CN103896603B - A kind of refractory castable for Molten salt chlorination furnace and its preparation method and application - Google Patents
A kind of refractory castable for Molten salt chlorination furnace and its preparation method and application Download PDFInfo
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- CN103896603B CN103896603B CN201210584280.6A CN201210584280A CN103896603B CN 103896603 B CN103896603 B CN 103896603B CN 201210584280 A CN201210584280 A CN 201210584280A CN 103896603 B CN103896603 B CN 103896603B
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Abstract
The invention provides a kind of refractory castable for Molten salt chlorination furnace and its preparation method and application.This refractory castable contains corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist and sclerosis additive.Refractory castable provided by the invention has the advantages such as anti-fused salt aggressiveness is good, thermal expansivity is little, good fluidity, can be used for Molten salt chlorination furnace surrounding them, Molten salt chlorination furnace electrode effectively can be avoided to leak salt, ensure TiCl
4steady and continuous produce, have good economic benefit and social benefit.
Description
Technical field
The invention belongs to technical field of refractory materials, be specifically related to a kind of refractory castable for Molten salt chlorination furnace and its preparation method and application.
Background technology
Produce in the technique of titanium sponge, Molten salt chlorination furnace furnace lining adopts clay brick to build by laying bricks or stones, and the clay combined with around Graphite Electrodes can produce small gap in dry shrinkage process around Graphite Electrodes.In fact, within the scope of 20 DEG C-1000 DEG C, the thermal expansivity of clay brick is 4.5-6.0 × 10
-6m/ DEG C, but in this temperature range, the thermal expansivity of Graphite Electrodes is 1.5 × 10
-6m/ DEG C, because thermal expansivity is inconsistent, causes the gap in temperature-rise period between Graphite Electrodes and refractory materials to increase.At the working temperature, fused salt can along this gap toward exosmosing, if the envrionment temperature that fused salt contacts in the process of exosmosing is lower, its front end there will be solidifies, and namely seepage can stop.But because Graphite Electrodes has big current to pass through, itself also can generate heat, salt in the molten state also can conductive exothermal, and the fused salt be therefore in around Graphite Electrodes does not have curing condition all the time, and the fused salt of front end just can along slit gradually toward exosmosing, until flow out outside stove.On the other hand, because the clay anti-fused salt erosion performance of former employing of laying bricks is poor, after salt adding post chlorization stove runs for some time, because the clay temperature around Graphite Electrodes is high, accelerate fused salt deteriorating to clay, easily formed around Graphite Electrodes and leak salt passage.At present, a kind of material is not also had can to solve the problem of Molten salt chlorination furnace leakage salt.
Summary of the invention
The object of the invention is the defect in order to overcome prior art, providing that a kind of anti-fused salt aggressiveness is good, thermal expansivity is little, have the refractory castable of better mobility.
For achieving the above object, the invention provides a kind of refractory castable for Molten salt chlorination furnace, wherein, this refractory castable contains corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist and sclerosis additive.
The present invention also provides the preparation method of this refractory castable, and this preparation method comprises corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist and sclerosis additive mix, and preferably, the method also comprises corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist, sclerosis additive and silicon ash mix.
The present invention also provides this refractory castable for the application in Molten salt chlorination furnace antiseep.
The present invention adopts corundum, mullite, α-Al
2o
3micro mist is main raw material, and is equipped with water reducer, bonding agent and additive, produces that little, the anti-fused salt aggressiveness of a kind of dry shrinkage is good, thermal expansivity is little, have the refractory castable of good mobility.This refractory castable is used for Molten salt chlorination furnace surrounding them, effectively prevent the leakage salt phenomenon of Molten salt chlorination furnace, ensure that TiCl
4steady and continuous produce, there is good economic benefit and social benefit.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification sheets, is used from explanation the present invention, but is not construed as limiting the invention with embodiment one below.In the accompanying drawings:
Fig. 1 is the design sketch that the anti-fused salt of refractory castable provided by the invention corrodes;
Fig. 2 is the schematic diagram of refractory castable provided by the invention for Molten salt chlorination furnace;
Fig. 3 is yield point value measuring apparatus figure.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind of refractory castable for Molten salt chlorination furnace, this refractory castable contains corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist and sclerosis additive.
