CN106380221A - Mullite lightweight fireproof material and preparation method thereof - Google Patents
Mullite lightweight fireproof material and preparation method thereof Download PDFInfo
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- CN106380221A CN106380221A CN201610772555.7A CN201610772555A CN106380221A CN 106380221 A CN106380221 A CN 106380221A CN 201610772555 A CN201610772555 A CN 201610772555A CN 106380221 A CN106380221 A CN 106380221A
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Abstract
The invention discloses a mullite lightweight fireproof material and a preparation method thereof. The mullite lightweight fireproof material is prepared from alumina, calcium oxide, calcium oxide, magnesium oxide, titanium oxide, calcium carbonate, and a pore-foaming agent, wherein the pore-foaming agent is composed of cane sugar, carbon powder, polyethylene microsphere, diatomite, and copper sulfate pentahydrate. The fireproof material is prepared by the following steps: ball milling, wet mixing, moulding, sintering, and a post treatment. The provided mullite lightweight fireproof material has the advantages of low volume density, large porosity, high using temperature, high compression strength, low thermal conductivity, and good thermal insulation effect.
Description
Technical field
The present invention relates to refractory material manufacturing technology field, especially relate to a kind of mullite lightweight refracrory and its system
Preparation Method.
Background technology
In traditional sense, refractory material refers to that refractoriness is not less than 1580 DEG C of Inorganic Non-metallic Materials, and it is for height
The basic material of temperature technique service, is used as the structural material of the Thermal Equipments such as high temperature kiln, and industrial high temperature container and portion
The material of part, and corresponding physicochemical change and mechanism can be born.
Most of refractory material is with natural crystal（As fire clay, silica, magnesite, dolomite）For raw material manufacture
, using some raw materials of industry and artificial-synthetic material（As commercial alumina, carborundum, mullite synthesizing, synthetic spinel
Deng）Also increasing, therefore, the species of refractory material is a lot.Refractory material can be divided into the siliceous, silicon of oxidation according to mineral composition
Sour aluminum, magnesia, dolomite matter, olivine matter, spinel, containing carbonaceous, contain zirconia refractory and special refractory；Press
Natural crystal and artifact can be divided into according to manufacture method；Block elements and unshape refractory can be divided into by its mode；
Not burned product, burnt product and melt-cast products can be divided into according to heat treatment mode；Can be divided into common, senior and special according to refractoriness
Level refractory product；Acidity, neutral and basic refractory can be divided into according to chemical property；Lightweight and weight can be divided into according to its density
Fire resistant materials；Shape and size according to its product can be divided into standard brick, special shaped brick, special special shaped brick, pipe and flame ware；Also
Blast furnace can be divided into use by its application, cement kiln is used, glass furnace use, ceramic kiln refractory etc..
Lightweight refracrory is used as heat-barrier material on Industrial Stoves and other Thermal Equipments, and it has porosity height, body
The refractory material that long-pending density is little, thermal conductivity is low；Industrial Stoves masonry accumulation of heat loss and body of heater surface heat radiating loss account for fuel and disappear
The 24～45% of consumption, energy loss is huge so that energy utilization rate is low, using the lightweight refracrory that thermal conductivity is low, thermal capacity is little
Make furnace binding material, fuel consumption can be saved；Simultaneously as kiln can be rapidly heated and cool down, equipment can be improved and produce
Efficiency；Body of heater weight can also be mitigated, simplify kiln construction, improve product quality, reduce environment temperature, improve working conditions.But
Be lightweight refracrory there is also mechanical strength low it is impossible to be used for load-bearing, and its anti-wear performance is also poor.
Content of the invention
For solving the above problems, a kind of porosity of present invention offer is high, bulk density is less, thermal conductivity is low, and mechanics
Intensity and anti-wear performance are higher than the mullite lightweight refracrory of general lightweight refracrory；
Present invention also offers a kind of step is succinct and high porosity, low bulk density, lower thermal conductivity, higher force can be obtained
Intensity and the preparation method of high wear resistance mullite lightweight refracrory.
