CN102659438A - Microporous lightweight mullite refractory aggregate and preparation method thereof - Google Patents
Microporous lightweight mullite refractory aggregate and preparation method thereof Download PDFInfo
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- CN102659438A CN102659438A CN201210173260XA CN201210173260A CN102659438A CN 102659438 A CN102659438 A CN 102659438A CN 201210173260X A CN201210173260X A CN 201210173260XA CN 201210173260 A CN201210173260 A CN 201210173260A CN 102659438 A CN102659438 A CN 102659438A
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Abstract
The invention discloses microporous lightweight mullite refractory aggregate and a preparation method thereof. The preparation method includes using 30-40wt% of silica powder and 60-70wt% of aluminum hydroxide powder as starting materials, adding 2-4wt% of bonder, 0.3-0.6wt% of additive, 20-30wt% of burning-out material and 0.5-2.0wt% of nucleating agent, subjecting the materials to wet co-milling and vacuum press-filtering forming, calcining a blank which is dried, and crushing products of calcining to obtain the microporous lightweight mullite refractory aggregate. The microporous lightweight mullite refractory aggregate has high mullite conversion rate, high size stability, high strength and the like.
Description
Technical field
The present invention relates to the used a kind of refractory aggregate of fire resisting material field, relate in particular to light porous mullite refractory aggregate and preparation method that a kind of lightweight refractory is used.
Background technology
The working efficiency that improves kiln is exactly to adopt lightweight refractory to replace the heavy refractory materials to construct inner lining of kiln with one of important measures that reduce hear rate and alleviate own wt.Require the use temperature of insulating refractory increasingly high.And there is the impurity height in traditional lightweight synthetic material, pore is big, effect of heat insulation is not good enough, use temperature is low, and it is usually less than 1200 ℃; Another kind of is senior insulating refractory, and use temperature is higher than 1500 ℃., but price is high, and intensity is low, is difficult to apply; And Industrial Stoves and the lining body of Thermal Equipment of use temperature between 1200 ℃-1500 ℃ mostly is molded article, has that globality is bad, intensity is low, the high inadequately deficiency of operating efficiency.Therefore it is very necessary at 1200 ℃-1500 ℃ lightweight heat-proof unshape refractory to develop use temperature.Therefore, can develop the raw material that satisfies unshape refractory and become key.Aglite is an important component part of forming the lightweight unshape refractory; Yet it is many that present used aggregate exists introducing impurity, the high volume poor stability; Heat-proof quality and intensity can not be taken into account and wait some shortcomings, thereby can not satisfy the requirement of high-performance light unshape refractory.
Explained among the patent documentation CN201010159664.4 at home and have the light porous aggregate of similar mullite of the present invention, but the present invention has different significantly with it.The raw material that uses is different, and thermal treatment process is different, makes that the transformation efficiency of mullite synthesizing is higher, and aglite unit weight is littler, thereby causes final product performance that completely difference is also arranged.
Summary of the invention
The objective of the invention is deficiency, a kind of purity height, high volume good stability, thermal insulation is good, intensity is high light porous mullite aggregate and preparation method thereof are provided in order to address the above problem.
The technical scheme that the present invention adopts is: a kind of light porous mullite refractory aggregate; Selecting ground silica and white lake for use is starting material; Add wedding agent, additive and burning lost article, a weight percent of expecting is: ground silica 30-40, white lake 60-70%; The per-cent that the add-on that adds wedding agent, additive, burning lost article and nucleus agent accounts for the starting material gross weight is: wedding agent 2-4%, additive be 0.3-0.6%, burn lost article 20-30% and nucleus agent 0.5-2.0%.
