CN103145444B - Method for preparing heat-insulation lightweight porous mullite ceramic at low cost - Google Patents

Method for preparing heat-insulation lightweight porous mullite ceramic at low cost Download PDF

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CN103145444B
CN103145444B CN201310104069.4A CN201310104069A CN103145444B CN 103145444 B CN103145444 B CN 103145444B CN 201310104069 A CN201310104069 A CN 201310104069A CN 103145444 B CN103145444 B CN 103145444B
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mullite
ceramic
porous
slurry
hours
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CN103145444A (en
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张和平
龚伦伦
张瑞芳
王永红
程旭东
杨晖
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中国科学技术大学
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Abstract

The invention relates to a method for preparing a heat-insulation lightweight porous mullite ceramic at low cost. The method specifically comprises the following operating steps of: (1) stirring and mixing industrial mullite powder, starch, a thickening agent and a dispersing agent to obtain a mixture; (2) adding water into the mixture, stirring, and ball-milling to obtain stable ceramic slurry; (3) adding a surfactant into the ceramic slurry, stirring and foaming to obtain foam slurry; (4) pouring the foam slurry into a mould, heating and curing; (5) demoulding and drying to obtain a porous ceramic blank; and (6) sintering the porous ceramic blank in a high-temperature sintering furnace to obtain the porous mullite ceramic. The porosity and coefficient of thermal conductivity of the porous mullite ceramic prepared by the method can be adjusted through the raw material ratio, solid phase content and sintering temperature; and the porosity of the porous mullite ceramic prepared by the method is 80-86%, the density of the porous mullite ceramic is 0.43-0.62g/cm<3>, the coefficient of thermal conductivity of the porous mullite ceramic is 0.09-0.22W/(m.K), and the compressive strength of the porous mullite ceramic is 1.0-5.0MPa.

Description

The preparation method of the light porous mullite ceramic of a kind of low-cost heat insulating
Technical field
The invention belongs to porous ceramic film material technical field, relate to the preparation method of the light porous mullite ceramic of a kind of low-cost heat insulating.
Background technology
Porous ceramics is owing to having low heat conduction, low density, and high hole, the excellent properties such as high temperature resistant and corrosion-resistant, is widely used in preparing filtering membrane, support of the catalyst, burner and lagging material etc.When porous ceramics is when the heat insulating, the thermal conductivity of material just becomes the parameter of a most critical, as the thermal conductivity of lagging material general requirement material, should be less than 0.2W/ (mK).Although prepare in recent years the porous ceramics of low thermal conductivity, had many progress, large-scale industrialization is produced the preparation technology who necessarily requires cheap raw material sources and simple economy.
Mullite is a kind of stupalith of classics, it is the crystalline phase that standard atmosphere is depressed unique stable existence in silicoaluminate system, it is unique to have advantages of, as low-gravity, good creep resistance, chemical stability and Heat stability is good, low thermal conductivity, is relatively applicable to being applied to the heat insulation field of industrial heat preservation.Present stage has had many methods to prepare the porous mullite material of low thermal conductivity, as sacrificed template, adds pore-forming material method and gel injection method etc.The people such as Li Yuanbing (CN102633512A) using sawmilling or powdered rice hulls as pore-forming material for the preparation of mullite light heat-insulation brick, thermal conductivity can reach 0.2W/ (mK), but when burnouting, organic pore-forming agents can discharge a large amount of gas, cause environmental pollution, and the cavity staying after discharging and the crackle mechanical property that can affect material.The people such as Huang Chunshu (CN102515820A) make the mullite ceramic of porous light by the method for gel casting forming, thermal conductivity 0.11~0.20W/ (mK), but gel injection method is owing to being used acrylamide gel system, improved cost and limited and apply.
Summary of the invention
For the shortcoming of prior art, the invention provides and take the preparation method of industrial electric smelting mullite powder as the light porous mullite ceramic of a kind of low-cost heat insulating of prepared using mechanical stirring foaming and the curing combination of starch.
