantee to suppress closely knit product, layer is effectively prevent to split Generation.
Preferably, the partial size of the basalt particle is 20~25mm.The partial size of basalt particle is excessive, can increase instead Add the crackle of brick body, partial size is too small, then effect is not significant, therefore limited in the present invention partial size of basalt particle as 20~ 25mm。
Preferably, the ceramic particle Al4SiC4It is made by the following method: in molar ratio by aluminium powder, silicon powder, carbon dust 4:1:4 mixing after, under nitrogen protection plus alcohol in ball mill ball milling at least for 24 hours, in 1600 in vacuum sintering funace It is sintered 2~3h at~1800 DEG C, grinds after cooling to get ceramic particle Al4SiC4。
Preferably, the ceramic particle Al4SiC4Partial size be 5~10 μm.
Preferably, the bonding agent is phenol-formaldehyde resin modified, the phenol-formaldehyde resin modified is made by the following method:
(a) by naphthalene sulphonate formaldehyde condensation polymer be dissolved in ethyl alcohol formed mass percent concentration be 0.5~1% mixing it is molten Liquid.
(b) nano silica of mixed solution quality 1~1.5%, ultrasonic disperse, score are incorporated as in mixed solution Dispersion liquid, for use.Easily reunite after silica dispersion, dispersibility is always the technological difficulties of this field, the naphthalene in the present invention Sodium sulfonate formaldehyde condensation products can be adsorbed on nanometer titanium dioxide silicon interface, charge nano silica interface, and generate ζ electricity Position, when the nano silica of dispersion is close to each other, due to electric double layer electrostatic repulsion and separate, to maintain its stably dispersing Property, keep it not easy to reunite, the present invention efficiently solves nano silica by ultrasound and naphthalenesulfonic acid-formaldehyde condensate and is not easy The problem of dispersion.
(c) press n (phenol): phenol is dissolved in formalin, obtains premixed liquid by n (formaldehyde)=1:1.25~1.32.
(d) press v (dispersion liquid): v (premixed liquid)=1:5~6 is added dispersion liquid in premixed liquid while stirring, then presses n (phenol): n (sodium hydroxide)=1:1.25~1.32 is added dropwise to sodium hydroxide solution while stirring, obtains reaction solution.
(d) reaction solution is heated with oil bath, heating stirring to after 50 DEG C, control heating rate is 0.5~0.6 DEG C/ Min is added after vacuum dehydration and produces until 2~3h of isothermal reaction, it is 6.5~7.0 that acid adding, which is neutralized to pH, after temperature is 90~95 DEG C The ethylene glycol of 0.5~1 times of volume of object, obtains phenol-formaldehyde resin modified.Phenolic resin is still widely used in magnesia carbon brick at present as viscous Mixture, but its thermal decomposition temperature and oxidation resistance are poor, therefore are no longer satisfied the use of novel refractory, the present invention In phenolic resin is modified with silica, make surface property phase of the inorganic nano silica with phenolic resin Match, compatibility, wettability and the caking property both improved, and effectively improve phenolic resin thermal decomposition temperature and anti-oxidant energy Power (thermal decomposition temperature can be improved about 190 DEG C, and oxidation of coal temperature can be improved about 1200 DEG C), moreover it is possible to improve the strong of magnesia carbon brick Degree, has widened its application field.
A kind of cracking resistance magnesia carbon brick preparation method, specific steps are as follows: according to the ratio will each raw material mix after be added sand mixer in into Row is kneaded, and compression moulding in punching block is added after mixing and obtains adobe, finally to after brick bat drying up to cracking resistance magnesia carbon brick.
Preferably, mixing time is 40~50min, briquetting pressure is 100~120Mpa, and drying temperature is 200~250 DEG C, drying time be 22~for 24 hours.
