CN106242619B - A kind of preparation method of homogeneous porous ceramics accumulation of heat basis material - Google Patents
A kind of preparation method of homogeneous porous ceramics accumulation of heat basis material Download PDFInfo
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- CN106242619B CN106242619B CN201610646467.2A CN201610646467A CN106242619B CN 106242619 B CN106242619 B CN 106242619B CN 201610646467 A CN201610646467 A CN 201610646467A CN 106242619 B CN106242619 B CN 106242619B
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
- C04B38/025—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents generated by microorganisms
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- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
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- C04B33/16—Lean materials, e.g. grog, quartz
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
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Abstract
The present invention relates to a kind of preparation methods of homogeneous porous ceramics accumulation of heat basis material, belong to heat-storing material preparation technical field.This method is pulverized after mixing mine soil, using aluminium metaphosphate as adhesion agent, slurrying is adulterated with the methane liquid rich in microorganism, green body is made with cow dung fermentation reactor system pore-creating again in pre-burning after injection molding compacting, and high-temperature calcination is after last water logging fast frozen up to thermal storage ceramic matrix.The present invention generates equally distributed stomata by the fermentation of microorganism in pre- green body, the principle that volume increases after recycling the moisture content immersed in green body to freeze is " ice is split " effect to widen aperture inside green body, increase porosity, finally obtained matrix, efficiently solve at present that common ceramic heat-storing basis material gas cell distribution is uneven, the porosity is low causes load capacity few, it the problem of influencing heat-storing energy efficiency, has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of homogeneous porous ceramics accumulation of heat basis material, belong to heat-storing material technology of preparing
Field.
Background technique
The fast development of contemporary society consumes mass energy, however along with the exhaustion of fossil fuel, the shortage of the energy
Become the big bottleneck for restricting human survival and development, it is extremely urgent to develop and utilize new energy.Solar energy, wind energy, Hydrogen Energy
As important new energy, have the advantages that inexhaustible, nexhaustible, and solar power generation is as a kind of cleanliness without any pollution
Energy utilization patterns have caused the extensive concern of whole world researcher.
Heat-storing material is one kind that recent research is more in terms of energy conservation, and wherein solid-liquid phase change material is because having use scope
Extensively, thermal coefficient is big, storage heat density is big, phase transformation volume change is small, be generally in neutrality, small toxicity, it is cheap the advantages that and it is general
All over being interested by researchers.But solid-liquid phase change material there are during phase-transition heat-storage along with the variation of state the shortcomings that,
Therefore the regularization of phase-change material phase transition process is at key point to solve this problem.The method solved at present mainly has phase
Become the microencapsulation of material and prepares composite heat storage material.In the preparation process of composite heat storage material, porous ceramic matrices suitable
Research is relatively more, wherein widely used is the porous ceramic matrices suitable of ceramic honey comb matrix and addition pore creating material preparation.And
Both porous ceramics for heat storage material matrix there are many disadvantages, such as ceramic honey comb there are apparent porosities low, aperture size
The problems such as porous ceramics of the problems such as excessive, addition pore creating material preparation are uneven there are gas cell distribution.
Ceramic heat-storing basis material common at present is made by addition pore creating material, and addition pore creating material be easy to cause base
The problem of body gas cell distribution is uneven, the porosity is low leads to load capacity less and influence heat accumulation function efficiency is successively studied a kind of homogeneous
Porous lines carrier regenerator material has splendid Research Prospects.
