CN102838379B - Lightweight foamed ceramics and preparation method thereof - Google Patents
Lightweight foamed ceramics and preparation method thereof Download PDFInfo
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Abstract
The invention relates to lightweight foamed ceramics and a preparation method of the lightweight foamed ceramics. The lightweight foamed ceramics are prepared by the steps as follows: mechanically agitating raw material, curing agent and foam based on a certain ratio, so as to obtain uniform ceramic size; moulding the ceramic size by casting; and curing and drying same at a certain temperature; and finally sintering the dried blank body to obtain the lightweight foamed ceramics. The lightweight foamed ceramics are important for efficiently utilizing the solid waste, reducing the pollution of the industrial solid waste to the environment, and reducing the production cost; the produced lightweight ceramics have the advantages of being more in closed air pores, relatively low in heat conductivity, relatively high in strength, and relatively low in sintering temperature; and the lightweight foamed ceramics are suitable to be applied to the fields of lightweight decorative material, building insulation wall material, sound insulating material, fireproof material and sinking preventing material.
Description
Technical field
The invention belongs to solid waste and utilize technical field, relate to a kind of light floamed ceramic, be specifically related to a kind of light floamed ceramic and preparation method thereof.
Background technology
China's phosphate rock resource is quite abundant, and reserves are only second to Morocco, occupies the 2nd, the world, and eight large phosphorus ores mainly are distributed in the provinces such as Hubei, Hunan, Sichuan, Jiangsu, Guizhou, Yunnan, but 80% is mid low grade phosphate rock stone.The solid waste of failing to be taken full advantage of of discharging when the phosphorus mine tailing is the phosphate rock floating concentrate.In recent years, along with the fast development of phosphorus chemical industry, and the grade of China's Rock Phosphate (72Min BPL) raw ore is not high, causes a large amount of phosphorus mine tailing of the annual generation of phosphorus chemical industry.The phosphorus mine tailing generally is fine sand shape natural shape and is deposited in Tailings Dam, not only expends fund, takies a large amount of soils, but also bring many environmental problems and safety problem.
At present, the utilization ratio of phosphorus mine tailing is also very low, and its comprehensive Utilization Ways mainly contains new medicament flotation again, recrystallization flotation again, prepares cement, prepares building brick, prepares devitrified glass, prepares phosphorus fertiliser containing magnesium etc.
In publication number CN1837129A patent, its method of processing the phosphorus mine tailing is: " in the phosphorus mine tailing, add ground silica, coke powder (or colliery powder), kaolin powder to mix by a certain percentage; to add water; old; with vacuum-extruder or the moulding of brick pressing machine production line; after oven dry, soak glaze, kiln loading vehicle enters tunnel furnace.Through preheating, after heating up, obtain phosphorous vapor and carbon monoxide, then absorb and obtain strong phosphoric acid through hydrated tower, fragment of brick after heat exchange is cooling as the heavy-load bearing brick product." this invention in to equipment requirements high and complex procedures, the temperature of reaction is higher (1280 ℃ ~ 1450 ℃) also.
In publication number CN1055724A patent, its method of processing the phosphorus mine tailing is: " using other mine tailings of phosphor tail slag or proximate component as main raw material; be aided with extra large sand, flyash or feldspar; add in right amount micro-nucleating agent, through preparing burden, found, moulding, annealing, coring, crystallization and the operations such as grinding, polishing make the method for marbled glass-ceramic again." sintering temperature high (1300 ℃ ~ 1450 ℃) in this invention, soaking time is long, and (10 ~ 16h), energy consumption is large, and adopts the Calcium Fluoride (Fluorspan) that is easy to etching apparatus to make raw material, is not easy to produce.
Summary of the invention
Technical problem to be solved by this invention is: a kind of light floamed ceramic and preparation method thereof is provided, and the density of gained foamed ceramics is low, and thermal conductivity is low, and ultimate compression strength is high; Realized the comprehensive utilization of phosphorus resource of tailings, turned waste into wealth.
