CN105130457A - Magnesium-calcium-carbon refractory material and preparation method thereof - Google Patents
Magnesium-calcium-carbon refractory material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a magnesium-calcium-carbon refractory material and a preparation method thereof. The refractory material comprises 100-120 parts of magnesia-calcia clinker particles, 40-50 parts of magnesia-calcia clinker fine powder, 15-35 parts of nano-magnesia, 20-30 parts of nano-calcia, 20-35 parts of zirconia, 10-20 parts of graphene, 5-10 parts of an additive, 7-12 parts of a binder and 5-12 parts of nano-carbon fibers. The inside of the refractory material prepared in the invention is compact, so the bulk density is improved, and the apparent porosity of the refractory material is reduced to prevent expansion, thereby all physical performances, such as the strength, the thermal shock resistance and the thermal impact resistance of the refractory material are further improved; and the preparation method has the advantages of simplicity, abundant raw materials, and suitableness for factory production.
Description
Technical field
The present invention relates to fire resisting material field, particularly relate to that a kind of refractoriness is high, erosion-resisting characteristics is excellent, thermal shock resistance is good, mg-ca-carbon refractory that sintering range is wide and preparation method thereof.
Background technology
Along with the growing tension of the energy, various countries are to the development of hot industry energy-saving material, production and use pay attention to day by day, and high temperature kiln needs to use the refractory materials with excellent properties or specialized character in a large number.Magnesite-dolomite refractories is a kind of basic refractory, is just used as the furnace lining material of steel-making converter from the sixties in last century, for China's converter steelmaking industrial expansion has made contribution.
Magnesia-calcium-carbon brick is the refractory product made for main raw material with dolomite sand, calcium magnesia sand, magnesia and carbon element, and its main advantage is the resistance to fouling under low alkalinity, suboxide iron iron blast furnace slag and vacuum condition.Heat-shock resistance is better than magnesia carbon brick, also helps the oxygen level of minimizing molten steel and is mingled with.But the hydration resistance of magnesia-calcium-carbon brick, not enough, heat-shock resistance also needs to improve oxidation-resistance simultaneously.
A kind of unfired magnesia-calcium carbon brick and preparation method (CN102351548A), its raw material is the calcium magnesia sand electrosmelted magnesite clinker of different-grain diameter, modifying asphalt bonding agent, crystalline flake graphite, metal magnesium powder additive.Its weak point is, the hydration resistance of magnesia-calcium-carbon brick, and not enough, heat-shock resistance also needs to improve oxidation-resistance simultaneously.
Summary of the invention
The object of the invention is to solve the existing hydration resistance preparing magnesia-calcium-carbon brick in the technique of mg-ca-carbon refractory, oxidation-resistance not enough, simultaneously heat-shock resistance also needs the defect that improves and provides that a kind of refractoriness is high, erosion-resisting characteristics is excellent, thermal shock resistance is good, antioxidant property is good, the mg-ca-carbon refractory that sintering range is wide.
Another object of the present invention is the preparation method in order to provide this refractory materials.
To achieve these goals, the present invention is by the following technical solutions:
A kind of mg-ca-carbon refractory, calcium magnesia sand particle 100-120 part, calcium magnesia sand fine powder 40-50 part, nano magnesia 15-35 part, nano calcium oxide 20-30 part, zirconium white 20-35 part, Graphene 10-20 part, additive 5-10 part, bonding agent 7-12 part and carbon nano fiber 5-12 part.In the technical program, Graphene is a kind of novel material of the individual layer sheet structure be made up of carbon atom, has the feature of the high ﹑ specific surface area of strong degree large ﹑ height chemical reaction property ﹑ alive high fillibility; In goods, add Graphene makes goods interior contact more tight, thus because of the stress produced that expands when reducing to burn till, prevents goods from loosening or cracking; The high strength of Graphene ensure that the excellent mechanical property of goods, can promote antiacid caustic corrosion performance and the oxidation-resistance of goods simultaneously.