In the present invention, corundum stable α – Al under referring to natural condition
2o
3variant, mullite refers to that chemical formula is 3Al
2o
32SiO
2rhombic mineral, corundum and mullite are the main raw materials of refractory castable.Described α-Al
2o
3powder size is less than 5 microns usually.Contriver finds, by corundum, mullite and water reducer, bonding agent, α-Al
2o
3micro mist and the mixing of sclerosis additive just can the refractory castablies of accomplished the object of the invention, but the present invention does not limit this.
According to the invention provides refractory castable, the content of each component can be regulated according to actual needs, in order to make the performance of refractory castable better, preferably, with the gross weight of described refractory castable for benchmark, described corundum content is 50-80 % by weight, described mullite content is 1-10 % by weight, described reduced water content is 0.01-0.2 % by weight, and described bonding agent content is 10-30 % by weight, described α-Al
2o
3powder content is 1-10 % by weight, and described sclerosis additive level is 1-5 % by weight, further preferably, described corundum content is 60-70 % by weight, and described mullite content is 4-6 % by weight, and described reduced water content is 0.08-0.12 % by weight, described bonding agent content is 15-25 % by weight, described α-Al
2o
3powder content is 4-6 % by weight, and described sclerosis additive level is 2-3 % by weight.
According to refractory castable provided by the invention, described corundum can be the corundum of this area routine, in order to make refractory castable performance better, preferably, the mixture of the corundum of described corundum to be granularity be 3-8mm, granularity to be the corundum of 0.1-3mm and granularity the be corundum of 0.01-0.08mm, the weight ratio of three can regulate according to actual needs, and the weight ratio of preferred three is 1:(0.8-1.2): (0.5-1).
According to refractory castable provided by the invention, the granularity of described mullite can be selected according to practical situation, and the granularity of preferred described mullite is 0.1-1mm.
According to refractory castable provided by the invention, described water reducer can be the water reducer of this area routine, and in order to play better dissemination and reduce the consumption of bonding agent, under preferable case, described water reducer is tripoly phosphate sodium STPP and/or Sodium hexametaphosphate 99.
According to refractory castable provided by the invention, described bonding agent can be the bonding agent of this area routine, and in order to make the performance of refractory castable better, described bonding agent is preferably aluminium dihydrogen phosphate and/or water glass.The volume density of described bonding agent is preferably greater than and equals 1.35g/cm
3, further preferably, the volume density of described bonding agent is 1.35-1.5g/cm
3.
According to refractory castable provided by the invention, described sclerosis additive can be the sclerosis additive of this area routine, and in order to make the performance of refractory castable better, described sclerosis additive is preferably pure calcium aluminate cement.
According to refractory castable provided by the invention, this refractory castable can also containing silicon ash, the content of described silicon ash can regulate according to practical situation, in order to the mobility and intensity that make refractory castable are better, under preferable case, with the gross weight of described refractory castable for benchmark, described silicon ash content is 1-5 % by weight.
According to refractory castable provided by the invention, a kind of most preferred scheme is that described refractory castable is by corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist, sclerosis additive and silicon ash composition, with the gross weight of described refractory castable for benchmark, described corundum content is 50-80 % by weight, described mullite content is 1-10 % by weight, described reduced water content is 0.01-0.2 % by weight, and described bonding agent content is 10-30 % by weight, described α-Al
2o
3powder content is 1-10 % by weight, described sclerosis additive level is 1-5 % by weight, described silicon ash content is 1-5 % by weight, further preferably, described corundum content is 60-70 % by weight, and described mullite content is 4-6 % by weight, and described reduced water content is 0.08-0.12 % by weight, described bonding agent content is 15-25 % by weight, described α-Al
2o
3powder content is 4-6 % by weight, and described sclerosis additive level is 2-3 % by weight, and described silicon ash content is 1-5 % by weight.But the present invention is not limited thereto.
The present invention also provides the preparation method of described refractory castable, and this preparation method can comprise corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist and sclerosis additive mix, and under preferable case, the method also comprises corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist, sclerosis additive and silicon ash mix.