The present invention solves its technical problem and adopts following technical scheme:
Light floamed ceramic provided by the invention, by this mass percent, this light floamed ceramic mainly is comprised of raw material 77～90%, solidifying agent 0.5～3%, foam 9.5～20%, wherein:
(1) raw material are comprised of the raw material of following mass percent: phosphorus mine tailing 10～30%, mud 5～10%, feldspar 10～14%, shale 4 ~ 10%, kaolin 3 ~ 7%, yellow ground 5～12%, dispersion agent 0.2～1%, water surplus; Wherein, dispersion agent is a kind of or two or more in Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, Sodium salts humic acids, Weibull sodium, sodium alginate;
(2) solidifying agent is a kind of or two or more in starch, gelatin, Sudan Gum-arabic, silicon sol, water glass, PVA solution;
(3) foam is that tensio-active agent 2～20%, suds-stabilizing agent 0.1～1.5% and water surplus form by mass percent; Described tensio-active agent is a kind of or two or more in sodium laurylsulfonate, rosined soap, Sodium dodecylbenzene sulfonate, tween; Described suds-stabilizing agent is a kind of or two or more in Xylo-Mucine, polyacrylamide, sodium lauryl sulphate.
Described raw material can be comprised of the raw material of following mass percent: phosphorus mine tailing 20%, mud 8%, feldspar 12%, shale 7%, kaolin 5%, yellow ground 7%, water 40.4%, dispersion agent 0.6%.
The mass ratio of described foam and raw material can be 1:5～10.
Described tween can be tween 20, Tween-40, Tween-60, tween-80.
The preparation method of light floamed ceramic provided by the invention, its step comprises:
(1) preparation of raw material:
Phosphorus mine tailing, mud, feldspar, shale, kaolin, yellow ground, water and dispersion agent are mixed in proportion, with light-duty ball mill ball milling, mix 12～18h, the mass percent of each component is: phosphorus mine tailing 10～30%, mud 5～10%, feldspar 10～14%, shale 4 ~ 10%, kaolin 3 ~ 7%, yellow ground 5～12%, dispersion agent 0.2～1%, water surplus;
(2) preparation of foam:
By mass percentage, tensio-active agent 2～20%, suds-stabilizing agent 0.1～1.5% and water surplus are placed in to container, mechanical rapid stirring 5～20min obtains foam; Described tensio-active agent is a kind of or two or more in sodium laurylsulfonate, rosined soap, Sodium dodecylbenzene sulfonate, tween; Described suds-stabilizing agent is a kind of or two or more in Xylo-Mucine, polyacrylamide, sodium lauryl sulphate;
(3) preparation of ceramic size:
By step (1) gained raw material and solidifying agent, step (2) gained foam, according to mass percent, be raw material 77～90%, solidifying agent 0.5～3%, foam 9.5～20% meterings, first in raw material, add solidifying agent, mechanical stirring 10～60min, add again foam, mechanical stirring 10～30min, obtain ceramic size;
(4) moulding of base substrate:
Step (3) gained ceramic size is cast in mould, is placed in the curing drying of 60～90 ℃ of environment and obtains base substrate;
(5) sintering:
Step (4) gained base substrate is put into to sintering oven, then from room temperature, with 2～10 ℃/min, be warmed up to 1060 ℃ ~ 1200 ℃, sintering 0.5 ~ 2h, obtain light floamed ceramic after cooling.
In above-mentioned steps (3), the solidification value after ceramic size is cast in mould can be 65～85 ℃.
In above-mentioned steps (5), the temperature rise rate during sintering is 4～8 ℃/min, and sintering temperature is 1100 ℃ ~ 1150 ℃, and sintering time is 0.5 ~ 1h.
In above-mentioned steps (1), described raw material can be comprised of the raw material of following mass percent: phosphorus mine tailing 20%, mud 8%, feldspar 12%, shale 7%, kaolin 5%, yellow ground 8%, water 39.4%, dispersion agent 0.6%.
In above-mentioned preparation method, the mass ratio of described foam and raw material can be 1:5～10.