As preferably, described additive is the mixture of diatom ooze, boron nitride, glass microballon and nano zine oxide, and the mass ratio of diatom ooze, boron nitride, glass microballon and nano zine oxide is 5:3:4:7.In the technical program, glass microballon granularity is suitable, good fluidity, dispersity is high, add glass microballon, can be dispersed in internal height, acceleration of sintering, and have evenly weave construction, improve intensity and the thermal shock resistance of goods, the granularity of nano zine oxide is tiny, can fill fine pores, reduce the void content of goods, improve volume density.
As preferably, described bonding agent is the mixture of Seaweed Extract and beeswax, and mass ratio is 2:1, and the preparation method of this bonding agent is as follows: 1) clean: the tap water that marine alga raw material is 45-50 DEG C soaks 2-3 hour, then cleans up;
2) pulverize, centrifugal: the marine alga cleaned up, vacuum breaking, add the ethanol of marine alga volume 30 times and fourth diester solution soaking and boil, the volume ratio of ethanol and fourth diester is 1:1, then centrifugation is removed slag to obtain marine alga clear liquid, the rotating speed of whizzer is 4000 ~ 6000rpm, and centrifugation time is 15-20min;
3) nanofiltration: diluted by the pure water of marine alga clear liquid with 5-10 times of volume, then carries out dialysis by nanofiltration membrane and concentrates, and the 0.1-0.2 that the dialysis of marine alga clear liquid is concentrated into dilution front volume doubly obtains nanofiltration concentrated solution, and the molecular weight cut-off of described nanofiltration membrane is 600-700Da;
4) concentrate drying: after nanofiltration concentrated solution adds beeswax, further vacuum concentration to solid content is 40-60%, and then spraying dry obtains the Powdered bonding agent of water content 2-3% in spray-dryer.In the technical program, Seaweed Extract, as bonding agent, can make goods inside combine closely, and Seaweed Extract then extracts obtained from naturally occurring marine alga, environmental protection.
As preferably, add glass microballon and nano zine oxide after diatom ooze mixes in ethanol with boron nitride, in a water bath after ultrasonic vibration 2h, drying obtains supplementary additive.
As preferably, the particle diameter of calcium magnesia sand particle is 0.2-2mm, and the particle diameter of calcium magnesia sand fine powder is 100-120 μm.
A kind of preparation method of mg-ca-carbon refractory, each raw material weighs by above proportioning, mixture after mixing take raw spirit as medium milling 10-12 hour, then powder is obtained at vacuum drying, reaction powder is applied to the plasma arc of 5000-7000 volt, make powder melting, by rare gas element the powder after melting blown to machine be installed with standby in be prepared into the molded article of various desired size, after dry at 120-150 DEG C 10-12 hour, at 450-480 DEG C, be incubated 30-50min obtain mg-ca-carbon refractory.In the technical program, plasma high-temperature fusion technology, add voltage between the two poles of the earth, plasma body is heated up instantaneously, the powder added in feed appliance is reached molten state rapidly, plasma body high-speed motion, sharp impacts can be there is between particle, material under molten state required for instant production, make refractory materials interior solid, improve volume density, reduce the apparent porosity of refractory materials, prevent from expanding, and then promote physical properties such as intensity, heat-shock resistance, the thermal-shock resistance of refractory materials further.
As preferably, vacuum drying vacuum tightness is 0.001-0.008MPa, and drying temperature is 130-150 DEG C, and time of drying is 10-12 hour.
As preferably, the part by weight of raw spirit and mixture is 15:1.
The invention has the beneficial effects as follows
1) Graphene makes goods interior contact more tight, thus because of the stress produced that expands when reducing to burn till, prevents goods from loosening or cracking; The high strength of Graphene ensure that the excellent mechanical property of goods, can promote antiacid caustic corrosion performance and the oxidation-resistance of goods simultaneously;
2) refractory materials interior solid of the present invention, improves volume density, reduces the apparent porosity of refractory materials, prevents from expanding, and then promotes physical properties such as intensity, heat-shock resistance, the thermal-shock resistance of refractory materials further;
3) glass microballon granularity is suitable, good fluidity, dispersity is high, adds glass microballon, can be dispersed in internal height, acceleration of sintering, and have evenly weave construction, improve the intensity of goods and thermal shock resistance, the granularity of nano zine oxide is tiny, can fine pores be filled, reduce the void content of goods, improve volume density;
4) preparation method of the present invention is simple, abundant raw material, is applicable to factorial praluction.