According to preparation method provided by the invention, the consumption of each component can regulate according to actual needs, in order to make the refractory castable performance of preparation better, preferably, the consumption of each component makes the gross weight of the refractory castable obtained for benchmark, and described corundum content is 50-80 % by weight, described mullite content is 1-10 % by weight, described reduced water content is 0.01-0.2 % by weight, and described bonding agent content is 10-30 % by weight, described α-Al
2o
3powder content is 1-10 % by weight, and described sclerosis additive level is 1-5 % by weight, further preferably, described corundum content is 60-70 % by weight, and described mullite content is 4-6 % by weight, and described reduced water content is 0.08-0.12 % by weight, described bonding agent content is 15-25 % by weight, described α-Al
2o
3powder content is 4-6 % by weight, and described sclerosis additive level is 2-3 % by weight.
According to preparation method provided by the invention, described mixing can adopt this area various ways, and in order to make the refractory castable performance of preparation better, preferably adopt the method for following mixing, the method for described mixing comprises: by corundum, mullite, water reducer, α-Al
2o
3micro mist carries out being mixed to get mixture with the bonding agent accounting for bonding agent total amount 1/3-1/2, and described mixture is carried out ageing mixture, is then mixed with the bonding agent accounting for bonding agent total amount 1/2-2/3 with sclerosis additive by the mixture after ageing mixture; Further preferably, the method for described mixing comprises: by corundum, mullite, water reducer, silicon ash, α-Al
2o
3micro mist carries out being mixed to get mixture with the bonding agent accounting for bonding agent total amount 1/3-1/2, and described mixture is carried out ageing mixture, is then mixed with the bonding agent accounting for bonding agent total amount 1/2-2/3 with sclerosis additive by the mixture after ageing mixture.Bulging may be there is owing to adopting in the process of different material production mould material, namely gas is produced in mould material, mould material is foamed, may reduce the void content of intensity and increase mould material inside, contriver finds to adopt above-mentioned preferred hybrid mode the material eliminating producing gas can be adjusted and avoid the generation of bulging phenomenon.
Preparation in accordance with the present invention, described ageing mixture refers to mixed mixture, under suitable humidity and temperature, store certain hour.Described humidity, temperature and time can be selected according to practical situation, and the time of described ageing mixture is preferably 20-30h.
The present invention also provides described refractory castable for the application in Molten salt chlorination furnace antiseep.The mode of application can be selected according to practical situation, such as, as shown in Figure 2, for Molten salt chlorination furnace surrounding them, between clay brick and Graphite Electrodes.
According to the application of refractory castable provided by the invention, the consumption of described refractory castable can regulate according to practical situation.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Below will be described the present invention by embodiment.
In the examples below, corundum is the compact alumina adopting electric smelting method to produce, and mullite is the electrofused mullite adopting electric smelting method to produce, and silicon ash is the dust-removing powder produced ferrosilicon or produce Pure Silicon Metal, and pure calcium aluminate cement is the CA71 produced by Kai Nuosi, α-Al
2o
3micro mist carrys out free Chalco.
Embodiment 1
The present embodiment is for illustration of the preparation that the invention provides refractory castable.
First corundum is ground to 8mm, 3mm, 0.08mm tri-kinds of different grain sizes, mullite being ground to granularity is 1mm.With the gross weight of the refractory castable of required preparation for benchmark, by each raw material according to 8mm corundum 24 % by weight, 3mm corundum 24 % by weight, 0.08mm corundum 15 % by weight, mullite 5 % by weight, silicon ash 5 % by weight, α-Al
2o
3(volume density is 1.35g/cm for micro mist 5 % by weight, tripoly phosphate sodium STPP 0.1 % by weight, aluminium dihydrogen phosphate
3) 6.5 % by weight ratio mix and obtain mixture, mixture is carried out ageing mixture, and the ageing mixture time is 24h, and then by the mixture after ageing mixture and pure calcium aluminate cement 2.5 % by weight and aluminium dihydrogen phosphate, (volume density is 1.35g/cm
3) 12.9 % by weight to mix, be Molten salt chlorination furnace refractory castable.
Embodiment 2
The present embodiment is for illustration of the preparation that the invention provides refractory castable.
First corundum is ground to 7mm, 2mm, 0.08mm tri-kinds of different grain sizes, mullite being ground to granularity is 1mm.With the gross weight of the refractory castable of required preparation for benchmark, by each raw material according to 7mm corundum 24 % by weight, 2mm corundum 24 % by weight, 0.08mm corundum 20 % by weight, mullite 5 % by weight, α-Al
2o
3(volume density is 1.35g/cm for micro mist 5 % by weight, tripoly phosphate sodium STPP 0.1 % by weight, aluminium dihydrogen phosphate
3) 6.8 % by weight ratio mix and obtain mixture, mixture is carried out ageing mixture, and the ageing mixture time is 24h, and then by the mixture after ageing mixture and pure calcium aluminate cement 2.1 % by weight and aluminium dihydrogen phosphate, (volume density is 1.35g/cm
3) 13 % by weight to mix, be Molten salt chlorination furnace refractory castable.