For achieving the above object, the technical solution used in the present invention is as follows：
A kind of mullite lightweight refracrory, is obtained by the raw material of following weight portion：660～710 parts of aluminum oxide, silica 180
～210 parts, 72～90 parts of calcium oxide, 54～72 parts of magnesia, 27～36 parts of titanium oxide, 10～20 parts of calcium carbonate, perforating agent 300
～500 parts.
Aluminum oxide can form mullite phase with the inorganic oxide of silica system, and mullite is that one kind has higher melt
Inorganic compound, more than 1850 DEG C, sieve and silica-sesquioxide system is a common and excellent refractory material system to its fusing point,
Simultaneous oxidation magnesium, calcium oxide are also the inorganic oxide with higher melt, and reacting formation solid solution with sial system oxide can
With promote refractory material refractoriness, but due to the raw material such as sial system oxide and magnesia, calcium oxide reaction temperature relatively
High so that the synthesis temperature of refractory material is higher, energy consumption is also very big, in order to not affect refractoriness or less impact refractoriness
Under the premise of suitably reduce synthesis temperature, therefore add again in the feed and there is the sintering aid reducing synthesis temperature, titanium oxide is
Some have the sintering aid of superperformance, can significantly reduce the synthesis temperature of refractory material in the case of a small amount of interpolation
Degree, the addition of this several sintering aid simultaneously also will not cause a larger shadow as potassium sodium system sintering aid to refractoriness
Ring.
Preferably, the purity of aluminum oxide is more than 98%, the purity of silica is more than 95%.
Preferably, perforating agent is made up of the raw material of following weight portion：20 parts of sucrose, 40～60 parts of powdered carbon, polyethylene is micro-
40～80 parts of ball, 50～60 parts of diatomite, 40～50 parts of cupric sulfate pentahydrate.
Lightweight refracrory is the effect due to wherein having more pore with lightweight heat-proof, prepares in prior art
Using single perforating agent, the generally more original perforating agent such as wood chip lightweight refracrory more；Single perforating agent, duct shape
The temperature becoming is single, and forms duct due to being almost in same temperature interval, namely in order to be formed in the middle of refractory material
Pore, can discharge substantial amounts of gas in same temperature interval, and the impact of a large amount of gases in the short time can cause structure of refractory
The mechanical strength becoming especially loose, prepared refractory material is very poor；Meanwhile, in prior art, some perforating agents are relatively low
Just make refractory material be internally formed duct when warm, but temperature raise after, under pyroreaction these ducts can be closed again or
Person is padded, and causes the porosity to decline, or even refractory material occurs collapse.Using compound perforating agent therefore in the present invention, make
Obtaining different phase in 100～1200 DEG C of interval ranges all can have perforating agent generation gas to form pore refractory material, system
The release of hole agent decomposition gas more relaxes, and the duration is also longer, does not thus result in gas and discharges at short notice, keeps away
Exempt from gas and impact the especially loose unfavorable situation of the structure of refractory leading to it is also possible to avoid continuing pyroreaction posterior spiracle
Situation about again being filled up.
These perforating agents are decomposed the different types of gas of releasing in the different times of whole pyroreaction, 100～
During 150 DEG C of temperature, cupric sulfate pentahydrate loses the crystallization water, and the char sucrose release steam in 300～450 DEG C of temperature, 600～800
During DEG C temperature, polyethylene microballoon occurs thermal decomposition to release gas, and the charcoal being formed after char sucrose and powdered carbon are also in this temperature range
React releasing gas, and copper sulphate also decomposes in this temperature range and generates sulfurous gas and cupric oxide, finally 1000～
In 1200 DEG C of temperature ranges, in perforating agent, all of high temperature decomposable asymmetric choice net material decomposes generation gas completely, and all substances become steady
Fixed.Many kinds of substance in perforating agent produces different types of gas so that being obtained in the different decomposition of different temperatures occurrence degree
Refractory material in pore abundanter, the distribution in aperture is also more various and uniform, and in whole process produce gas
Body, occurs drilling reaction to make situation about again will not be filled up because of the pore that reaction temperature raised portion first generates.