Summary of the invention
Present invention mainly solves the technical issues of：For the porous regenerator ceramic matrix prepared at present by addition pore creating material
That there are gas cell distributions is uneven, the porosity is low causes load capacity few, influences the defect of heat-storing energy efficiency, provides a kind of homogeneous
The preparation method of porous ceramics accumulation of heat basis material, this method is pulverized after mixing mine soil, using aluminium metaphosphate as adhesion agent,
Slurrying is adulterated with the methane liquid rich in microorganism, green body is made with cow dung fermentation reactor system pore-creating again in pre-burning after injection molding compacting, finally
High-temperature calcination is after water logging fast frozen up to thermal storage ceramic matrix.The present invention is produced in pre- green body by the fermentation of microorganism
Raw equally distributed stomata, recycling the principle for immersing volume increase after the moisture in green body freezes is that " ice is split " acts on to widen
Aperture inside green body increases porosity, and matrix is finally made, and efficiently solves current common ceramic heat-storing basis material stomata point
It the problem of cloth is uneven, the porosity is low causes load capacity few, influence heat-storing energy efficiency, has broad application prospects.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
（1）Weigh 300~400g kaolin, 250~300g mullite, 200~250g red mud and 220~250g river sand
It is put into ore flour mill after mixing, obtains composite ore soil to cross 200 meshes after 70~80kW power grinding, 20~30min
Powder；
（2）It is in mass ratio 1:8 are fitted into aluminium metaphosphate and above-mentioned composite ore soil powder in ceramic pot together, then to ceramics
It is added the fowl and animal excrement methane-generating pit biogas slurry at the middle and upper levels of composite ore soil total powder quality 1/2 in tank, after mixing evenly with stirring rod
Expect to pureed and be transferred in the square mould that side length is 5cm, suppresses 15 with hydraulic press with the pressure pressure maintaining of 4~6MPa
It is put into baking oven dry 40~50min at 180~200 DEG C after~20min, obtains pre- green body；
（3）Above-mentioned pre- green body is wrapped with gauze and is placed on jar for picking vegetable bottom, covers altar after cow dung is filled into altar, it will
Jar for picking vegetable is placed in 30~40 DEG C of greenhouses heat-preservation fermentation 2~3 weeks, is taken out the pre- green body of gauze package, is put it into Muffle furnace,
It is taken out after firing 1~2h with 300~400 DEG C of temperature, is cooled to room temperature, obtains ceramic body；
（4）Above-mentioned ceramic body is immersed in 5~8 times of deionized waters of its volume, with sonic oscillation instrument with 200~300W function
The deionized water immersed in green body hole is set to freeze with 1~2min of liquid nitrogen flash freezer after 12~14h of rate oscillation dipping, after quick-frozen
To its spontaneous recovery to room temperature, make the ice-out in hole, by it is aforementioned immersion, it is quick-frozen, melt the step of operate repeatedly 3~5 times,
Ceramic matrix crude product is obtained after drying；
（5）Ceramic matrix crude product obtained above is put into tube type resistance furnace, is first warming up to 5 DEG C/min rate program
1~2h are calcined in 400~500 DEG C of heat preservations, then with 3 DEG C/min rate be warming up to 600~700 DEG C continue 2~4h of calcining after discharge, tear open
Up to homogeneous porous ceramics accumulation of heat basis material after mould.
Application method of the invention：Solid-liquid phase change is loaded using homogeneous porous ceramics accumulation of heat basis material produced by the present invention
It is wrapped up after material with epoxy resin, can be prepared by phase change heat storage material, through detecting, accumulation of heat basis material produced by the present invention shows gas
Porosity is 85.0~89.9%, and compression strength reaches 2.05~2.20MPa, can solve solid-liquid phase change material phase transition process without fixed
The problem of type.
The beneficial effects of the invention are as follows：
（1）Homogeneous porous ceramics accumulation of heat basis material raw material produced by the present invention are easy to get, and preparation process is simple to operation,
It is low in cost；
（2）Homogeneous porous ceramics accumulation of heat basis material apparent porosity produced by the present invention is 85.0~89.9%, compression strength
Reach 2.05~2.20MPa, there is excellent mechanical property and uniform microstructure, have broad application prospects.
Specific embodiment
It is mixed to weigh 300~400g kaolin, 250~300g mullite, 200~250g red mud and 220~250g river sand
It is put into ore flour mill after closing uniformly, obtains composite ore soil powder to cross 200 meshes after 70~80kW power grinding, 20~30min
End；It is in mass ratio 1:8 are fitted into aluminium metaphosphate and above-mentioned composite ore soil powder in ceramic pot together, then are added into ceramic pot
The fowl and animal excrement methane-generating pit of composite ore soil total powder quality 1/2 biogas slurry at the middle and upper levels, it is pre- that pureed is obtained with stirring rod after mixing evenly
Expect and be transferred in the square mould that side length is 5cm, 15~20min is suppressed with the pressure pressure maintaining of 4~6MPa with hydraulic press
After be put into baking oven dry 40~50min at 180~200 DEG C, obtain pre- green body；Above-mentioned pre- green body is wrapped with gauze and is placed on
Jar for picking vegetable bottom covers altar after filling cow dung into altar, and jar for picking vegetable is placed on heat-preservation fermentation 2~3 in 30~40 DEG C of greenhouses
Week the pre- green body of gauze package is taken out, Muffle furnace is put it into, taken out, be cooled to after firing 1~2h with 300~400 DEG C of temperature
Room temperature obtains ceramic body；Above-mentioned ceramic body is immersed in 5~8 times of deionized waters of its volume, with sonic oscillation instrument with 200
The deionized water immersed in green body hole is set to freeze with 1~2min of liquid nitrogen flash freezer after 12~14h of~300W oscillation of power dipping, speed
To its spontaneous recovery to room temperature after jelly, make the ice-out in hole, by it is aforementioned immersion, it is quick-frozen, melt the step of grasp repeatedly
Make 3~5 times, obtains ceramic matrix crude product after dry；Ceramic matrix crude product obtained above is put into tube type resistance furnace, first with
5 DEG C/min rate program is warming up to 400~500 DEG C of heat preservations and calcines 1~2h, then is warming up to 600~700 DEG C with 3 DEG C/min rate
It discharges after continuing 2~4h of calcining, up to homogeneous porous ceramics accumulation of heat basis material after demoulding.