Embodiment
Below in conjunction with specific embodiment, the present invention is further explained, the restriction not to its protection domain.
The particle diameter of the calcium magnesia sand particle that the present invention adopts is 0.2-2mm, and the particle diameter of calcium magnesia sand fine powder is 100-120 μm.
The present invention's additive used is the mixture of diatom ooze, boron nitride, glass microballon and nano zine oxide, and the mass ratio of diatom ooze, boron nitride, glass microballon and nano zine oxide is 5:3:4:7.
Add glass microballon and nano zine oxide after diatom ooze mixes in ethanol with boron nitride, in a water bath after ultrasonic vibration 2h, drying obtains supplementary additive.
The present invention's bonding agent used is the mixture of Seaweed Extract and beeswax, and mass ratio is 2:1, and the preparation method of this bonding agent is as follows: 1) clean: the tap water that marine alga raw material is 45-50 DEG C soaks 2-3 hour, then cleans up;
2) pulverize, centrifugal: the marine alga cleaned up, vacuum breaking, add the ethanol of marine alga volume 30 times and fourth diester solution soaking and boil, the volume ratio of ethanol and fourth diester is 1:1, then centrifugation is removed slag to obtain marine alga clear liquid, the rotating speed of whizzer is 4000 ~ 6000rpm, and centrifugation time is 15-20min;
3) nanofiltration: diluted by the pure water of marine alga clear liquid with 5-10 times of volume, then carries out dialysis by nanofiltration membrane and concentrates, and the 0.1-0.2 that the dialysis of marine alga clear liquid is concentrated into dilution front volume doubly obtains nanofiltration concentrated solution, and the molecular weight cut-off of described nanofiltration membrane is 600-700Da;
4) concentrate drying: after nanofiltration concentrated solution adds beeswax, further vacuum concentration to solid content is 40-60%, and then spraying dry obtains the Powdered bonding agent of water content 2-3% in spray-dryer.
Technical solution of the present invention can utilize existing plasma spraying equipment to complete, such as ZB-80 type or DH-1080 type, DH-X2 type.
In the present invention, if not refer in particular to, the raw material adopted all can be buied from market or this area is conventional, and the method in following embodiment, if no special instructions, is the ordinary method of this area.
Embodiment 1
A kind of mg-ca-carbon refractory, mg-ca-carbon refractory is made up of the raw material of following mass fraction: calcium magnesia sand particle 100 parts, calcium magnesia sand fine powder 40 parts, nano magnesia 15 parts, nano calcium oxide 20 parts, zirconium white 20 parts, Graphene 10 parts, additive 5 parts, bonding agent 7 parts and carbon nano fiber 5 parts.
A kind of preparation method of mg-ca-carbon refractory, each raw material weighs by above proportioning, mixture after mixing take raw spirit as medium milling 10 hours, then powder is obtained at vacuum drying, reaction powder is applied to the plasma arc of 5000 volts, make powder melting, by rare gas element the powder after melting blown to machine be installed with standby in be prepared into the molded article of various desired size, after at 120 DEG C dry 10 hour, at 450 DEG C, be incubated 30min obtain mg-ca-carbon refractory; Vacuum drying vacuum tightness is 0.001-0.008MPa, and drying temperature is 130 DEG C, and time of drying is 10 hours; The part by weight of raw spirit and mixture is 15:1.
The volume density of the mg-ca-carbon refractory that the present embodiment obtains is 4.15g/cm
3, apparent porosity is 10-12%, and cold crushing strength is 240MPa, refractoriness under load > 1750 DEG C, and heat-shock resistance [1100 DEG C of * water-cooleds] is 45 times.
Embodiment 2
A kind of mg-ca-carbon refractory, mg-ca-carbon refractory is made up of the raw material of following mass fraction: calcium magnesia sand particle 110 parts, calcium magnesia sand fine powder 45 parts, nano magnesia 25 parts, nano calcium oxide 25 parts, zirconium white 30 parts, Graphene 15 parts, additive 7 parts, bonding agent 10 parts and carbon nano fiber 8 parts.