A kind of preparation method of mullite lightweight refracrory, comprises the following steps：
a）Add the absolute ethyl alcohol of 2～2.5 times of raw material weight in addition to perforating agent in the raw material in addition to perforating agent, in rotating speed be
Ball milling 4～6 hours under 2000～2500rpm, are then added thereto to perforating agent again, are ball under 1000～1200rpm in rotating speed
Mill 1～2 hour, finally dries；
b）By the raw material compression molding after processing through step a；
c）Raw material after compression molding is sintered, is started to warm up by room temperature, be incubated 20～40 minutes at 100～150 DEG C,
300～450 DEG C are incubated 20～40 minutes, are incubated 60～80 minutes at 600～800 DEG C, little in 1000～1200 DEG C of insulations 1～3
When, sinter 6～8 hours at 1300～1400 DEG C, then naturally cool to room temperature, prepared mullite lightweight refracrory first product；
d）The mullite lightweight refracrory first product that will be obtained, soaks 20～60 minutes, then cleaning, drying in hydrochloric acid solution
Mullite lightweight refracrory is obtained afterwards.
Two step ball-milling methods make the raw material more uniform and smooth in addition to perforating agent, improve sintering character it is also possible to make to burn
The refractory material of knot is more fine and close in non-bore region, strengthens intensity；The interval sintering method of multi-temperature is cooperation drilling
The species of agent, allows different perforating agents play the effect of drilling within the scope of respective temperature；When last hydrochloric acid solution soaks
In order to remove the unreacted reactant of some impact refractoriness such as remaining, unsintered calcium oxide etc. in apparent pore.
Preferably, the pressure of compression molding is 10～12MPa in step b.
Preferably, in step b, raw material carries out isostatic cool pressing after 10～12MPa compression molding again under 12～14MPa
Shaping, the dwell time is 1～2 minute.
Preferably, the pH value of hydrochloric acid solution is 5.8～6.2 in step d.
Therefore, the invention has the advantages that：
（1）Refractory material in the present invention has a relatively low bulk density, the larger porosity；
（2）Refractory material in the present invention also has higher Shi Yong temperature and higher compressive resistance；
（3）Refractory material in the present invention also has relatively low thermal conductivity, has good heat-blocking action.
Specific embodiment
With reference to specific embodiment, technical scheme is further described.
Embodiment 1
A kind of mullite lightweight refracrory, is obtained by the raw material of following weight portion：660 parts of aluminum oxide, 180 parts of silica, oxygen
Change 72 parts of calcium, 54 parts of magnesia, 27 parts of titanium oxide, 10 parts of calcium carbonate, 300 parts of perforating agent；
Wherein, perforating agent is made up of the raw material of following weight portion：20 parts of sucrose, 40 parts of powdered carbon, 40 parts of polyethylene microballoon, diatomite
50 parts, 40 parts of cupric sulfate pentahydrate.
A kind of preparation method of mullite lightweight refracrory, comprises the following steps：
a）Add the absolute ethyl alcohol of 2 times of raw material weight in addition to perforating agent in the raw material in addition to perforating agent, be 2000rpm in rotating speed
Lower ball milling 4 hours, is then added thereto to perforating agent again, is ball milling under 1000rpm 1 hour in rotating speed, finally dries；
b）By the raw material compression molding after processing through step a；The pressure of compression molding is 10MPa；
c）Raw material after compression molding is sintered, is started to warm up by room temperature, be incubated 20 minutes at 100 DEG C, be incubated at 300 DEG C
20 minutes, it is incubated 60 minutes at 600 DEG C, is incubated 1 hour at 1000 DEG C, sinter 6 hours at 1300 DEG C, then naturally cool to room
Temperature, prepared mullite lightweight refracrory first product；
d）The mullite lightweight refracrory first product that will be obtained, soaks in hydrochloric acid solution 20 minutes, then makes after cleaning, drying
Obtain mullite lightweight refracrory.
Embodiment 2
A kind of mullite lightweight refracrory, is obtained by the raw material of following weight portion：685 parts of aluminum oxide, 195 parts of silica, oxygen
Change 80 parts of calcium, 60 parts of magnesia, 32 parts of titanium oxide, 15 parts of calcium carbonate, 400 parts of perforating agent；
Wherein, perforating agent is made up of the raw material of following weight portion：20 parts of sucrose, 50 parts of powdered carbon, 60 parts of polyethylene microballoon, diatomite
55 parts, 45 parts of cupric sulfate pentahydrate.