The preparation manipulation step of the light porous mullite ceramic of low-cost heat insulating is as follows:
(1) batch mixing
By industrial mullite powder with by the starch of industrial mullite powder quality 10 ~ 20wt%, by the thickening material of industrial mullite powder quality 0.2 ~ 0.5wt%, be uniformly mixed by the dispersion agent of industrial mullite powder quality 0.2 ~ 0.6wt%, obtain compound; Described starch is W-Gum or sweet potato starch or yam starch; Thickening material is Xylo-Mucine or high molecular weight sodium polyacrylate, and described high molecular weight sodium polyacrylate is molecular weight M wshould be not less than 2,000,000; Dispersion agent is Sodium hexametaphosphate 99 or Triammonium citrate;
(2) prepare slurry
In compound, add water and stir, be mixed with the slurry that solid load is 60 ~ 68wt%, ball milling 10~24 hours, obtains stable ceramic size;
(3) foaming
In ceramic size, add the tensio-active agent of pressing ceramic size quality 0.4 ~ 0.8wt%, treat that tensio-active agent dissolves completely, be not less than agitator violent stirring under 600 revs/min of conditions produce a large amount of foams at rotating speed, churning time is greater than 3 minutes, stir, obtain foamed slurry; Described tensio-active agent is sodium lauryl sulphate or Triton series emulsifying agent;
(4) be heating and curing
Foamed slurry is poured in mould, in the baking oven that immigration temperature is 80 ℃, be incubated 0.5 ~ 1 hour;
(5) demoulding is dry
Naturally cooling retreats mould, natural air drying under room temperature; Move into again in the baking oven of temperature 60 C dryly, be incubated 10~12 hours; Last dry in the baking oven of 120 ℃, be incubated 20~24 hours; Obtain porous ceramics base substrate;
(6) sintering
By porous ceramics base substrate sintering in high temperature sintering furnace, sintering condition is: before 500 ℃, temperature rise rate is 1 ℃/min, and 500 ℃ of insulations of temperature 60 minutes, after 500 ℃, temperature rise rate is 5 ℃/min, until 1300 ~ 1500 ℃ of outlet temperatures, and be incubated 2 hours, obtain porous mullite pottery; The porosity of gained porous mullite pottery is 80~86%, and density is 0.43~0.62g/cm 3, thermal conductivity is 0.09~0.22W/ (mK), ultimate compression strength is 1.0~5.0MPa.
Described industrial mullite powder is 300 order industry mullite powders.
The material of described mould is glass or stainless steel or silica gel or tetrafluoroethylene.
Porous mullite pottery porosity prepared by the present invention is 80~86%, and density is 0.43~0.62g/cm 3, thermal conductivity is 0.09~0.22 W/ (mK), ultimate compression strength is 1.0~5.0MPa.
The present invention compares with other prior aries, and advantage of the present invention is:
1. it is skeleton that the porous ceramics that prepared by the present invention adopts mullite material, and mullite has advantages of low thermal conductivity, low-gravity, Heat stability is good, has the uniquenesses such as good creep resistance and resistance to fouling; In addition, raw materials is mainly industrial mullite and agriculture starch, wide material sources;
2. the foaming technique in the present invention adopts mechanical stirring foaming, first in the ceramic size making, a certain amount of interpolation tensio-active agent produces a large amount of foams by mechanical stirring again and obtains foamed slurry, in this process without organic formwork or add organic volatilizable pore-forming material, so not a large amount of discharges, both cost-saving also protection of the environment; Gelling material starch used is carbohydrate, and after-flame is emitted carbonic acid gas and water, there is no other pollutents;
3. the present invention combines mechanical stirring foaming and starch curing, first by mechanical stirring, foam and obtain foamed slurry, then moving into baking oven for heating makes starch pasting form the gelling system with some strength, reach the object of fixed foam system within a short period of time, this technique is simple, easy handling;
4. porosity and the thermal conductivity of the porous mullite pottery that prepared by the present invention can regulate by proportioning raw materials, solid load and sintering temperature.Porous mullite pottery porosity prepared by the present invention is 80~86%, and density is 0.43~0.62g/cm 3, thermal conductivity is 0.09~0.22 W/ (mK), ultimate compression strength is 1.0~5.0MPa.
Accompanying drawing explanation
Fig. 1 is the figure of embodiment 3 and embodiment 4 finished product section photos.(left side is example 3, and the right side is example 4).
Fig. 2 is the figure of scanning electronic microscope (SEM) photo of embodiment 4 finished product sections.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, the present invention is further described.