Therefore, the invention has the following beneficial effects:
(1) present invention defect existing for existing magnesia carbon brick formula, has carried out re-optimization improvement to it, especially It is added to basalt particle, cupric sulfate pentahydrate and ceramic particle Al4SiC4, and the size distribution of magnesia is adjusted, can have Effect avoids brick body layer from splitting, and substantially reduces carbon loss vector, improves the resistance to slag and antioxygenic property of magnesia carbon brick, improve using the longevity Life, brick body quality and excellent performance；
(2) a kind of cracking resistance magnesia carbon brick preparation method is provided, processing step is simple, strong operability, to equipment without special It is required that preparation cost is low, it is suitble to industrialized production.
Specific embodiment
Below by specific embodiment, the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material is commercially available or the industry is common are following Method in embodiment is unless otherwise instructed conventional method in that art.
Embodiment 1
(1) ceramic particle Al is prepared4SiC4
By aluminium powder, silicon powder, carbon dust after 4:1:4 is mixed in molar ratio, under nitrogen protection plus alcohol ball milling in ball mill At least for 24 hours, 3h is sintered at 1600 DEG C in vacuum sintering funace, is ground after cooling, the ceramic particle that partial size is 5 μm is obtained Al4SiC4, for use；
(2) phenol-formaldehyde resin modified is prepared
(a) naphthalene sulphonate formaldehyde condensation polymer is dissolved in and forms the mixed solution that mass percent concentration is 0.5% in ethyl alcohol；
(b) nano silica of mixed solution quality 1% is incorporated as in mixed solution, ultrasonic disperse obtains dispersion liquid, For use；
(c) press n (phenol): phenol is dissolved in formalin, obtains premixed liquid by n (formaldehyde)=1:1.25；
(d) press v (dispersion liquid): v (premixed liquid)=1:5 is added dispersion liquid in premixed liquid while stirring, then presses n (benzene Phenol): n (sodium hydroxide)=1:1.25 is added dropwise to sodium hydroxide solution while stirring, obtains reaction solution；
(e) reaction solution being heated with oil bath, for heating stirring to after 50 DEG C, control heating rate is 0.5 DEG C/min, until After temperature is 90 DEG C, isothermal reaction 3h, it is 6.5 that acid adding, which is neutralized to pH, and the second two of 0.5 times of volume of product is added after vacuum dehydration Alcohol obtains phenol-formaldehyde resin modified, for use；
(3) cracking resistance magnesia carbon brick is prepared
By 75kg magnesia, 7kg partial size is the basalt particle of 20mm, 5kg cupric sulfate pentahydrate, 0.3kg hexa, 15kg graphite, 3kg ceramic particle Al4SiC4, the weight proportion of 3kg bonding agent (phenol-formaldehyde resin modified) will each raw material mix after plus Enter in sand mixer and be kneaded, compression moulding in punching block is added after mixing and obtains adobe, finally to after brick bat drying up to cracking resistance magnesium Carbon brick, wherein magnesia is mixed by the different-grain diameter magnesia of following weight proportion: the magnesia of 20kg3mm, the magnesium of 25kg1mm Sand, the magnesia of 10kg0.3mm, the magnesia of 5kg0.05mm, mixing time 40min, briquetting pressure 100Mpa, drying temperature It is 200 DEG C, drying time is for 24 hours.