Used ground silica in the raw material, dioxide-containing silica is greater than 98%; The content of white lake is greater than 98%; Used wedding agent is a yellow starch gum; Burning lost article is the coke fine powder; Additive is a calcium lignin sulphonate; The nucleus agent is the fused mullite crystal seed.Starting material is put into the levigate mixing of ball mill wet method after broken the pulverizing; Material after mixing is through the vacuum filter mud; Be of a size of 230 * 114 * 65 millimeters base substrate through pug mill and mud extruder formation; Base substrate seasoning after 24 hours at ambient temperature; With base substrate in moisture eliminator under 100-150 ℃ the temperature dry 20-35 hour, then with dried base substrate in the high temperature kiln 1350-1450 ℃ of calcining down, the block mullite after the calcining is just obtained this light porous mullite aggregate through crusher in crushing.
Principle of the present invention is to utilize the nucleus agent to induce the generation of mullite, generates at a lower temperature with the promotion mullite, or higher at equal conditions mullite growing amount.Theoretical according to the physical chemistry nucleus, non-spontaneous nucleation can reduce the energy of reaction, makes that chemical reaction more is prone to carry out.The present invention is exactly in order to reduce the potential barrier of sporadic nucleation in the reaction process; Introduce mullite seed; Make activated alumina and fine silica that the white lake pyrolytic decomposition forms can under relatively low temperature, react rapidly under the effect of mullite seed; Generate a kind of stable in properties, the mullite phase of superior performance.Because after introducing the nucleus agent, under the equal conditions, become anxious gathering of nuclear volume to increase, the therefore final mullite crystal grain that forms is tiny, has lower thermal expansivity, higher thermal shock resistance and excellent high-temperature performance.In addition, to synthetic light porous mullite aggregate, it is fit closely adopting the synthetic light-weight mullite material of white lake and ground silica.White lake is decomposed to form oxide of high activity aluminium, and material decomposes not only can make the material production pore make more lighting of material, and highly active aluminum oxide can improve the transformation efficiency of mullite again.In addition, in the starting material that is adopted, added a certain amount of coke fine powder of burning, thereby can form a large amount of little pores at material internal.According to heat transfer principle, under the certain situation of void content, pore is more little, and thermal conductivity is more little, and intensity is high more simultaneously.Therefore the light porous mullite aggregate of the present invention's preparation has higher mullite production rate, higher intensity, lower thermal conductivity.
The present invention, the preparation method of light porous mullite aggregate is:
Step 1, raw material are prepared, and broken respectively ground silica, white lake, coke, granularity is less than 325 orders.
Step 2; The preparation compound; According to a certain ratio ground silica, white lake, coke fine powder and admixture yellow starch gum, additive calcium lignin sulphonate, nucleus agent mullite are added in the ball mill; Adding accounts for whole material and weighs 100% water in ball mill again, carries out ball milling with zirconia ball as grinding medium, and all materials grind in ball mill and obtained 500-800 purpose mixture slip in 12-24 hour.
Step 3, vacuum filter mud, refining mud and crowded mud become pie with the mixed slurry press filtration in the vacuum mud press, the material cake that filter is good is placed on to be handled in the pug mill, are extruded into through mud extruder then to be of a size of 230 * 114 * 65 millimeters base substrate.
Step 4, seasoning and oven dry, base substrate seasoning after 24 hours at ambient temperature was with base substrate in moisture eliminator under 100-150 ℃ the temperature dry 20-35 hour.
Step 5, calcining and fragmentation are calcined dried base substrate down at 1350-1450 ℃ in the high temperature kiln, and 1100 ℃ of following temperature rise rates are 5 ℃/min, are 3 ℃/min at 1100 ℃ of-1450 ℃ of temperature rise rates, burn to obtain block micro-pore mullite goods after 20-30 hour; Block mullite after the calcining is just obtained this light porous mullite aggregate through crusher in crushing.
Resulting aggregate volume density is between 0.7-1.0g/cm
3Between, void content is at 60-85%; Through diffraction analysis, show that the mullite content in the aggregate is higher than 90%, the inner pore of aggregate mainly is in below 10 microns, concentrates to be distributed in below 2 microns.Through scanning electron microscope analysis, the aggregate internal porosity is evenly distributed.