Following instance industrial mullite used is the business mullite powder (300 order) that " Zhengzhou City Bo Ya Refractory Co., ltd " produces, the molecular formula 3Al of mullite 2o 32SiO 2; W-Gum and sweet potato starch are that Shandong Linghua Group Co., Ltd. produces; Yam starch is that Shandong Jin Cheng limited-liability company produces; Xylo-Mucine, Triammonium citrate, Sodium hexametaphosphate 99, triton x-100 (OP-10 emulsifying agent) and sodium lauryl sulphate are that Chemical Reagent Co., Ltd., Sinopharm Group produces; The molecular weight M of high molecular weight sodium polyacrylate wbe 500~8,000,000, be purchased from Aladdin reagent (China) company limited.
Embodiment 1:
By the W-Gum of industrial mullite powder and mullite powder quality 10wt%, the Xylo-Mucine of 0.2wt% and the Triammonium citrate of 0.5wt% mix, and add water and stir the slurry that is mixed with solid load 62.5wt%, and ball milling obtains stable ceramic size after 10 hours.The sodium lauryl sulphate of stock quality 0.4wt% is added in slurry, after dissolving completely, stir 5 minutes under the rotating speed of 800 revs/min, slurry produces a large amount of foams, and volumetric expansion is to 3 times of left and right of original volume.Foamed slurry is poured in silica gel mould, moved in 80 ℃ of baking ovens and place after 1 hour.After insulation, slowly the cooling mould that moves back, places after natural air drying under room temperature, then moves in the baking oven of 60 ℃ dry 12 hours, last in the baking oven of 120 ℃ dry 24 hours.Dried base substrate is warming up to 500 ℃ with 1 ℃/min, is incubated 1 hour, then is warming up to 1300 ℃ with 5 ℃/min, and be incubated 2 hours, just obtains porous mullite pottery after cooling.
The porosity of resulting product is 85.8%, and density is 0.449g/cm 3, thermal conductivity is 0.10W/ (mK), ultimate compression strength is 1.2MPa.
Embodiment 2:
By the W-Gum of industrial mullite powder and mullite powder quality 10wt%, the Xylo-Mucine of 0.2wt% and the Triammonium citrate of 0.5wt% mix, and add water and stir the slurry that is mixed with solid load 62.5wt%, and ball milling obtains stable ceramic size after 10 hours.The sodium lauryl sulphate of stock quality 0.4wt% is added in slurry, after dissolving completely, stir 5 minutes under the rotating speed of 800 revs/min, slurry produces a large amount of foams, and volumetric expansion is to 3 times of left and right of original volume.Foamed slurry is poured in silica gel mould, moved in 80 ℃ of baking ovens and place after 1 hour.After insulation, slowly the cooling mould that moves back, places after natural air drying under room temperature, then moves in the baking oven of 60 ℃ dry 12 hours, last in the baking oven of 120 ℃ dry 24 hours.Dried base substrate is warming up to 500 ℃ with 1 ℃/min, is incubated 1 hour, then is warming up to 1400 ℃ with 5 ℃/min, and be incubated 2 hours, just obtains porous mullite pottery after cooling.
The porosity of resulting product is 84.8%, and density is 0.479g/cm 3, thermal conductivity is 0.13W/ (mK), ultimate compression strength is 1.8MPa.
Embodiment 3:
By the W-Gum of industrial mullite powder and mullite powder quality 10wt%, the Xylo-Mucine of 0.2wt% and the Triammonium citrate of 0.5wt% mix, and add water and stir the slurry that is mixed with solid load 62.5wt%, and ball milling obtains stable ceramic size after 10 hours.The sodium lauryl sulphate of stock quality 0.4wt% is added in slurry, after dissolving completely, stir 5 minutes under the rotating speed of 800 revs/min, slurry produces a large amount of foams, and volumetric expansion is to 3 times of left and right of original volume.Foamed slurry is poured in silica gel mould, moved in 80 ℃ of baking ovens and place after 1 hour.After insulation, slowly the cooling mould that moves back, places after natural air drying under room temperature, then moves in the baking oven of 60 ℃ dry 12 hours, last in the baking oven of 120 ℃ dry 24 hours.Dried base substrate is warming up to 500 ℃ with 1 ℃/min, is incubated 1 hour, then is warming up to 1500 ℃ with 5 ℃/min, and be incubated 2 hours, just obtains porous mullite pottery after cooling.
The porosity of resulting product is 82.8%, and density is 0.542g/cm 3, thermal conductivity is 0.16W/ (mK), ultimate compression strength is 3.0MPa.Left side object in Fig. 1 is shown in by finished product section photo, and Fig. 1 is the macroporosity pattern of making porous mullite pottery, contains as seen from the figure a large amount of spherical void structures in sample.