Embodiment 2
(1) ceramic particle Al is prepared4SiC4
By aluminium powder, silicon powder, carbon dust after 4:1:4 is mixed in molar ratio, under nitrogen protection plus alcohol ball milling in ball mill At least for 24 hours, 2h is sintered at 1800 DEG C in vacuum sintering funace, is ground after cooling, the ceramic particle that partial size is 10 μm is obtained Al4SiC4, for use；
(2) phenol-formaldehyde resin modified is prepared
(a) naphthalene sulphonate formaldehyde condensation polymer is dissolved in and forms the mixed solution that mass percent concentration is 1% in ethyl alcohol；
(b) nano silica of mixed solution quality 1.5% is incorporated as in mixed solution, ultrasonic disperse must disperse Liquid, for use；
(c) press n (phenol): phenol is dissolved in formalin, obtains premixed liquid by n (formaldehyde)=1:1.32；
(d) press v (dispersion liquid): v (premixed liquid)=1:6 is added dispersion liquid in premixed liquid while stirring, then presses n (benzene Phenol): n (sodium hydroxide)=1:1.32 is added dropwise to sodium hydroxide solution while stirring, obtains reaction solution；
(e) reaction solution being heated with oil bath, for heating stirring to after 50 DEG C, control heating rate is 0.6 DEG C/min, until After temperature is 95 DEG C, isothermal reaction 2h, it is 7.0 that acid adding, which is neutralized to pH, and the ethylene glycol of 1 times of volume of product is added after vacuum dehydration, Phenol-formaldehyde resin modified is obtained, for use；
(3) cracking resistance magnesia carbon brick is prepared
By 80kg magnesia, 7kg partial size is the basalt particle of 25mm, 5kg cupric sulfate pentahydrate, 0.5kg hexa, 18kg graphite, 5kg ceramic particle Al4SiC4, the weight proportion of 5kg bonding agent (phenol-formaldehyde resin modified) will each raw material mix after plus Enter in sand mixer and be kneaded, compression moulding in punching block is added after mixing and obtains adobe, finally to after brick bat drying up to cracking resistance magnesium Carbon brick, wherein magnesia is mixed by the different-grain diameter magnesia of following weight proportion: the magnesia of 25kg5mm, the magnesium of 30kg2mm Sand, the magnesia of 15kg0.5mm, the magnesia of 8kg0.08mm, mixing time 50min, briquetting pressure 120Mpa, drying temperature It is 250 DEG C, drying time 22h.
Embodiment 3
(1) ceramic particle Al is prepared4SiC4
By aluminium powder, silicon powder, carbon dust after 4:1:4 is mixed in molar ratio, under nitrogen protection plus alcohol ball milling in ball mill At least for 24 hours, 2.5h is sintered at 1700 DEG C in vacuum sintering funace, is ground after cooling, the ceramic particle that partial size is 8 μm is obtained Al4SiC4, for use；
(2) phenol-formaldehyde resin modified is prepared
(a) naphthalene sulphonate formaldehyde condensation polymer is dissolved in and forms the mixed solution that mass percent concentration is 0.7% in ethyl alcohol；
(b) nano silica of mixed solution quality 1.2% is incorporated as in mixed solution, ultrasonic disperse must disperse Liquid, for use；
(c) press n (phenol): phenol is dissolved in formalin, obtains premixed liquid by n (formaldehyde)=1:1.28；
(d) press v (dispersion liquid): v (premixed liquid)=1:5.5 is added dispersion liquid in premixed liquid while stirring, then presses n (benzene Phenol): n (sodium hydroxide)=1:1.26 is added dropwise to sodium hydroxide solution while stirring, obtains reaction solution；
(e) reaction solution being heated with oil bath, for heating stirring to after 50 DEG C, control heating rate is 0.55 DEG C/min, After being 92 DEG C to temperature, isothermal reaction 2.5h, it is 6.8 that acid adding, which is neutralized to pH, and the second of 0.7 times of volume of product is added after vacuum dehydration Glycol obtains phenol-formaldehyde resin modified, for use；
(3) cracking resistance magnesia carbon brick is prepared
By 78kg magnesia, 8kg partial size is the basalt particle of 22mm, 7kg cupric sulfate pentahydrate, 0.4kg hexa, 17kg graphite, 4kg ceramic particle Al4SiC4, after the weight of 4kg bonding agent (phenol-formaldehyde resin modified) mixes each raw material Be added in sand mixer and be kneaded, compression moulding in punching block is added after mixing and obtains adobe, finally to after brick bat drying up to cracking resistance Magnesia carbon brick, wherein magnesia is mixed by the different-grain diameter magnesia of following different weight part: the magnesia of 22kg4mm, 28kg1.5mm Magnesia, the magnesia of 12kg0.4mm, the magnesia of 6kg0.07mm, mixing time 45min, briquetting pressure 110Mpa are dry Temperature is 230 DEG C, drying time 22.5h.
Cracking resistance magnesia carbon brick performance indicator of the invention is as follows:
The porosity (%): 2.1；
Bulk density (g/cm3): 3.02；
Decarburized layer (mm): 1.32；
Compressive resistance (Mpa): 46；
High temperature break resistant intensity (Mpa, 1400 DEG C × 1h bury carbon): 20.2.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.

