CN104193394B - A kind of preparation method of light aluminum oxide hollow ball insulating product - Google Patents
A kind of preparation method of light aluminum oxide hollow ball insulating product Download PDFInfo
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- CN104193394B CN104193394B CN201410434384.8A CN201410434384A CN104193394B CN 104193394 B CN104193394 B CN 104193394B CN 201410434384 A CN201410434384 A CN 201410434384A CN 104193394 B CN104193394 B CN 104193394B
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Abstract
The present invention relates to a kind of preparation method of light aluminum oxide hollow ball insulating product.Be aggregate with alumina hollow ball, take alumina powder as substrate material, in alumina powder, add water, whipping agent, by mixed foaming, in hollow ball brick substrate material, introduce pore, obtain porous matrix; Utilizing organic monomer and linking agent polymerization reaction take place under initiator and catalyst action in foamed slurry, realize foamed slurry solidification, through leaving standstill, the demoulding, obtaining the base substrate that porous matrix and hollow ball aggregate form; By base substrate through super-dry, sintering, obtain light aluminum oxide hollow ball insulating brick; Low (600-1000 ㎏/the m of hollow ball insulating product density prepared by the present invention
3), the low (0.36-0.83Wm of thermal conductivity
-1k
-1), good heat-insulation effect, accumulation of heat is little, and energy-saving effect is remarkable.
Description
Technical field
The present invention relates to a kind of Preparation Method of light aluminum oxide hollow ball insulating product, belong to light thermal-shield refractory Material Field.
Technical background
The energy-saving and cost-reducing direction having become the current whole society and made joint efforts, uses insulating refractory to be one of energy-saving and cost-reducing important measures of kiln industrial realization.Along with China's rapid economic development, energy starved contradiction, this energy-saving effect to insulating refractory proposes requirements at the higher level.
In numerous light thermal-shield refractory material, alumina hollow ball product has that use temperature is high, fire performance is excellent, thermal shock resistance advantages of higher, is widely used in high temperature kiln work liner.Alumina hollow ball product, usually using alumina hollow ball as aggregate, using aluminum oxide fine powder as matrix, adds appropriate bonding agent, through shaping, dry and burn till and be prepared from.To burn till and the hot environment of working process makes base portion generation nodulizing be densification, which results in higher (the usual 1600 ㎏/m of alumina hollow ball product density
3left and right, 1200oC thermal conductivity 2.0Wm
-1k
-1left and right), by literature search, do not find that density is less than 1000 ㎏/m
3alumina hollow ball product.High-density makes alumina hollow ball product thermal conductivity higher, and accumulation of heat is large, and intensification rate of temperature fall is comparatively slow, causes that high temperature kiln industrial energy consumption is large, production efficiency is low.
Summary of the invention
The present invention overcomes deficiency of the prior art, provides a kind of preparation method of light aluminum oxide hollow ball insulating brick, the hollow ball insulating brick density 600-1000 ㎏/m of preparation
3, thermal conductivity 0.36-0.83Wm
-1k
-1, compared with conventional aluminium oxide hollow ball insulating brick, there is the features such as thermal conductivity is low, accumulation of heat is little, good heat-insulation effect, density are low.
The technical scheme that the present invention completes the employing of invention task is: take alumina hollow ball as aggregate, take alumina powder as substrate material, in alumina powder, add water, whipping agent, pass through mixed foaming, in hollow ball brick substrate material, introduce pore, obtain porous matrix; Utilizing organic monomer and linking agent polymerization reaction take place under initiator and catalyst action in foamed slurry, realize foamed slurry solidification, through leaving standstill, the demoulding, obtaining the base substrate that porous matrix and hollow ball aggregate form; By base substrate through super-dry, sintering, obtain light aluminum oxide hollow ball insulating brick; The light aluminum oxide hollow ball insulating brick density 600-1000 ㎏/m of preparation
3, thermal conductivity 0.36-0.83Wm
-1k
-1.