Embodiment 4:
By the W-Gum of industrial mullite powder and mullite powder quality 10wt%, the Xylo-Mucine of 0.2wt% and the Triammonium citrate of 0.5wt% mix, and add water and stir the slurry that is mixed with solid load 67.5wt%, and ball milling obtains stable ceramic size after 10 hours.The sodium lauryl sulphate of stock quality 0.4wt% is added in slurry, after dissolving completely, stir 5 minutes under the rotating speed of 800 revs/min, slurry produces a large amount of foams, and volumetric expansion is to 2 times of left and right of original volume.Foamed slurry is poured in rustless steel mould, moved in 80 ℃ of baking ovens and place after 1 hour.After insulation, slowly the cooling mould that moves back, places after natural air drying under room temperature, then moves in the baking oven of 60 ℃ dry 12 hours, last in the baking oven of 120 ℃ dry 24 hours.Dried base substrate is warming up to 500 ℃ with 1 ℃/min, is incubated 1 hour, then is warming up to 1500 ℃ with 5 ℃/min, and be incubated 2 hours, just obtains porous mullite pottery after cooling.
The porosity of resulting product is 80.3%, and density is 0.624g/cm 3, thermal conductivity is 0.22W/ (mK), ultimate compression strength is 5.0MPa.Right side object in Fig. 1 is shown in by finished product section photo, Fig. 1 is the macroporosity pattern of making porous mullite pottery, in sample, contain as seen from the figure a large amount of spherical void structures, and can find that by 2 samples in contrast left and right the sample that porosity is larger (left side) contains more macropore; Fig. 2 is shown in by the scanning electronic microscope of finished product section (SEM) photo, makes as seen from Figure 2 the microscopic void pattern of porous mullite pottery, and the micropore structure that finished product have been described is spherical void structure.
Embodiment 5:
By the yam starch of industrial mullite powder and mullite powder quality 20wt%, the Xylo-Mucine of 0.2wt% and the Sodium hexametaphosphate 99 of 0.2wt% mix, and add water and stir the slurry that is mixed with solid load 60wt%, and ball milling obtains stable ceramic size after 10 hours.The sodium lauryl sulphate of stock quality 0.4wt% is added in slurry, after dissolving completely, stir 5 minutes under the rotating speed of 800 revs/min, slurry produces a large amount of foams, and volumetric expansion is to 3 times of left and right of original volume.Foamed slurry is poured in glass mold, moved in 80 ℃ of baking ovens and place after 1 hour.After insulation, slowly the cooling mould that moves back, places after natural air drying under room temperature, then moves in the baking oven of 60 ℃ dry 12 hours, last in the baking oven of 120 ℃ dry 24 hours.Dried base substrate is warming up to 500 ℃ with 1 ℃/min, is incubated 1 hour, then is warming up to 1300 ℃ with 5 ℃/min, and be incubated 2 hours, just obtains porous mullite pottery after cooling.
The porosity of resulting product is 86.3%, and density is 0.432g/cm 3, thermal conductivity is 0.09W/ (mK), ultimate compression strength is 1.0MPa.
Embodiment 6:
By the sweet potato starch of industrial mullite powder and mullite powder quality 10wt%, the sodium polyacrylate of 0.6wt% and the Sodium hexametaphosphate 99 of 0.5wt% mix, and add water and stir the slurry that is mixed with solid load 62.5wt%, and ball milling obtains stable ceramic size after 10 hours.The triton x-100 of stock quality 0.8wt% is added dropwise in slurry, after stirring at low speed is even, stirs 5 minutes under the rotating speed of 800 revs/min, slurry produces a large amount of foams, and volumetric expansion is to 2 times of left and right of original volume.Foamed slurry is poured in tetrafluoroethylene mould, moved in 80 ℃ of baking ovens and place after 1 hour.After insulation, slowly the cooling mould that moves back, places after natural air drying under room temperature, then moves in the baking oven of 60 ℃ dry 12 hours, last in the baking oven of 120 ℃ dry 24 hours.Dried base substrate is warming up to 500 ℃ with 1 ℃/min, is incubated 1 hour, then is warming up to 1300 ℃ with 5 ℃/min, and be incubated 2 hours, just obtains porous mullite pottery after cooling.
The porosity of resulting product is 81.7%, and density is 0.578g/cm 3, thermal conductivity is 0.18W/ (mK), ultimate compression strength is 3.7MPa.