Claims (3)

1. a kind of cracking resistance magnesia carbon brick, which is characterized in that the cracking resistance magnesia carbon brick is made of the component of following parts by weight: 75~80 parts Magnesia, 7~10 parts of basalt particles, 5~10 parts of cupric sulfate pentahydrates, 0.3~0.5 part of hexa, 15~18 parts of graphite, 3~5 parts of ceramic particle Al4SiC4, 3~5 parts of bonding agents；The magnesia is mixed by the different-grain diameter magnesia of following parts by weight: The magnesia of 20~25 parts of 3~5mm, the magnesia of 25~30 parts of 1~2mm, the magnesia of 10~15 parts of 0.3~0.5mm, 5~8 part 0.05 The magnesia of~0.08mm；The partial size of the basalt particle is 20~25mm；The ceramic particle Al4SiC4By the following method Be made: by aluminium powder, silicon powder, carbon dust after 4:1:4 is mixed in molar ratio, under nitrogen protection plus alcohol ball milling is at least in ball mill For 24 hours, 2~3h is sintered at 1600~1800 DEG C in vacuum sintering funace, is ground after cooling to get ceramic particle Al4SiC4；The ceramic particle Al4SiC4Partial size be 5~10 μm；The bonding agent is phenol-formaldehyde resin modified, the modified phenol Urea formaldehyde is made by the following method:
(a) naphthalene sulphonate formaldehyde condensation polymer is dissolved in and forms the mixed solution that mass percent concentration is 0.5~1% in ethyl alcohol；
(b) nano silica of mixed solution quality 1~1.5% is incorporated as in mixed solution, ultrasonic disperse must disperse Liquid, for use；
(c) press n (phenol): phenol is dissolved in formalin, obtains premixed liquid by n (formaldehyde)=1:1.25~1.32；
(d) press v (dispersion liquid): v (premixed liquid)=1:5~6 is added dispersion liquid in premixed liquid while stirring, then presses n (benzene Phenol): n (sodium hydroxide)=1:1.25~1.32 is added dropwise to sodium hydroxide solution while stirring, obtains reaction solution；
(e) reaction solution being heated with oil bath, for heating stirring to after 50 DEG C, control heating rate is 0.5~0.6 DEG C/min, After being 90~95 DEG C to temperature, 2~3h of isothermal reaction, it is 6.5~7.0 that acid adding, which is neutralized to pH, and product 0.5 is added after vacuum dehydration The ethylene glycol of~1 times of volume, obtains phenol-formaldehyde resin modified.
2. a kind of cracking resistance magnesia carbon brick preparation method as described in claim 1, which is characterized in that specific steps are as follows: according to the ratio will It is added in sand mixer and is kneaded after each raw material mixing, compression moulding in punching block is added after mixing and obtains adobe, it is finally dry to adobe Up to cracking resistance magnesia carbon brick after dry.
3. cracking resistance magnesia carbon brick preparation method according to claim 2, which is characterized in that mixing time is 40~50min, at Type pressure be 100~120Mpa, drying temperature be 200~250 DEG C, drying time be 22~for 24 hours.
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CN109942198A (en) * 2019-05-05 2019-06-28 商洛学院 The method for using hot pressing sintering method to prepare glass water-permeable brick as raw material using Pb-Zn tailings
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CN102329136A (en) * 2011-06-29 2012-01-25 江苏苏嘉集团新材料有限公司 Method for preparing magnesia carbon brick
CN105503212A (en) * 2015-12-21 2016-04-20 江苏苏嘉集团新材料有限公司 Magnesia carbon brick and preparation method thereof

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CN102276271A (en) * 2011-06-29 2011-12-14 江苏苏嘉集团新材料有限公司 Preparation method of normal temperature solidified magnesium carbon brick
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CN105503212A (en) * 2015-12-21 2016-04-20 江苏苏嘉集团新材料有限公司 Magnesia carbon brick and preparation method thereof

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