CN104193394A - Method for preparing lightweight alumina hollow sphere heat insulation product - Google Patents

Method for preparing lightweight alumina hollow sphere heat insulation product Download PDF

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Publication number
CN104193394A
CN104193394A CN201410434384.8A CN201410434384A CN104193394A CN 104193394 A CN104193394 A CN 104193394A CN 201410434384 A CN201410434384 A CN 201410434384A CN 104193394 A CN104193394 A CN 104193394A
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hollow ball
alumina
alumina hollow
add
lightweight
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CN201410434384.8A
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CN104193394B (en
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陈阔
袁波
王刚
韩建燊
董宾宾
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

The invention relates to a method for preparing a lightweight alumina hollow sphere heat insulation product. The method comprises the following steps: by taking an alumina hollow sphere as aggregate and alumina micro powder as a matrix, adding water and a foaming agent into the alumina micro powder, mixing and foaming, introducing pores into the hollow sphere brick matrix, thereby obtaining a porous matrix; carrying out a polymerization reaction between an organic monomer and a crosslinking agent in a foaming slurry under the actions of an initiator and a catalyst, curing the foaming slurry, standing and demolding, thereby obtaining a blank consisting of the porous matrix and the hollow sphere aggregate; and drying and sintering the blank, thereby obtaining the lightweight alumina hollow sphere heat insulation brick. The hollow sphere heat insulation product prepared by the invention has low density of 600-1000kg/mg<3> and low heat conductivity of 0.36-0.83W.m<-1>.K<-1> and is good in heat insulation effect, low in heat storage and obvious in energy-saving effect.