A kind of preparation method of mullite lightweight refracrory, comprises the following steps：
a）Add the absolute ethyl alcohol of 2.2 times of raw material weight in addition to perforating agent in the raw material in addition to perforating agent, in rotating speed be
Ball milling 5 hours under 2200rpm, are then added thereto to perforating agent again, are ball milling under 1100rpm 1.5 hours in rotating speed, finally dry
Dry；
b）By the raw material compression molding after processing through step a；The pressure of compression molding is 11MPa；
c）Raw material after compression molding is sintered, is started to warm up by room temperature, be incubated 30 minutes at 120 DEG C, be incubated at 375 DEG C
30 minutes, it is incubated 70 minutes at 7800 DEG C, is incubated 2 hours at 1100 DEG C, sinter 7 hours at 1350 DEG C, then naturally cool to
Room temperature, prepared mullite lightweight refracrory first product；
d）The mullite lightweight refracrory first product that will be obtained, soaks in hydrochloric acid solution 40 minutes, then makes after cleaning, drying
Obtain mullite lightweight refracrory.
Embodiment 3
A kind of mullite lightweight refracrory, is obtained by the raw material of following weight portion：710 parts of aluminum oxide, 210 parts of silica, oxygen
Change 90 parts of calcium, 72 parts of magnesia, 36 parts of titanium oxide, 20 parts of calcium carbonate, 500 parts of perforating agent；
Wherein, perforating agent is made up of the raw material of following weight portion：20 parts of sucrose, 60 parts of powdered carbon, 80 parts of polyethylene microballoon, diatomite
60 parts, 50 parts of cupric sulfate pentahydrate.
A kind of preparation method of mullite lightweight refracrory, comprises the following steps：
a）Add the absolute ethyl alcohol of 2.5 times of raw material weight in addition to perforating agent in the raw material in addition to perforating agent, in rotating speed be
Ball milling 6 hours under 2500rpm, are then added thereto to perforating agent again, are ball milling under 1200rpm 2 hours in rotating speed, finally dry
Dry；
b）By the raw material compression molding after processing through step a；The pressure of compression molding is 12MPa；
c）Raw material after compression molding is sintered, is started to warm up by room temperature, be incubated 40 minutes at 150 DEG C, be incubated at 450 DEG C
40 minutes, it is incubated 80 minutes at 800 DEG C, is incubated 3 hours at 1200 DEG C, sinter 8 hours at 1400 DEG C, then naturally cool to room
Temperature, prepared mullite lightweight refracrory first product；
d）The mullite lightweight refracrory first product that will be obtained, soaks in hydrochloric acid solution 60 minutes, then makes after cleaning, drying
Obtain mullite lightweight refracrory.
Embodiment 4
A kind of mullite lightweight refracrory, is obtained by the raw material of following weight portion：660 parts of aluminum oxide, 210 parts of silica, oxygen
Change 72 parts of calcium, 54 parts of magnesia, 27 parts of titanium oxide, 10 parts of calcium carbonate, 300 parts of perforating agent；The purity of aluminum oxide is 98%, oxidation
The purity of silicon is 95%；
Wherein, perforating agent is made up of the raw material of following weight portion：20 parts of sucrose, 40 parts of powdered carbon, 40 parts of polyethylene microballoon, diatomite
50 parts, 40 parts of cupric sulfate pentahydrate.
A kind of preparation method of mullite lightweight refracrory, comprises the following steps：
a）Add the absolute ethyl alcohol of 2 times of raw material weight in addition to perforating agent in the raw material in addition to perforating agent, be 2000rpm in rotating speed
Lower ball milling 4 hours, is then added thereto to perforating agent again, is ball milling under 1000rpm 1 hour in rotating speed, finally dries；
b）Raw material after processing through step a is carried out cold isostatic compaction, pressurize after 10MPa compression molding again under 12MPa
Time is 1 minute；
c）Raw material after compression molding is sintered, is started to warm up by room temperature, be incubated 20 minutes at 100 DEG C, be incubated at 300 DEG C
20 minutes, it is incubated 60 minutes at 600 DEG C, is incubated 1～3 hour at 1000 DEG C, sinter 6 hours at 1300 DEG C, then natural cooling
To room temperature, prepared mullite lightweight refracrory first product；
d）Will be obtained mullite lightweight refracrory first product, pH value be 5.8 hydrochloric acid solution in soak 20 minutes, then clearly
Mullite lightweight refracrory is obtained after washing drying.