In above-mentioned preparation method, described tween can be tween 20, Tween-40, Tween-60.
Principle of the present invention: utilize foam, make ceramic size vesicular structure that is solidified to form due to solidifying agent when certain temperature.The phosphorus mine tailing provides necessary component, strengthens the intensity after base substrate burns till, and feldspar provides necessary component, as solubility promoter, reduces the sintering temperature of base substrate, and the shale sintering temperature is low, and kaolin provides necessary component, and yellow ground provides SiO
2Increase the intensity of burning till rear base substrate, base substrate burns till at 1050 ℃ ~ 1200 ℃.
The advantage that the present invention compared with prior art has is mainly: the utilization ratio of phosphorus mine tailing high (reaching 50%), utilize simultaneously waste mud, and economize on resources, be conducive to environmental protection; The controllability of products obtained therefrom is good, can control according to different demands pore size, the density of product, easily reprocessing; This material produce has that firing temperature is low, and the cycle is short, cost low (raw material cheapness), the advantages such as thermal conductivity low (<0.080W/ (mK)), intensity high (can reach 14.69MPa).
The accompanying drawing explanation
Fig. 1 is the sample SEM figure that adds 14% foam.
Fig. 2 is the sample SEM figure that adds 20% foam.
Embodiment
The present invention will be further described in detail below in conjunction with embodiment.
Embodiment 1:
Get phosphorus mine tailing 20g, mud 8g, feldspar 12g, shale 7g, kaolin 5g, yellow ground 7g, water 40.4g, tripoly phosphate sodium STPP 0.6g put into light-duty ball mill ball milling mixing 15h, the raw material that obtain mixing; Get rosined soap 4g, sodium laurylsulfonate 7g, Xylo-Mucine 0.8g, water 80g, be placed in the mechanical rapid stirring 15min of container and obtain foam; In raw material, add the 25.9g foam, mechanical stirring 10min, then add 3.9g starch, and continue to stir 20min, obtain ceramic size; By the ceramic size casting, be placed in the curing drying of 90 ℃ of baking ovens and obtain base substrate; Base substrate is put into to sintering oven, then from room temperature, with 6 ℃/min, be warmed up to 1150 ℃, sintering 1h, obtain light floamed ceramic after cooling.
Through Archimedes's drainage, survey density, rebound method test ultimate compression strength, the test of flat band method test thermal conductivity method, light floamed ceramic density is 0.256g/cm
3, ultimate compression strength is 11.98MPa, thermal conductivity is 0.069W/ (mK).
Embodiment 2:
Get phosphorus mine tailing 30g, mud 5g, feldspar 11g, shale 4g, kaolin 3g, yellow ground 6.4g, water 40g, Sodium hexametaphosphate 99 0.6g ball milling mixing 18h, the raw material that obtain mixing; Get rosined soap 5g, sodium laurylsulfonate 4g, polyacrylamide 0.1g, water 86g, be placed in the mechanical rapid stirring 20min of container and obtain foam; In raw material, add the 10.6g foam, mechanical stirring 20min, then add the 0.6g Sudan Gum-arabic, and continue to stir 10min, obtain ceramic size; By the ceramic size casting, be placed in the curing drying of 75 ℃ of baking ovens and obtain base substrate; Base substrate is put into to sintering oven, then from room temperature, with 2 ℃/min, be warmed up to 1130 ℃, sintering 1.5h, obtain light floamed ceramic after cooling.
Testing method is with embodiment 1, and light floamed ceramic density is 0.264g/cm
3, ultimate compression strength is 13.08MPa, thermal conductivity is 0.073W/ (mK).