A kind of preparation method of light aluminum oxide hollow ball insulating brick, with alumina hollow ball and alumina powder for basic raw material, first in alumina powder, water, dispersion agent, organic monomer, linking agent, catalyzer is added, ball milling mixing 0.5-2h, add whipping agent, stir foaming, in matrix, introduce bubble, obtain foamed slurry; Then in foamed slurry, alumina hollow ball is added and initiator is fully mixed to evenly, under initiator and catalyst action, organic monomer and linking agent polymerization reaction take place realize foamed slurry solidification, and leave standstill after 12-24h and carry out the demoulding, obtain the base substrate that porous matrix and hollow ball aggregate form;
Base substrate is put into constant temperature and humidity drying case dry, temperature, humidity control respectively at 40-60oC, 60-90%, and time of drying is 48-96h; Carrying out dry temperature at common loft drier controls at 80-110oC, and time of drying is 36-48h; After drying, base substrate is sintered, described sintering process, with the ramp of 0.5-1oC/min, and be incubated 0.5-1h in 450-650oC; Then with the ramp of 1-3oC/min, and be incubated 3-6h in 1600-1700oC, naturally cool to room temperature.
Described alumina hollow ball, the mass percent of alumina powder are respectively 50-65%, 35-50%, and alumina hollow ball and the equal >98% of alumina powder purity, wherein alumina hollow ball density is 600-800 ㎏/m
3, particle diameter 0.5-3mm, alumina powder granularity <44 μm.
Described water add-on is the 15-20% of alumina powder quality.
Described dispersion agent is the one in Sodium hexametaphosphate 99, polyoxyethylene glycol based polyalcohol FS10, poly carboxylic acid fat based polyalcohol FS20, sodium polyacrylate, and add-on is the 0.5-2% of alumina powder quality.
Described whipping agent is the one in sodium lauryl sulphate, ammonium lauryl sulfate, Sodium dodecylbenzene sulfonate and dodecyltriethanolamine sulfate, and add-on is the 1-2% of alumina powder quality.
Described organic monomer is the one in acrylamide AM, Methacrylamide MAM, and add-on is the 3-10% of alumina powder quality.
Described linking agent is the one in methylene-bisacrylamide MBAM, diallyl tartrate diamide DATDA, and add-on is the 0.5-2% of alumina powder quality.
Described catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine TEMED, add-on is the 0.05-0.3% of alumina powder quality.
Described initiator is the one in ammonium persulphate, Sodium Persulfate, Potassium Persulphate, and add-on is 0.5-5% of alumina powder quality.
The present invention's beneficial effect is compared with prior art as follows:
Being aggregate with alumina hollow ball, take alumina powder as substrate material, adds whipping agent and stirs foaming, in matrix, introduce pore, and final to obtain density be 600-1000 ㎏/m
3alumina hollow ball insulation product;
The present invention utilizes organic monomer and linking agent polymerization reaction take place under initiator and catalyst action in foamed slurry, realizes slurry curing, obtains the base substrate that porous matrix and hollow ball aggregate form.
Alumina hollow ball insulating brick prepared by the present invention compared with conventional aluminium oxide hollow ball insulating brick, the low (600-1000 ㎏/m of density
3), the low (0.36-0.83Wm of thermal conductivity
-1k
-1), good heat-insulation effect, accumulation of heat be little, as the inner lining material of high temperature kiln, at high temperature life-time service, realize hot industry and save energy and reduce the cost.
Embodiment
Alumina hollow ball and the equal >98% of alumina powder purity, wherein alumina hollow ball particle diameter 0.5-3mm in the embodiment provided, alumina powder granularity <44 μm; For avoiding repetition, be not repeated in following examples.
Embodiment 1
By 5000g alumina powder, 750g water, 100g Sodium hexametaphosphate 99,250g acrylamide AM50g methylene-bisacrylamide MBAM, 2.5gN, N, N ', N '-Tetramethyl Ethylene Diamine TEMED puts into ball grinder, with the rotating speed planetary ball mill 0.5h of 20r/min, obtains slurry; Then in slurry, add 50g sodium lauryl sulphate, stir foaming, obtain foamed slurry, add 5000g alumina hollow ball and 50g ammonium persulphate in the most backward foamed slurry and be stirred to evenly and inject mould, leave standstill 12h, the demoulding.Base substrate after the demoulding is placed in constant temperature constant humidity baking oven, and temperature humidity is respectively 40oC and 60%, dry 60h, then proceeds to dry 48h in the common loft drier of 80oC.Base substrate after oven dry rises to 450oC with the temperature rise rate of 1oC/min and is incubated 0.5h, and then rise to 1600oC with the temperature rise rate of 1oC/min and be incubated 6h, obtaining alumina hollow ball insulation product, its density is 1000 ㎏/m
3, 1200oC thermal conductivity is 0.83Wm
-1k
-1.