Claims (2)

1. a preparation method for the light porous mullite ceramic of low-cost heat insulating, is characterized in that concrete operation step is as follows:
(1) batch mixing
By industrial mullite powder with by the starch of industrial mullite powder quality 10~20wt%, by the thickening material of industrial mullite powder quality 0.2~0.5wt%, be uniformly mixed by the dispersion agent of industrial mullite powder quality 0.2~0.6wt%, obtain compound; Described starch is W-Gum or sweet potato starch or yam starch; Thickening material is Xylo-Mucine or high molecular weight sodium polyacrylate, and described high molecular weight sodium polyacrylate is molecular weight M wshould be not less than 2,000,000; Dispersion agent is Sodium hexametaphosphate 99 or Triammonium citrate;
Described industrial mullite powder is 300 order industry mullite powders;
(2) prepare slurry
In compound, add water and stir, be mixed with the slurry that solid load is 60~68wt%, ball milling 10~24 hours, obtains stable ceramic size;
(3) foaming
In ceramic size, add the tensio-active agent of pressing ceramic size quality 0.4~0.8wt%, treat that tensio-active agent dissolves completely, be not less than agitator violent stirring under 600 revs/min of conditions produce a large amount of foams at rotating speed, churning time is greater than 3 minutes, stir, obtain foamed slurry; Described tensio-active agent is sodium lauryl sulphate or Triton series emulsifying agent;
(4) be heating and curing
Foamed slurry is poured in mould, in the baking oven that immigration temperature is 80 ℃, be incubated 0.5~1 hour;
(5) demoulding is dry
Naturally cooling retreats mould, natural air drying under room temperature; Move into again in the baking oven of temperature 60 C dryly, be incubated 10~12 hours; Last dry in the baking oven of 120 ℃, be incubated 20~24 hours; Obtain porous ceramics base substrate;
(6) sintering
By porous ceramics base substrate sintering in high temperature sintering furnace, sintering condition is: before 500 ℃, temperature rise rate is 1 ℃/min, and 500 ℃ of insulations of temperature 60 minutes, after 500 ℃, temperature rise rate is 5 ℃/min, until 1300~1500 ℃ of outlet temperatures, and be incubated 2 hours, obtain porous mullite pottery; The porosity of gained porous mullite pottery is 80~86%, and density is 0.43~0.62g/cm 3, thermal conductivity is 0.09~0.22W/ (mK), ultimate compression strength is 1.0~5.0MPa.
2. the preparation method of the light porous mullite ceramic of a kind of low-cost heat insulating according to claim 1, is characterized in that: the material of described mould is glass or stainless steel or silica gel or tetrafluoroethylene.
CN201310104069.4A 2013-03-28 2013-03-28 Method for preparing heat-insulation lightweight porous mullite ceramic at low cost CN103145444B (en)

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CN104177119B (en) * 2014-08-14 2015-09-16 合肥科斯孚安全科技有限公司 A kind of preparation method of light flyash heat insulating porous ceramics
HUE045060T2 (en) * 2014-09-24 2019-12-30 Matthias Rath Method for producing a foamed ceramic
CN104446623B (en) * 2014-11-27 2017-01-11 武汉科技大学 Mullite porous ceramic and preparation method thereof
CN104446625A (en) * 2014-11-28 2015-03-25 中国科学技术大学先进技术研究院 High-porosity porous ceramic and preparation method thereof
CN105503238A (en) * 2015-12-16 2016-04-20 韩功篑 Foaming-ceramic heat insulating board and preparing method thereof
CN106146034B (en) * 2016-08-11 2018-12-11 华北水利水电大学 A kind of porous mullite-corundum load perovskite La1-xKxCo0.7Fe0.3O3The preparation method of material
CN106316444A (en) * 2016-08-11 2017-01-11 华北水利水电大学 Preparing method of porous mullite ceramic
CN106242637A (en) * 2016-08-11 2016-12-21 华北水利水电大学 A kind of preparation method of porous mullite corundum ceramic
CN106518095B (en) * 2016-09-29 2019-03-19 中国科学院上海硅酸盐研究所 A kind of method that surfactant hydrophobic modifiers dispersants prepare foamed ceramics
CN107552795B (en) * 2017-09-26 2019-06-21 成都新柯力化工科技有限公司 A method of foam metal is prepared using porous-starch foaming
CN109133977A (en) * 2018-08-29 2019-01-04 佛山市森昂生物科技有限公司 A kind of preparation method of porous bio-ceramic
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