Useful result of the present invention is: with the like product ratio, internal holes is a micron order, and mullite transformation efficiency height can reach more than 90%, and the mullite aggregate volume density that makes the present invention make is littler, better heat preservation; Because this product is the lightweight solid phase material, inside is mainly a contact, and is insensitive to the solid phase mass transfer, so this product at high temperature shrinks down, and volume stability is good; Mostly the aggregate internal porosity is the globosity of sealing, so the product thermal conductivity coefficient is little, and intensity is high.
Embodiment
Following examples have at length been explained the present invention.
Embodiment 1
The white lake of ground silica and 98% is prepared in the ratio of 34:66, added coke fine powder 25%, yellow starch gum 3%, calcium lignin sulphonate 0.5%, mullite seed 0.5% (being the per-cent that accounts for the starting material gross weight).With the above-mentioned raw materials weighing good after, put into ball mill with grinding medium zirconia ball, water.Three's weight ratio is a raw material: mill ball: water=1:1:1.Drum's speed of rotation is set at 25 rpms.Time consuming is 18 hours altogether.
With carrying out press filtration in the material introducing vacuum mud press that mill is good altogether, the slip after the press filtration drops into after pugging in the mud extruder, extrudes the back cutting and obtains base substrate.Base substrate seasoning after 24 hours at ambient temperature; With base substrate in moisture eliminator under 120 ℃ the temperature dry 20 hours; Dried base substrate is calcined down at 1450 ℃ in the high temperature kiln; 1100 ℃ of following temperature rise rates are 5 ℃/min, are 3 ℃/min at 1100 ℃ of-1450 ℃ of temperature rise rates, and 1450 ℃ are incubated 20 hours.Behind the product kiln discharge, the mullite after the calcining is just obtained this light porous mullite aggregate through crusher in crushing.
Embodiment 2
The white lake of ground silica and 98% is prepared in the ratio of 30:70, added coke fine powder 20%, yellow starch gum 2%, calcium lignin sulphonate 0.6%, mullite seed 1.0% (being the per-cent that accounts for the starting material gross weight).With the above-mentioned raw materials weighing good after, put into ball mill with grinding medium zirconia ball, water.Three's weight ratio is a raw material: mill ball: water=1:1:1.Drum's speed of rotation is set at 25 rpms.Time consuming is 24 hours altogether.
With carrying out press filtration in the material introducing vacuum mud press that mill is good altogether, the slip after the press filtration drops into after pugging in the mud extruder, extrudes the back cutting and obtains base substrate.Base substrate seasoning after 24 hours at ambient temperature; With base substrate in moisture eliminator under 150 ℃ the temperature dry 25 hours; Dried base substrate is calcined down at 1400 ℃ in the high temperature kiln; 1100 ℃ of following temperature rise rates are 5 ℃/min, are 3 ℃/min at 1100 ℃ of-1400 ℃ of temperature rise rates, and 1400 ℃ are incubated 25 hours.Behind the product kiln discharge, the mullite after the calcining is just obtained this light porous mullite aggregate through crusher in crushing.
Embodiment 3
The white lake of ground silica and 98% is prepared in the ratio of 40:60, added coke fine powder 30%, yellow starch gum 4%, calcium lignin sulphonate 0.3%, mullite seed 2.0% (being the per-cent that accounts for the starting material gross weight).With the above-mentioned raw materials weighing good after, put into ball mill with grinding medium zirconia ball, water.Three's weight ratio is a raw material: mill ball: water=1:1:1.Drum's speed of rotation is set at 25 rpms.Time consuming is 24 hours altogether.
With carrying out press filtration in the material introducing vacuum mud press that mill is good altogether, the slip after the press filtration drops into after pugging in the mud extruder, extrudes the back cutting and obtains base substrate.Base substrate seasoning after 24 hours at ambient temperature; With base substrate in moisture eliminator under 150 ℃ the temperature dry 30 hours; Dried base substrate is calcined down at 1350 ℃ in the high temperature kiln; 1100 ℃ of following temperature rise rates are 5 ℃/min, are 3 ℃/min at 1100 ℃ of-1350 ℃ of temperature rise rates, and 1350 ℃ are incubated 30 hours.Behind the product kiln discharge, the mullite after the calcining is just obtained this light porous mullite aggregate through crusher in crushing.