A kind of preparation method of mg-ca-carbon refractory, each raw material weighs by above proportioning, mixture after mixing take raw spirit as medium milling 11 hours, then powder is obtained at vacuum drying, reaction powder is applied to the plasma arc of 6000 volts, make powder melting, by rare gas element the powder after melting blown to machine be installed with standby in be prepared into the molded article of various desired size, after at 140 DEG C dry 11 hour, at 465 DEG C, be incubated 40min obtain mg-ca-carbon refractory; Vacuum drying vacuum tightness is 0.001-0.008MPa, and drying temperature is 145 DEG C, and time of drying is 11 hours; The part by weight of raw spirit and mixture is 15:1.
The volume density of the mg-ca-carbon refractory that the present embodiment obtains is 4.25g/cm
3, apparent porosity is 10-12%, and cold crushing strength is 245MPa, refractoriness under load > 1750 DEG C, and heat-shock resistance [1100 DEG C of * water-cooleds] is 48 times.
Embodiment 3
A kind of mg-ca-carbon refractory, mg-ca-carbon refractory is made up of the raw material of following mass fraction: calcium magnesia sand particle 120 parts, calcium magnesia sand fine powder 50 parts, nano magnesia 35 parts, nano calcium oxide 30 parts, zirconium white 35 parts, Graphene 20 parts, additive 10 parts, bonding agent 12 parts and carbon nano fiber 12 parts.
A kind of preparation method of mg-ca-carbon refractory, each raw material weighs by above proportioning, mixture after mixing take raw spirit as medium milling 12 hours, then powder is obtained at vacuum drying, reaction powder is applied to the plasma arc of 7000 volts, make powder melting, by rare gas element the powder after melting blown to machine be installed with standby in be prepared into the molded article of various desired size, after at 150 DEG C dry 12 hour, at 480 DEG C, be incubated 50min obtain mg-ca-carbon refractory; Vacuum drying vacuum tightness is 0.001-0.008MPa, and drying temperature is 150 DEG C, and time of drying is 12 hours; The part by weight of raw spirit and mixture is 15:1.
The volume density of the mg-ca-carbon refractory that the present embodiment obtains is 4.33g/cm
3, apparent porosity is 10-12%, and cold crushing strength is 251MPa, refractoriness under load > 1750 DEG C, and heat-shock resistance [1100 DEG C of * water-cooleds] is 51 times.
Claims (8)
1. a mg-ca-carbon refractory, it is characterized in that, described mg-ca-carbon refractory is made up of the raw material of following mass fraction: calcium magnesia sand particle 100-120 part, calcium magnesia sand fine powder 40-50 part, nano magnesia 15-35 part, nano calcium oxide 20-30 part, zirconium white 20-35 part, Graphene 10-20 part, additive 5-10 part, bonding agent 7-12 part and carbon nano fiber 5-12 part.
2. a kind of mg-ca-carbon refractory according to claim 1, it is characterized in that, described additive is the mixture of diatom ooze, boron nitride, glass microballon and nano zine oxide, and the mass ratio of diatom ooze, boron nitride, glass microballon and nano zine oxide is 5:3:4:7.
3. a kind of mg-ca-carbon refractory according to claim 1, it is characterized in that, described bonding agent is the mixture of Seaweed Extract and beeswax, mass ratio is 2:1, the preparation method of this bonding agent is as follows: 1) clean: the tap water that marine alga raw material is 45-50 DEG C soaks 2-3 hour, then cleans up;
2) pulverize, centrifugal: the marine alga cleaned up, vacuum breaking, add the ethanol of marine alga volume 30 times and fourth diester solution soaking and boil, the volume ratio of ethanol and fourth diester is 1:1, then centrifugation is removed slag to obtain marine alga clear liquid, the rotating speed of whizzer is 4000 ~ 6000rpm, and centrifugation time is 15-20min;
3) nanofiltration: diluted by the pure water of marine alga clear liquid with 5-10 times of volume, then carries out dialysis by nanofiltration membrane and concentrates, and the 0.1-0.2 that the dialysis of marine alga clear liquid is concentrated into dilution front volume doubly obtains nanofiltration concentrated solution, and the molecular weight cut-off of described nanofiltration membrane is 600-700Da;
4) concentrate drying: after nanofiltration concentrated solution adds beeswax, further vacuum concentration to solid content is 40-60%, and then spraying dry obtains the Powdered bonding agent of water content 2-3% in spray-dryer.