Embodiment 2
By 4500g alumina powder, 765g water, 67.5g polyoxyethylene glycol based polyalcohol FS10,135g Methacrylamide MAM, 22.5g diallyl tartrate diamide DATDA, 6.75gN, N, N ', N '-Tetramethyl Ethylene Diamine TEMED puts into ball grinder, with the rotating speed planetary ball mill 1h of 40r/min, obtain slurry; Then in slurry, add 67.5g ammonium lauryl sulfate, stir foaming, obtain foamed slurry, add 5500g alumina hollow ball and 22.5g Potassium Persulphate in the most backward foamed slurry and be stirred to evenly and inject mould, leave standstill 16h, the demoulding.Base substrate after the demoulding is placed in constant temperature constant humidity baking oven, and temperature humidity is respectively 55oC and 70%, dry 80h, then proceeds to dry 36h in the common loft drier of 90oC.Base substrate after oven dry rises to 600oC with the temperature rise rate of 2oC/min and is incubated 1h, and then rise to 1700oC with the temperature rise rate of 2oC/min and be incubated 3h, obtaining alumina hollow ball insulation product, its density is 900 ㎏/m
3, 1200oC thermal conductivity is 0.75Wm
-1k
-1.
Embodiment 3
By 4000g alumina powder, 720g water, 40g poly carboxylic acid fat based polyalcohol FS20,280g acrylamide AM, 60g diallyl tartrate diamide DATDA, 4gN, N, N ', N '-Tetramethyl Ethylene Diamine TEMED, puts into ball grinder, with the rotating speed planetary ball mill 1.5h of 30r/min, obtains slurry; Then in slurry, add 72g Sodium dodecylbenzene sulfonate, stir foaming, obtain foamed slurry, the most backward foamed slurry adds 6000g alumina hollow ball and 120g Sodium Persulfate and is stirred to evenly and injects mould, leaves standstill 18h, the demoulding.Base substrate after the demoulding is placed in constant temperature constant humidity baking oven, and temperature humidity is respectively 50oC and 80%, dry 96h, then proceeds to dry 40h in the common loft drier of 100oC.Base substrate after oven dry rises to 650oC with the temperature rise rate of 1.5oC/min and is incubated 0.8h, and then rise to 1680oC with the temperature rise rate of 1.5oC/min and be incubated 5h, obtaining alumina hollow ball insulation product, its density is 800 ㎏/m
3, 1200oC thermal conductivity is 0.57Wm
-1k
-1.
Embodiment 4
By 3500g alumina powder, 700g water, 17.5g sodium polyacrylate, 350g Methacrylamide MAM, 70g methylene-bisacrylamide MBAM, 10.5gN, N, N ', N '-Tetramethyl Ethylene Diamine TEMED, puts into ball grinder, with the rotating speed planetary ball mill 2h of 50r/min, obtains slurry; Then in slurry, add 70g dodecyltriethanolamine sulfate, stir foaming, obtain foamed slurry, add 6500g alumina hollow ball and 175g Potassium Persulphate in the most backward foamed slurry and be stirred to evenly and inject mould, leave standstill 24h, the demoulding.Base substrate after the demoulding is placed in constant temperature constant humidity baking oven, and temperature humidity is respectively 60oC and 90%, dry 48h, then proceeds to dry 45h in the common loft drier of 110oC.Base substrate after oven dry rises to 500oC with the temperature rise rate of 0.5oC/min and is incubated 0.5h, and then rise to 1650oC with the temperature rise rate of 3oC/min and be incubated 3h, obtaining alumina hollow ball insulation product, its density is 600 ㎏/m
3, 1200oC thermal conductivity is 0.36Wm
-1k
-1.