Embodiment 3:
Get phosphorus mine tailing 20g, mud 7.5g, feldspar 14g, shale 6g, kaolin 7g, yellow ground 5.3g, water 40g, Sodium salts humic acids 0.2g ball milling mixing 12h, the raw material that obtain mixing; Get tween 3g, dodecyl to sodium sulfonate 3g, polyacrylamide 0.3g, water 90g, be placed in the mechanical rapid stirring 12.5min of container and obtain foam; In raw material, add the 18g foam, mechanical stirring 25min, then add the 2g gelatin, and continue to stir 35min, obtain ceramic size; By the ceramic size casting, be placed in the curing drying of 70 ℃ of baking ovens and obtain base substrate; Base substrate is put into to sintering oven, then from room temperature, with 5 ℃/min, be warmed up to 1060 ℃, sintering 0.5h, obtain light floamed ceramic after cooling.
Testing method is with embodiment 1, and light floamed ceramic density is 0.263g/cm
3, ultimate compression strength is 12.64MPa, thermal conductivity is 0.071W/ (mK).
Embodiment 4:
Get phosphorus mine tailing 10g, mud 10g, feldspar 13g, shale 10g, kaolin 4g, yellow ground 5g, water 47.5g, Weibull sodium 0.5g ball milling mixing 14h, the raw material that obtain mixing; Get rosined soap 4g, sodium laurylsulfonate 16g, sodium lauryl sulphate 1.5g, water 95g, be placed in the mechanical rapid stirring 5min of container and obtain foam; In raw material, add the 20g foam, mechanical stirring 30min, then add the 3g silicon sol, and continue to stir 60min, obtain ceramic size; By the ceramic size casting, be placed in the curing drying of 60 ℃ of baking ovens and obtain base substrate; Base substrate is put into to sintering oven, then from room temperature, with 10 ℃/min, be warmed up to 1140 ℃, sintering 2h, obtain light floamed ceramic after cooling.
Testing method is with embodiment 1, and light floamed ceramic density is 0.271g/cm
3, ultimate compression strength is 13.06MPa, thermal conductivity is 0.075W/ (mK).
Embodiment 5:
Get phosphorus mine tailing 10g, mud 5g, feldspar 10g, shale 4g, kaolin 3g, yellow ground 12g, water 55g, Sodium hexametaphosphate 99 1g ball milling mixing 14h, the raw material that obtain mixing; Get rosined soap 1g, tween 1g, polyacrylamide 0.1g, water 87.5g, be placed in the mechanical rapid stirring 13min of container and obtain foam; In raw material, add the 14g foam, mechanical stirring 30min, then add 2g water glass, and continue to stir 25min, obtain ceramic size; By the ceramic size casting, be placed in the curing drying of 70 ℃ of baking ovens and obtain base substrate; Base substrate is put into to sintering oven, then from room temperature, with 4 ℃/min, be warmed up to 1200 ℃, sintering 0.5h, obtain light floamed ceramic after cooling.
Testing method is with embodiment 1, and light floamed ceramic density is 0.285g/cm
3, ultimate compression strength is 14.69MPa, thermal conductivity is 0.080W/ (mK).
Embodiment 6:
Get phosphorus mine tailing 22g, mud 7g, feldspar 11g, shale 4g, kaolin 5g, yellow ground 7.5g, water 42.8g, sodium alginate 0.7g ball milling mixing 16h, the raw material that obtain mixing; Get rosined soap 2g, Sodium dodecylbenzene sulfonate 3g, polyacrylamide 0.6g, water 89g, be placed in the mechanical rapid stirring 10min of container and obtain foam; In raw material, add the 12g foam, mechanical stirring 10min, then add 1.5g starch, and continue to stir 15min, obtain ceramic size; By the ceramic size casting, be placed in the curing drying of 70 ℃ of baking ovens and obtain base substrate; Base substrate is put into to sintering oven, then from room temperature, with 7 ℃/min, be warmed up to 1080 ℃, sintering 1h, obtain light floamed ceramic after cooling.
Testing method is with embodiment 1, and light floamed ceramic density is 0.276g/cm
3, ultimate compression strength is 13.37MPa, thermal conductivity is 0.079W/ (mK).