Embodiment 3
The present embodiment is for illustration of the preparation that the invention provides refractory castable.
First corundum is ground to 6mm, 1mm, 0.08mm tri-kinds of different grain sizes, mullite being ground to granularity is 1mm.With the gross weight of the refractory castable of required preparation for benchmark, by each raw material according to 6mm corundum 24 % by weight, 1mm corundum 24 % by weight, 0.08mm corundum 19 % by weight, mullite 5 % by weight, silicon ash 3 % by weight, α-Al
2o
3(volume density is 1.35g/cm for micro mist 5 % by weight, Sodium hexametaphosphate 99 0.1 % by weight, aluminium dihydrogen phosphate
3) 7 % by weight ratio mix and obtain mixture, mixture is carried out ageing mixture, and the ageing mixture time is 24h, and then by the mixture after ageing mixture and pure calcium aluminate cement 2.9 % by weight and aluminium dihydrogen phosphate, (volume density is 1.35g/cm
3) 10 % by weight to mix, be Molten salt chlorination furnace refractory castable.
Embodiment 4
The present embodiment is for illustration of the preparation that the invention provides refractory castable.
First corundum is ground to 5mm, 0.5mm, 0.08mm tri-kinds of different grain sizes, mullite being ground to granularity is 1mm.With the gross weight of the refractory castable of required preparation for benchmark, by each raw material according to 5mm corundum 25 % by weight, 0.5mm corundum 23 % by weight, 0.08mm corundum 17.5 % by weight, mullite 6 % by weight, silicon ash 2.5 % by weight, α-Al
2o
3(volume density is 1.35g/cm for micro mist 4 % by weight, Sodium hexametaphosphate 99 0.12 % by weight, aluminium dihydrogen phosphate
3) 6 % by weight ratio mix and obtain mixture, mixture is carried out ageing mixture, and the ageing mixture time is 24h, and then by the mixture after ageing mixture and pure calcium aluminate cement 2.88 % by weight and aluminium dihydrogen phosphate, (volume density is 1.35g/cm
3) 13 % by weight to mix, be Molten salt chlorination furnace refractory castable.
Performance test
1, the performance test of refractory castable main raw material
Respectively to corundum, mullite, silicon ash, α-Al
2o
3chemical composition and the refractoriness of micro mist and pure calcium aluminate cement measure.Measuring method is GB/T3044-89(2004), GB6900.2 ~ 6900.5, GB/T6900-2006, GB7322.
Result is as shown in table 1 below.
The physical and chemical index of table 1 refractory castable main raw material
2, the performance test of refractory castable
The clay brick of the refractory castable prepared by embodiment 1-4 and prior art is carried out to the mensuration of chemical composition, volume density, compressive strength, reheating linear change rate on reheating, mobility and thermal expansivity.Measuring method is respectively GB/T6900-2006, GB/T2997-2006, GB/T5072.2-2006, GB/T5988-2006, GB/T7320.1-2006, fluidity test method are as follows.
Refractory castable fluidity test method:
Empty round platform mould (see figure 3) is placed on platform, then the mould material be stirred is poured in mould, after material feeding to be poured is full of, the mould material exceeding mould suitable for reading is scraped off, mention mould vertically upward immediately, open vibrating device simultaneously, stop after vibrating for 10 seconds, after vibration, mould material is rounded substantially, this circular flat is divided into 8 deciles, measure the diameter at 4 places, the mean value of calculated diameter, calculate yield point value by following formula mould material:
The performance test results is as shown in table 2 below.
The physical and chemical index of table 2 refractory castable
The result showing 1-2 from embodiment 1-4 and performance test is known, compared with the clay brick of prior art, refractory castable provided by the invention has the advantages such as anti-fused salt aggressiveness is good, thermal expansivity is little, good fluidity, can be used for Molten salt chlorination furnace surrounding them, Molten salt chlorination furnace electrode effectively can be avoided to leak salt, ensure TiCl
4steady and continuous produce, have good economic benefit and social benefit.