Embodiment 5
A kind of mullite lightweight refracrory, is obtained by the raw material of following weight portion：680 parts of aluminum oxide, 190 parts of silica, oxygen
Change 78 parts of calcium, 60 parts of magnesia, 32 parts of titanium oxide, 15 parts of calcium carbonate, 400 parts of perforating agent；The purity of aluminum oxide is 99%, oxidation
The purity of silicon is 98%；
Wherein, perforating agent is made up of the raw material of following weight portion：20 parts of sucrose, 50 parts of powdered carbon, 60 parts of polyethylene microballoon, diatomite
55 parts, 45 parts of cupric sulfate pentahydrate.
A kind of preparation method of mullite lightweight refracrory, comprises the following steps：
a）Add the absolute ethyl alcohol of 2.3 times of raw material weight in addition to perforating agent in the raw material in addition to perforating agent, in rotating speed be
Ball milling 5 hours under 2300rpm, are then added thereto to perforating agent again, are ball milling under 1100rpm 1.5 hours in rotating speed, finally dry
Dry；
b）Raw material after processing through step a is carried out cold isostatic compaction, pressurize after 11MPa compression molding again under 13MPa
Time is 1.5 minutes；
c）Raw material after compression molding is sintered, is started to warm up by room temperature, be incubated 30 minutes at 130 DEG C, be incubated at 380 DEG C
30 minutes, it is incubated 70 minutes at 700 DEG C, is incubated 23 hours at 1100 DEG C, sinter 7 hours at 1350 DEG C, then naturally cool to
Room temperature, prepared mullite lightweight refracrory first product；
d）Will be obtained mullite lightweight refracrory first product, pH value be 6 hydrochloric acid solution in soak 40 minutes, then clean
Mullite lightweight refracrory is obtained after drying.
Embodiment 6
A kind of mullite lightweight refracrory, is obtained by the raw material of following weight portion：660 parts of aluminum oxide, 210 parts of silica, oxygen
Change 90 parts of calcium, 72 parts of magnesia, 36 parts of titanium oxide, 20 parts of calcium carbonate, 500 parts of perforating agent；The purity of aluminum oxide is 99.9%, oxygen
The purity of SiClx is 99%；
Wherein, perforating agent is made up of the raw material of following weight portion：20 parts of sucrose, 60 parts of powdered carbon, 80 parts of polyethylene microballoon, diatomite
60 parts, 50 parts of cupric sulfate pentahydrate.
A kind of preparation method of mullite lightweight refracrory, comprises the following steps：
a）Add the absolute ethyl alcohol of 2.5 times of raw material weight in addition to perforating agent in the raw material in addition to perforating agent, in rotating speed be
Ball milling 6 hours under 2500rpm, are then added thereto to perforating agent again, are ball milling under 1200rpm 2 hours in rotating speed, finally dry
Dry；
b）Raw material after processing through step a is carried out cold isostatic compaction, pressurize after 12MPa compression molding again under 14MPa
Time is 2 minutes；
c）Raw material after compression molding is sintered, is started to warm up by room temperature, be incubated 40 minutes at 150 DEG C, be incubated at 450 DEG C
40 minutes, it is incubated 80 minutes at 800 DEG C, is incubated 3 hours at 1200 DEG C, sinter 8 hours at 1400 DEG C, then naturally cool to room
Temperature, prepared mullite lightweight refracrory first product；
d）Will be obtained mullite lightweight refracrory first product, pH value be 6.2 hydrochloric acid solution in soak 60 minutes, then clearly
Mullite lightweight refracrory is obtained after washing drying.
Technical indicator：
1. the porosity 40～45%；
2. bulk density 1.5g/cm3And it is following；
3. highest can use 1300 DEG C of temperature；
4. thermal conductivity（Under 1000 DEG C of environment）：0.8W/（m·℃）
5. cold crushing strength：≥200MPa.