Embodiment 7:
Get phosphorus mine tailing 25g, mud 6g, feldspar 10g, shale 7g, kaolin 4g, yellow ground 7g, water 40.2g, Sodium hexametaphosphate 99 0.8g ball milling mixing 17h, the raw material that obtain mixing; Get rosined soap 3g, tween 2g, polyacrylamide 0.7g, water 83g, be placed in the mechanical rapid stirring 17min of container and obtain foam; In raw material, add the 16g foam, mechanical stirring 35min, then add 1.2g starch, and continue to stir 18min, obtain ceramic size; By the ceramic size casting, be placed in the curing drying of 70 ℃ of baking ovens and obtain base substrate; Base substrate is put into to sintering oven, then from room temperature, with 5 ℃/min, be warmed up to 1120 ℃, sintering 1h, obtain light floamed ceramic after cooling.
Testing method is with embodiment 1, and light floamed ceramic density is 0.262g/cm
3, ultimate compression strength is 13.19MPa, thermal conductivity is 0.073W/ (mK).
Embodiment 8:
Get phosphorus mine tailing 16g, mud 8g, feldspar 13g, shale 5g, kaolin 5g, yellow ground 9g, water 43.4g, Weibull sodium 0.6g ball milling mixing 15h, the raw material that obtain mixing; Get tween 2g, Sodium dodecylbenzene sulfonate 3g, polyacrylamide 0.7g, water 80g, be placed in the mechanical rapid stirring 10min of container and obtain foam; In raw material, add the 21g foam, mechanical stirring 10min, then add 2.5gPVA solution, and continue to stir 42min, obtain ceramic size; By the ceramic size casting, be placed in the curing drying of 70 ℃ of baking ovens and obtain base substrate; Base substrate is put into to sintering oven, then from room temperature, with 4 ℃/min, be warmed up to 1170 ℃, sintering 0.5h, obtain light floamed ceramic after cooling.
Testing method is with embodiment 1, and light floamed ceramic density is 0.259g/cm
3, ultimate compression strength is 12.05MPa, thermal conductivity is 0.070W/ (mK).
The chief component of the phosphorus mine tailing that uses in above-described embodiment is Al
2O
31.51%～5.27%, SiO
213.26%～34.21%, CaO21.23%～37.45%, Na
2O0.65%～2.94%, P
2O
56.86%～19.60%, Fe
2O
31.26%～4.29% and MgO4.25%～15.41%, be mass percent.
The chief component of the mud that uses in above-described embodiment is Al
2O
39.04%～18.51%, SiO
216.53%～38.46%, CaO1.30%～8.99%, Na
2O0.65%～2.94%, P
2O
51.43%～5.82%, Fe
2O
31.57%～6.46% and MgO0.69%～4.85%,, be mass percent
The chief component of the feldspar that uses in above-described embodiment is Al
2O
316.27%～21.84%, SiO
265.19%～73.39%, CaO0.028%～0.37%, Na
2O9.38%～11.72%, K
2O0.05%～0.45%, Fe
2O
30.027%～0.810% and TiO
20.09%～0.47%, be mass percent.
The chief component of the shale that uses in above-described embodiment is Al
2O
314.39%～21.06%, SiO
251.58%～67.27%, CaO0.10%～1.43%, K
2O5.43%～7.72%, Fe
2O
35.39%～9.25%, MgO0.82%～1.85%, be mass percent.
The kaolinic chief component that uses in above-described embodiment is Al
2O
336.62%～46.97%, SiO
250.02%～53.41%, CaO0.14%～0.33%, Na
2O0.08%～0.27%, K
2O0.38%～0.57% and Fe
2O
30.33%～0.96%, be mass percent.
Light floamed ceramic prepared by above-described embodiment, as can be known by Fig. 1 and Fig. 2, the pore structure that produces is circular closed pore, hole size is even.