Description

A kind of preparation method of lightweight alumina hollow ball insulation product
Technical field
The present invention relates to a kind of Preparation Method of lightweight alumina hollow ball insulation product, belong to light thermal-shield refractory Material Field.
Technical background
The energy-saving and cost-reducing direction that has become the joint efforts of the current whole society, using insulating refractory is 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 materials, alumina hollow ball product has that use temperature is high, fire performance is good, thermal shock resistance advantages of higher, is widely used in high temperature kiln work liner.Alumina hollow ball product is usingd alumina hollow ball conventionally as aggregate, usings aluminum oxide fine powder as matrix, adds appropriate bonding agent, through moulding, dry and burn till and be prepared from.Burn till and the hot environment of working process makes matrix that nodulizing partly occur to be densification, this has caused higher (the common 1600 ㎏/m of alumina hollow ball product density 3left and right, 1200 oC thermal conductivity 2.0 Wm -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 slower, 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, and a kind of preparation method of lightweight alumina hollow ball insulating brick is provided, the hollow ball insulating brick density 600-1000 ㎏/m of preparation 3, thermal conductivity 0.36-0.83Wm -1k -1, compare with conventional aluminium oxide hollow ball insulating brick, have that thermal conductivity is low, accumulation of heat is little, a feature such as 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; Utilize organic monomer and linking agent polymerization reaction take place under initiator and catalyst action in foamed slurry, realize foamed slurry and solidify, through standing, the demoulding, obtain the base substrate that porous matrix and hollow ball aggregate form; Base substrate, through super-dry, sintering, is obtained to lightweight alumina hollow ball insulating brick; The lightweight alumina 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 lightweight alumina hollow ball insulating brick, take alumina hollow ball and alumina powder as basic raw material, first in alumina powder, add water, dispersion agent, organic monomer, linking agent, catalyzer, ball milling mixing 0.5-2h, add whipping agent, stir foaming, in matrix, introduce bubble, obtain foamed slurry; Then in foamed slurry, add alumina hollow ball and initiator to be fully mixed to evenly, under initiator and catalyst action, organic monomer and linking agent polymerization reaction take place are realized foamed slurry and are solidified, and after standing 12-24h, 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 are controlled at respectively 40-60oC, 60-90%, and be 48-96h time of drying; At common loft drier, carry out dry temperature and be controlled at 80-110oC, be 36-48h time of drying; After dry, base substrate is carried out to sintering, described sintering process, with the speed intensification of 0.5-1oC/min, and in 450-650oC insulation 0.5-1h; Then the speed with 1-3oC/min heats up, and in 1600-1700oC insulation 3-6h, naturally cools to room temperature.
Described alumina hollow ball, the mass percent of alumina powder are respectively 50-65%, 35-50%, alumina hollow ball and the equal >98% of alumina powder purity, and wherein alumina hollow ball density is 600-800 ㎏/m 3, particle diameter 0.5-3mm, alumina powder granularity <44 μ m.
Described water add-on is the 15-20% of alumina powder quality.
Described dispersion agent is a kind of 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 a kind of 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 a kind of in acrylamide AM, Methacrylamide MAM, and add-on is the 3-10% of alumina powder quality.
Described linking agent is a kind of 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, and N ', N '-Tetramethyl Ethylene Diamine TEMED, add-on is the 0.05-0.3% of alumina powder quality.
Described initiator is a kind of 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:
Take alumina hollow ball as aggregate, take alumina powder as substrate material, add whipping agent and stir foaming, in matrix, introduce pore, finally obtaining density is 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.
The prepared alumina hollow ball insulating brick of the present invention is 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, realizes hot industry energy-saving and cost-reducing.
Embodiment
Alumina hollow ball and the equal >98% of alumina powder purity in the embodiment providing, alumina hollow ball particle diameter 0.5-3mm wherein, alumina powder granularity <44 μ m; For avoiding repetition, in following examples, be not repeated.
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, and the rotating speed planetary ball mill 0.5h with 20r/min, obtains slurry; Then in slurry, add 50g sodium lauryl sulphate, stir foaming, obtain foamed slurry, in the most backward foamed slurry, add 5000g alumina hollow ball and 50g ammonium persulphate to be stirred to evenly rear injection mould, standing 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%, and then dry 60h proceeds to dry 48h in the common loft drier of 80oC.Base substrate after oven dry rises to 450oC insulation 0.5h with the temperature rise rate of 1oC/min, and then the temperature rise rate with 1oC/min rises to 1600oC and is incubated 6h, obtains alumina hollow ball insulation product, and its density is 1000 ㎏/m 3, 1200oC thermal conductivity is 0.83 Wm -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, rotating speed planetary ball mill 1h with 40r/min, obtains slurry; Then in slurry, add 67.5g ammonium lauryl sulfate, stir foaming, obtain foamed slurry, in the most backward foamed slurry, add 5500g alumina hollow ball and 22.5g Potassium Persulphate to be stirred to evenly rear injection mould, standing 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%, and then dry 80h proceeds to dry 36h in the common loft drier of 90oC.Base substrate after oven dry rises to 600oC insulation 1h with the temperature rise rate of 2oC/min, and then the temperature rise rate with 2oC/min rises to 1700oC and is incubated 3h, obtains alumina hollow ball insulation product, and 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, 60 g diallyl tartrate diamide DATDA, 4gN, N, N ', N '-Tetramethyl Ethylene Diamine TEMED, puts into ball grinder, and the rotating speed planetary ball mill 1.5h with 30r/min, obtains slurry; Then in slurry, add 72g Sodium dodecylbenzene sulfonate, stir foaming, obtain foamed slurry, the most backward foamed slurry injects mould, standing 18h, the demoulding after adding 6000g alumina hollow ball and 120g Sodium Persulfate to be stirred to evenly.Base substrate after the demoulding is placed in constant temperature constant humidity baking oven, and temperature humidity is respectively 50oC and 80%, and then dry 96h proceeds to dry 40h in the common loft drier of 100oC.Base substrate after oven dry rises to 650oC insulation 0.8h with the temperature rise rate of 1.5oC/min, and then the temperature rise rate with 1.5oC/min rises to 1680oC and is incubated 5h, obtains alumina hollow ball insulation product, and its density is 800 ㎏/m 3, 1200oC thermal conductivity is 0.57 Wm -1k -1.
Embodiment 4
By 3500g alumina powder, 700 g 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, and the rotating speed planetary ball mill 2h with 50r/min, obtains slurry; Then in slurry, add 70g dodecyltriethanolamine sulfate, stir foaming, obtain foamed slurry, in the most backward foamed slurry, add 6500g alumina hollow ball and 175g Potassium Persulphate to be stirred to evenly rear injection mould, standing 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%, and then dry 48h proceeds to dry 45h in the common loft drier of 110oC.Base substrate after oven dry rises to 500oC insulation 0.5h with the temperature rise rate of 0.5oC/min, and then the temperature rise rate with 3oC/min rises to 1650oC and is incubated 3h, obtains alumina hollow ball insulation product, and its density is 600 ㎏/m 3, 1200oC thermal conductivity is 0.36 Wm -1k -1.