4. a kind of mg-ca-carbon refractory according to claim 1 and 2, is characterized in that, adds glass microballon and nano zine oxide after diatom ooze mixes in ethanol with boron nitride, and in a water bath after ultrasonic vibration 2h, drying obtains supplementary additive.
5. a kind of mg-ca-carbon refractory according to claim 1, is characterized in that, the particle diameter of calcium magnesia sand particle is 0.2-2mm, and the particle diameter of calcium magnesia sand fine powder is 100-120 μm.
6. the preparation method of a mg-ca-carbon refractory as claimed in claim 1, it is characterized in that, each raw material weighs by above proportioning, mixture after mixing take raw spirit as medium milling 10-12 hour, then powder is obtained at vacuum drying, reaction powder is applied to the plasma arc of 5000-7000 volt, make powder melting, by rare gas element the powder after melting blown to machine be installed with standby in be prepared into the molded article of various desired size, after dry at 120-150 DEG C 10-12 hour, at 450-480 DEG C, be incubated 30-50min obtain mg-ca-carbon refractory.
7. the preparation method of a kind of mg-ca-carbon refractory according to claim 6, is characterized in that, vacuum drying vacuum tightness is 0.001-0.008MPa, and drying temperature is 130-150 DEG C, and time of drying is 10-12 hour.
8. the preparation method of a kind of mg-ca-carbon refractory according to claim 6, is characterized in that, the part by weight of raw spirit and mixture is 15:1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107235740A (en) * | 2017-06-30 | 2017-10-10 | 长兴泓矿炉料有限公司 | A kind of fiber reinforced refractory material |
| CN107235738A (en) * | 2017-06-30 | 2017-10-10 | 长兴泓矿炉料有限公司 | A kind of preparation method of fiber reinforced refractory material |
| CN107298588A (en) * | 2017-08-14 | 2017-10-27 | 浙江中茂耐火材料股份有限公司 | Low temperature fast firing refractory material and preparation method thereof |
| CN107382336A (en) * | 2017-06-30 | 2017-11-24 | 长兴泓矿炉料有限公司 | A kind of fiber reinforced refractory material powder |
| CN111439990A (en) * | 2020-04-03 | 2020-07-24 | 攀枝花市昌宁冶金材料有限责任公司 | Magnesium-aluminum-carbon gunning mix for high-titanium blast furnace slag high-temperature carbonization electric furnace and preparation method thereof |
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| CN102249712A (en) * | 2011-05-31 | 2011-11-23 | 浙江大学 | Magnesium-calcium hollow sphere and preparation method thereof |
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| CN104190161A (en) * | 2014-09-12 | 2014-12-10 | 济南圣泉倍进陶瓷过滤器有限公司 | Ceramic filter containing graphene for molten metal |
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| CN102249712A (en) * | 2011-05-31 | 2011-11-23 | 浙江大学 | Magnesium-calcium hollow sphere and preparation method thereof |
| CN103601506A (en) * | 2013-10-09 | 2014-02-26 | 瑞泰科技股份有限公司 | Low-porosity magnesium aluminate spinel-zirconia composite sintered refractory material and production technology thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107235740A (en) * | 2017-06-30 | 2017-10-10 | 长兴泓矿炉料有限公司 | A kind of fiber reinforced refractory material |
| CN107235738A (en) * | 2017-06-30 | 2017-10-10 | 长兴泓矿炉料有限公司 | A kind of preparation method of fiber reinforced refractory material |
| CN107382336A (en) * | 2017-06-30 | 2017-11-24 | 长兴泓矿炉料有限公司 | A kind of fiber reinforced refractory material powder |
| CN107298588A (en) * | 2017-08-14 | 2017-10-27 | 浙江中茂耐火材料股份有限公司 | Low temperature fast firing refractory material and preparation method thereof |
| CN111439990A (en) * | 2020-04-03 | 2020-07-24 | 攀枝花市昌宁冶金材料有限责任公司 | Magnesium-aluminum-carbon gunning mix for high-titanium blast furnace slag high-temperature carbonization electric furnace and preparation method thereof |
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