Claims (1)
1. a light floamed ceramic, is characterized in that by mass percentage, and this light floamed ceramic mainly is comprised of raw material 77～90%, solidifying agent 0.5～3%, foam 9.5～20%, wherein:
(1) raw material are comprised of the raw material of following mass percent: phosphorus mine tailing 10～30%, mud 5～10%, feldspar 10～14%, shale 4 ~ 10%, kaolin 3 ~ 7%, yellow ground 5～12%, dispersion agent 0.2～1%, water surplus; Wherein, dispersion agent is a kind of or two or more in Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, Sodium salts humic acids, Weibull sodium, sodium alginate;
(2) solidifying agent is a kind of or two or more in starch, gelatin, Sudan Gum-arabic, silicon sol, water glass, PVA solution;
(3) foam is that tensio-active agent 2～20%, suds-stabilizing agent 0.1～1.5% and water surplus form by mass percent; Described tensio-active agent is a kind of or two or more in sodium laurylsulfonate, rosined soap, Sodium dodecylbenzene sulfonate, tween; Described suds-stabilizing agent is a kind of or two or more in Xylo-Mucine, polyacrylamide, sodium lauryl sulphate.
2. light floamed ceramic according to claim 1, is characterized in that described raw material are comprised of the raw material of following mass percent: phosphorus mine tailing 20%, mud 8%, feldspar 12%, shale 7%, kaolin 5%, yellow ground 7%, water 40.4%, dispersion agent 0.6%.
3. light floamed ceramic according to claim 1, is characterized in that described tween is tween 20, Tween-40, Tween-60, or tween-80.
4. the preparation method of a light floamed ceramic is characterized in that comprising the following steps:
(1) preparation of raw material:
Phosphorus mine tailing, mud, feldspar, shale, kaolin, yellow ground, water and dispersion agent are mixed in proportion, with light-duty ball mill ball milling, mix 12～18h, the mass percent of each component is: phosphorus mine tailing 10～30%, mud 5～10%, feldspar 10～14%, shale 4 ~ 10%, kaolin 3 ~ 7%, yellow ground 5～12%, dispersion agent 0.2～1%, water surplus;
(2) preparation of foam:
By mass percentage, tensio-active agent 2～20%, suds-stabilizing agent 0.1～1.5% and water surplus are placed in to container, mechanical rapid stirring 5～20min obtains foams; Described tensio-active agent is a kind of or two or more in sodium laurylsulfonate, rosined soap, Sodium dodecylbenzene sulfonate, tween; Described suds-stabilizing agent is a kind of or two or more in Xylo-Mucine, polyacrylamide, sodium lauryl sulphate;
(3) preparation of ceramic size:
By step (1) gained raw material and solidifying agent, step (2) gained foam, according to mass percent, be raw material 77～90%, solidifying agent 0.5～3%, foam 9.5～20% meterings, first in raw material, add solidifying agent, mechanical stirring 10～60min, add again foam, mechanical stirring 10～30min, obtain ceramic size;
(4) moulding of base substrate:
Step (3) gained ceramic size is cast in mould, is placed in the curing drying of 60～90 ℃ of environment and obtains base substrate;
(5) sintering:
Step (4) gained base substrate is put into to sintering oven, then from room temperature, with 2～10 ℃/min, be warmed up to 1060 ℃ ~ 1200 ℃, sintering 0.5 ~ 2h, obtain light floamed ceramic after cooling.
5. the preparation method of light floamed ceramic according to claim 4, is characterized in that the solidification value after the ceramic size that makes in step (3) is cast in mould is 65～85 ℃.
6. the preparation method of light floamed ceramic according to claim 4, the temperature rise rate while it is characterized in that sintering in step (5) is 4～8 ℃/min, and sintering temperature is 1100 ℃ ~ 1150 ℃, and sintering time is 0.5 ~ 1h.
7. the preparation method of light floamed ceramic according to claim 4, is characterized in that raw material described in step (1) are comprised of the raw material of following mass percent: phosphorus mine tailing 20%, mud 8%, feldspar 12%, shale 7%, kaolin 5%, yellow ground 8%, water 39.4%, dispersion agent 0.6%.
8. the preparation method of light floamed ceramic according to claim 4, is characterized in that described tween is tween 20, Tween-40, Tween-60.
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