Claims (10)

1. a preparation method for lightweight alumina hollow ball insulation product, is characterized in that: take alumina hollow ball as aggregate, 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; Utilize organic monomer and linking agent polymerization reaction take place under initiator and catalyst action in foamed slurry, realize foamed slurry and solidify, through standing, the demoulding, obtain the base substrate that porous matrix and hollow ball aggregate form; Base substrate, through super-dry, sintering, is obtained to lightweight alumina hollow ball insulating brick; The lightweight alumina hollow ball insulating brick density 600-1000 ㎏/m of preparation 3, thermal conductivity 0.36-0.83Wm -1k -1.
2. the preparation method of a kind of lightweight alumina hollow ball insulating brick as claimed in claim 1, it is characterized in that: take alumina hollow ball and alumina powder as basic raw material, first in alumina powder, add water, dispersion agent, organic monomer, linking agent, catalyzer, ball milling mixing 0.5-2h, add whipping agent, stir foaming, in matrix, introduce bubble, obtain foamed slurry; Then in foamed slurry, add alumina hollow ball and initiator to be fully mixed to evenly, under initiator and catalyst action, organic monomer and linking agent polymerization reaction take place are realized foamed slurry and are solidified, and after standing 12-24h, 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 are controlled at respectively 40-60oC, 60-90%, and be 48-96h time of drying; At common loft drier, carry out dry temperature and be controlled at 80-110oC, be 36-48h time of drying; After dry, base substrate is carried out to sintering, described sintering process, with the speed intensification of 0.5-1oC/min, and in 450-650oC insulation 0.5-1h; Then the speed with 1-3oC/min heats up, and in 1600-1700oC insulation 3-6h, naturally cools to room temperature.
3. the preparation method of a kind of lightweight alumina hollow ball insulation product as claimed in claim 1 or 2, it is characterized in that described alumina hollow ball, the mass percent of alumina powder are respectively 50-65%, 35-50%, 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 μ m.
4. the preparation method of a kind of lightweight alumina hollow ball insulation product as claimed in claim 1 or 2, is characterized in that described water add-on is the 15-20% of alumina powder quality.
5. the preparation method of a kind of lightweight alumina hollow ball insulation product as claimed in claim 1 or 2, it is characterized in that described dispersion agent is a kind of 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.
6. the preparation method of a kind of lightweight alumina hollow ball insulation product as claimed in claim 1 or 2, it is characterized in that described whipping agent is a kind of in sodium lauryl sulphate, ammonium lauryl sulfate, Sodium dodecylbenzene sulfonate and dodecyltriethanolamine sulfate, add-on is the 1-2% of alumina powder quality.
7. the preparation method of a kind of lightweight alumina hollow ball insulation product as claimed in claim 1 or 2, is characterized in that described organic monomer is a kind of in acrylamide AM, Methacrylamide MAM, and add-on is the 3-10% of alumina powder quality.
8. the preparation method of a kind of lightweight alumina hollow ball insulation product as claimed in claim 1 or 2, it is characterized in that described linking agent is a kind of in methylene-bisacrylamide MBAM, diallyl tartrate diamide DATDA, add-on is the 0.5-2% of alumina powder quality.
9. the preparation method of a kind of lightweight alumina hollow ball insulation product as claimed in claim 1 or 2, is characterized in that described catalyzer is N, N, and N ', N '-Tetramethyl Ethylene Diamine TEMED, add-on is the 0.05-0.3% of alumina powder quality.
10. the preparation method of a kind of lightweight alumina hollow ball insulation product as claimed in claim 1 or 2, is characterized in that described initiator is a kind of in ammonium persulphate, Sodium Persulfate, Potassium Persulphate, and add-on is 0.5-5% of alumina powder quality.
CN201410434384.8A 2014-08-29 2014-08-29 A kind of preparation method of light aluminum oxide hollow ball insulating product Active CN104193394B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105503216A (en) * 2015-12-24 2016-04-20 中钢集团洛阳耐火材料研究院有限公司 Preparation method of light and high-strength alumina bubble 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
CN109095948A (en) * 2018-08-06 2018-12-28 清华大学 A method of there is connection hole wall foamed ceramics using hollow microsphere preparation
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

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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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105503216A (en) * 2015-12-24 2016-04-20 中钢集团洛阳耐火材料研究院有限公司 Preparation method of light and high-strength alumina bubble product
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
CN109095948A (en) * 2018-08-06 2018-12-28 清华大学 A method of there is connection hole wall foamed ceramics using hollow microsphere preparation
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

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