Claims (8)
1. the preparation method of a light aluminum oxide hollow ball insulating brick, it is characterized in that: with alumina hollow ball and alumina powder for basic raw material, first in alumina powder, water, dispersion agent, organic monomer, linking agent, catalyzer is added, ball milling mixing 0.5-2h, add whipping agent, stir foaming, in matrix, introduce bubble, obtain foamed slurry; Then in foamed slurry, alumina hollow ball is added and initiator is fully mixed to evenly, under initiator and catalyst action, organic monomer and linking agent polymerization reaction take place realize foamed slurry solidification, and leave standstill after 12-24h and carry out the demoulding, obtain the base substrate that porous matrix and hollow ball aggregate form;
Base substrate is put into constant temperature and humidity drying case dry, temperature, humidity control respectively at 40-60oC, 60-90%, and time of drying is 48-96h; Carrying out dry temperature at common loft drier controls at 80-110oC, and time of drying is 36-48h; After drying, base substrate is sintered, described sintering process, with the ramp of 0.5-1oC/min, and be incubated 0.5-1h in 450-650oC; Then with the ramp of 1-3oC/min, and be incubated 3-6h in 1600-1700oC, naturally cool to room temperature;
The light aluminum oxide hollow ball insulating brick density 600-1000 ㎏/m of preparation
3, thermal conductivity 0.36-0.83Wm
-1k
-1; Described alumina hollow ball, the mass percent of alumina powder are respectively 50-65%, 35-50%, and alumina hollow ball and the equal >98% of alumina powder purity, wherein alumina hollow ball density is 600-800 ㎏/m
3, particle diameter 0.5-3mm, alumina powder granularity <44 μm.
2. the preparation method of a kind of light aluminum oxide hollow ball insulating brick as claimed in claim 1, is characterized in that the add-on of described water is the 15-20% of alumina powder quality.
3. the preparation method of a kind of light aluminum oxide hollow ball insulating brick as claimed in claim 1, it is characterized in that described dispersion agent is the one in Sodium hexametaphosphate 99, polyoxyethylene glycol based polyalcohol FS10, poly carboxylic acid fat based polyalcohol FS20, sodium polyacrylate, add-on is the 0.5-2% of alumina powder quality.
4. the preparation method of a kind of light aluminum oxide hollow ball insulating brick as claimed in claim 1, it is characterized in that described whipping agent is the one in sodium lauryl sulphate, ammonium lauryl sulfate, Sodium dodecylbenzene sulfonate and dodecyltriethanolamine sulfate, add-on is the 1-2% of alumina powder quality.
5. the preparation method of a kind of light aluminum oxide hollow ball insulating brick as claimed in claim 1, it is characterized in that described organic monomer is the one in acrylamide AM, Methacrylamide MAM, add-on is the 3-10% of alumina powder quality.
6. the preparation method of a kind of light aluminum oxide hollow ball insulating brick as claimed in claim 1, it is characterized in that described linking agent is the one in methylene-bisacrylamide MBAM, diallyl tartrate diamide DATDA, add-on is the 0.5-2% of alumina powder quality.
7. the preparation method of a kind of light aluminum oxide hollow ball insulating brick as claimed in claim 1, is characterized in that described catalyzer is N, N, N ', N '-Tetramethyl Ethylene Diamine TEMED, add-on is the 0.05-0.3% of alumina powder quality.
8. the preparation method of a kind of light aluminum oxide hollow ball insulating brick as claimed in claim 1, it is characterized in that described initiator is the one in ammonium persulphate, Sodium Persulfate, Potassium Persulphate, add-on is 0.5-5% of alumina powder quality.
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| CN105503216B (en) * | 2015-12-24 | 2019-04-12 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of preparation method of high-strength light alumina hollow ball product |
| CN107805081A (en) * | 2017-10-31 | 2018-03-16 | 湖南镭目科技有限公司 | A kind of porous ceramics and preparation method thereof |
| CN108675809A (en) * | 2018-07-02 | 2018-10-19 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of Ultralight corundum castable and preparation method thereof |
| CN109095948B (en) * | 2018-08-06 | 2020-08-25 | 清华大学 | Method for preparing foamed ceramic with communicated pore walls by using hollow microspheres |
| CN110436959A (en) * | 2019-07-31 | 2019-11-12 | 辽宁科技大学 | A kind of magnesium aluminate spinel whisker reinforcement alumina hollow ball porous ceramics |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173852A (en) * | 2011-01-29 | 2011-09-07 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique |
| CN102491761A (en) * | 2011-11-16 | 2012-06-13 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of hollow alumina ball thermal insulation refractory material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102173852A (en) * | 2011-01-29 | 2011-09-07 | 中钢集团洛阳耐火材料研究院有限公司 | Method for preparing alumina porous ceramics by emulsion/gel-combined die casting technique |
| CN102491761A (en) * | 2011-11-16 | 2012-06-13 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of hollow alumina ball thermal insulation refractory material |
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