Claims (4)
1. light porous mullite refractory aggregate, it is characterized in that: selecting ground silica and white lake for use is starting material, adds wedding agent, additive, burning lost article and nucleus agent, works a weight percent of expecting to be: ground silica 30-40, white lake 60-70%; The per-cent that the add-on that adds wedding agent, additive, burning lost article and admixture accounts for the starting material gross weight is: wedding agent 2-4%, additive be 0.3-0.6%, burn lost article 20-30% and nucleus agent 0.5-2.0%.
2. a kind of light porous mullite refractory aggregate according to claim 1 is characterized in that: wedding agent is a yellow starch gum, and burning lost article is the coke fine powder, and additive is a calcium lignin sulphonate, and the nucleus agent is a mullite seed.
3. a kind of light porous mullite refractory aggregate according to claim 1 is characterized in that: the dioxide-containing silica in the ground silica is greater than 98%, and the white lake content in the white lake is greater than 98%.
4. the preparation method of light porous mullite refractory aggregate according to claim 1 is characterized in that: step 1, raw material are prepared, and broken respectively ground silica, white lake, coke, granularity is less than 325 orders; Step 2; The preparation compound; According to a certain ratio ground silica, white lake, coke fine powder and admixture yellow starch gum, additive calcium lignin sulphonate, bonder mullite seed are added in the ball mill; Adding accounts for whole material and weighs 100% water in ball mill again, carries out ball milling with zirconia ball as grinding medium, and all materials grind in ball mill and obtained 500-800 purpose mixture slip in 12-24 hour; Step 3, vacuum filter mud, pugging and crowded mud become pie with the mixed slurry press filtration in the vacuum mud press, the material cake that filter is good is placed on to be handled in the pug mill, are extruded into through mud extruder then to be of a size of 230 * 114 * 65 millimeters base substrate; Step 4, seasoning and oven dry, base substrate seasoning after 24 hours at ambient temperature was with base substrate in moisture eliminator under 100-150 ℃ the temperature dry 20-35 hour; Step 5, calcining and fragmentation are calcined dried base substrate down at 1350-1450 ℃ in the high temperature kiln, and 1100 ℃ of following temperature rise rates are 5 ℃/min, are 3 ℃/min at 1100 ℃ of-1450 ℃ of temperature rise rates, burn to obtain block micro-pore mullite goods after 20-30 hour; Mullite after the calcining is just obtained this light porous mullite aggregate through crusher in crushing.
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| CN201210173260XA CN102659438A (en) | 2012-05-30 | 2012-05-30 | Microporous lightweight mullite refractory aggregate and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056310A (en) * | 2017-04-17 | 2017-08-18 | 武汉科技大学 | A kind of high-strength micro-pore mullite refractory aggregate and preparation method thereof |
| CN107954738A (en) * | 2017-11-06 | 2018-04-24 | 宜兴摩根热陶瓷有限公司 | A kind of method that low heat conduction mullite insulating brick is quickly prepared based on foam method |
-
2012
- 2012-05-30 CN CN201210173260XA patent/CN102659438A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 山国强 等: "煅烧制度对合成轻质微孔莫来石骨料性能的影响", 《现代技术陶瓷》 * |
| 山国强: "微孔轻质莫来石合成料性能影响因素的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056310A (en) * | 2017-04-17 | 2017-08-18 | 武汉科技大学 | A kind of high-strength micro-pore mullite refractory aggregate and preparation method thereof |
| CN107954738A (en) * | 2017-11-06 | 2018-04-24 | 宜兴摩根热陶瓷有限公司 | A kind of method that low heat conduction mullite insulating brick is quickly prepared based on foam method |
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Application publication date: 20120912 |