Claims (9)
1. for a refractory castable for Molten salt chlorination furnace, it is characterized in that, this refractory castable is by corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist, sclerosis additive and silicon ash composition, wherein, with the gross weight of described refractory castable for benchmark, described corundum content is 50-80 % by weight, described mullite content is 1-10 % by weight, described reduced water content is 0.01-0.2 % by weight, and described bonding agent content is 10-30 % by weight, described α-Al
2o
3powder content is 1-10 % by weight, and described sclerosis additive level is 1-5 % by weight, and described silicon ash content is 1-5 % by weight, and described corundum is α-Al stable under natural condition
2o
3variant,
Wherein, the mixture of the corundum of described corundum to be granularity be 3-8mm, granularity to be the corundum of 0.1-3mm and granularity the be corundum of 0.01-0.08mm, the weight ratio of three is 1:(0.8-1.2): (0.5-1), the granularity of described mullite is 0.1-1mm, and the volume density of described bonding agent is more than or equal to 1.35g/cm
3.
2. refractory castable according to claim 1, wherein, with the gross weight of described refractory castable for benchmark, described corundum content is 60-70 % by weight, described mullite content is 4-6 % by weight, described reduced water content is 0.08-0.12 % by weight, and described bonding agent content is 15-25 % by weight, described α-Al
2o
3powder content is 4-6 % by weight, and described sclerosis additive level is 2-3 % by weight.
3. refractory castable according to claim 1 and 2, wherein, described water reducer is tripoly phosphate sodium STPP and/or Sodium hexametaphosphate 99, and described bonding agent is aluminium dihydrogen phosphate and/or water glass, and described sclerosis additive is pure calcium aluminate cement.
4. refractory castable according to claim 1, wherein, the volume density of described bonding agent is 1.35-1.5g/cm
3.
5. claim 1 is for a preparation method for the refractory castable of Molten salt chlorination furnace, it is characterized in that, this preparation method comprises corundum, mullite, water reducer, bonding agent, α-Al
2o
3micro mist, sclerosis additive and silicon ash mix,
Wherein, the consumption of each component makes the gross weight of the refractory castable obtained for benchmark, and described corundum content is 50-80 % by weight, described mullite content is 1-10 % by weight, described reduced water content is 0.01-0.2 % by weight, and described bonding agent content is 10-30 % by weight, described α-Al
2o
3powder content is 1-10 % by weight, and described sclerosis additive level is 1-5 % by weight, and described silicon ash content is 1-5 % by weight.
6. preparation method according to claim 5, wherein, described corundum content is 60-70 % by weight, and described mullite content is 4-6 % by weight, and described reduced water content is 0.08-0.12 % by weight, and described bonding agent content is 15-25 % by weight, described α-Al
2o
3powder content is 4-6 % by weight, and described sclerosis additive level is 2-3 % by weight.
7. the preparation method according to claim 5 or 6, wherein, the method for described mixing comprises: by corundum, mullite, water reducer, silicon ash, α-Al
2o
3micro mist carries out being mixed to get mixture with the bonding agent accounting for bonding agent total amount 1/3-1/2, and described mixture is carried out ageing mixture, is then mixed with the bonding agent accounting for bonding agent total amount 1/2-2/3 with sclerosis additive by the mixture after ageing mixture.
8. preparation method according to claim 7, wherein, the time of described ageing mixture is 20-30h.
9. the refractory castable in claim 1-4 described in any one is for the application in Molten salt chlorination furnace antiseep.
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| CN109456068A (en) * | 2018-11-09 | 2019-03-12 | 长沙县新光特种陶瓷有限公司 | A kind of castable refractory |
| CN109678532A (en) * | 2018-11-09 | 2019-04-26 | 长沙县新光特种陶瓷有限公司 | A kind of castable refractory |
| CN109336568A (en) * | 2018-11-09 | 2019-02-15 | 长沙县新光特种陶瓷有限公司 | A kind of castable refractory |
| CN109678531A (en) * | 2018-11-09 | 2019-04-26 | 长沙县新光特种陶瓷有限公司 | A kind of castable refractory |
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| CN1597608A (en) * | 2004-07-27 | 2005-03-23 | 西安秦翔科技有限责任公司 | Lining material composition of mains frequency core induction melt furnace |
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