Claims (7)
1. a kind of mullite lightweight refracrory is it is characterised in that be obtained by the raw material of following weight portion：Aluminum oxide 660～710
Part, 180～210 parts of silica, 72～90 parts of calcium oxide, 54～72 parts of magnesia, 27～36 parts of titanium oxide, calcium carbonate 10～20
Part, 300～500 parts of perforating agent.
2. a kind of mullite lightweight refracrory according to claim 1 it is characterised in that：The purity of described aluminum oxide is
More than 98%, the purity of silica is more than 95%.
3. a kind of mullite lightweight refracrory according to claim 1 is it is characterised in that described perforating agent is by following
The raw material composition of weight portion：20 parts of sucrose, 40～60 parts of powdered carbon, 40～80 parts of polyethylene microballoon, 50～60 parts of diatomite, five water
40～50 parts of copper sulphate.
4. a kind of preparation method of mullite lightweight refracrory according to claim 1 is it is characterised in that include following
Step：
a）Add the absolute ethyl alcohol of 2～2.5 times of raw material weight in addition to perforating agent in the raw material in addition to perforating agent, in rotating speed be
Ball milling 4～6 hours under 2000～2500rpm, are then added thereto to perforating agent again, are ball under 1000～1200rpm in rotating speed
Mill 1～2 hour, finally dries；
b）By the raw material compression molding after processing through step a；
c）Raw material after compression molding is sintered, is started to warm up by room temperature, be incubated 20～40 minutes at 100～150 DEG C,
300～450 DEG C are incubated 20～40 minutes, are incubated 60～80 minutes at 600～800 DEG C, little in 1000～1200 DEG C of insulations 1～3
When, sinter 6～8 hours at 1300～1400 DEG C, then naturally cool to room temperature, prepared mullite lightweight refracrory first product；
d）The mullite lightweight refracrory first product that will be obtained, soaks 20～60 minutes, then cleaning, drying in hydrochloric acid solution
Mullite lightweight refracrory is obtained afterwards.
5. a kind of mullite lightweight refracrory according to claim 4 preparation method it is characterised in that：Described step
In b, the pressure of compression molding is 10～12MPa.
6. a kind of mullite lightweight refracrory according to claim 4 or 5 preparation method it is characterised in that：Described
In step b, raw material carries out cold isostatic compaction after 10～12MPa compression molding again under 12～14MPa, and the dwell time is 1
～2 minutes.
7. a kind of mullite lightweight refracrory according to claim 4 preparation method it is characterised in that：Described step
In d, the pH value of hydrochloric acid solution is 5.8～6.2.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041096A (en) * | 2019-01-16 | 2019-07-23 | 深圳陶陶科技有限公司 | Diatomite-based Porous Ceramics and preparation method thereof and system |
| CN110698188A (en) * | 2019-11-29 | 2020-01-17 | 湖北理工学院 | Method for preparing mullite powder from waste diatomite and mullite powder prepared based on method |
| CN111302773A (en) * | 2020-03-26 | 2020-06-19 | 攀枝花学院 | Preparation method of mullite porous ceramic |
| CN113292316A (en) * | 2021-05-10 | 2021-08-24 | 江苏苏嘉集团新材料有限公司 | Refractory brick capable of permeating water and reducing temperature at high temperature and processing technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110041096A (en) * | 2019-01-16 | 2019-07-23 | 深圳陶陶科技有限公司 | Diatomite-based Porous Ceramics and preparation method thereof and system |
| CN110698188A (en) * | 2019-11-29 | 2020-01-17 | 湖北理工学院 | Method for preparing mullite powder from waste diatomite and mullite powder prepared based on method |
| CN111302773A (en) * | 2020-03-26 | 2020-06-19 | 攀枝花学院 | Preparation method of mullite porous ceramic |
| CN113292316A (en) * | 2021-05-10 | 2021-08-24 | 江苏苏嘉集团新材料有限公司 | Refractory brick capable of permeating water and reducing temperature at high temperature and processing technology |
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Application publication date: 20170208 |