Example 1
It weighs 300g kaolin, 250g mullite, 200g red mud and 220g river sand and is put into ore milling after mixing
In machine, composite ore soil powder is obtained to cross 200 meshes after 70kW power grinding 20min；It is in mass ratio 1:8 by aluminium metaphosphate and
Above-mentioned composite ore soil powder is fitted into ceramic pot together, then the poultry of composite ore soil total powder quality 1/2 is added into ceramic pot
Excrement methane-generating pit biogas slurry at the middle and upper levels obtains pureed after mixing evenly with stirring rod and expects and be transferred to the pros that side length is 5cm
In mould, it is put into baking oven dry 40min at 180 DEG C after suppressing 15min with hydraulic press with the pressure pressure maintaining of 4MPa, is obtained pre-
Green body；Above-mentioned pre- green body is wrapped with gauze and is placed on jar for picking vegetable bottom, covers altar after cow dung is filled into altar, by jar for picking vegetable
It is placed in 30 DEG C of greenhouses heat-preservation fermentation 2 weeks, takes out the pre- green body of gauze package, put it into Muffle furnace, burnt with 300 DEG C of temperature
It takes out, is cooled to room temperature after 1h processed, obtain ceramic body；Above-mentioned ceramic body is immersed in 5 times of deionized waters of its volume, with super
Sound oscillation instrument makes the deionized water immersed in green body hole freeze after impregnating 12h with 200W oscillation of power with liquid nitrogen flash freezer 1min,
To its spontaneous recovery to room temperature after quick-frozen, make the ice-out in hole, by it is aforementioned immersion, it is quick-frozen, melt the step of repeatedly
Operation 3 times obtains ceramic matrix crude product after dry；Ceramic matrix crude product obtained above is put into tube type resistance furnace, first with 5
DEG C/min rate program is warming up to 400 DEG C of heat preservations calcining 1h, then is warming up to 600 DEG C with 3 DEG C/min rate and continues to go out after calcining 2h
Material, up to homogeneous porous ceramics accumulation of heat basis material after demoulding.
Application method of the invention：Solid-liquid phase change is loaded using homogeneous porous ceramics accumulation of heat basis material produced by the present invention
It is wrapped up after material with epoxy resin, can be prepared by phase change heat storage material, through detecting, accumulation of heat basis material produced by the present invention shows gas
The problem of porosity is 85.0%, and compression strength reaches 2.05MPa, can solve solid-liquid phase change material phase transition process partial amorphism.
Example 2
It weighs 350g kaolin, 280g mullite, 230g red mud and 240g river sand and is put into ore milling after mixing
In machine, composite ore soil powder is obtained to cross 200 meshes after 75kW power grinding 25min；It is in mass ratio 1:8 by aluminium metaphosphate and
Above-mentioned composite ore soil powder is fitted into ceramic pot together, then the poultry of composite ore soil total powder quality 1/2 is added into ceramic pot
Excrement methane-generating pit biogas slurry at the middle and upper levels obtains pureed after mixing evenly with stirring rod and expects and be transferred to the pros that side length is 5cm
In mould, it is put into baking oven dry 45min at 190 DEG C after suppressing 18min with hydraulic press with the pressure pressure maintaining of 5MPa, is obtained pre-
Green body；Above-mentioned pre- green body is wrapped with gauze and is placed on jar for picking vegetable bottom, covers altar after cow dung is filled into altar, by jar for picking vegetable
It is placed in 35 DEG C of greenhouses heat-preservation fermentation 2 weeks, takes out the pre- green body of gauze package, put it into Muffle furnace, burnt with 350 DEG C of temperature
It takes out, is cooled to room temperature after 2h processed, obtain ceramic body；Above-mentioned ceramic body is immersed in 6 times of deionized waters of its volume, with super
Sound oscillation instrument makes the deionized water immersed in green body hole freeze after impregnating 13h with 250W oscillation of power with liquid nitrogen flash freezer 2min,
To its spontaneous recovery to room temperature after quick-frozen, make the ice-out in hole, by it is aforementioned immersion, it is quick-frozen, melt the step of repeatedly
Operation 4 times obtains ceramic matrix crude product after dry；Ceramic matrix crude product obtained above is put into tube type resistance furnace, first with 5
DEG C/min rate program is warming up to 450 DEG C of heat preservations calcining 2h, then is warming up to 650 DEG C with 3 DEG C/min rate and continues to go out after calcining 3h
Material, up to homogeneous porous ceramics accumulation of heat basis material after demoulding.
Application method of the invention：Solid-liquid phase change is loaded using homogeneous porous ceramics accumulation of heat basis material produced by the present invention
It is wrapped up after material with epoxy resin, can be prepared by phase change heat storage material, through detecting, accumulation of heat basis material produced by the present invention shows gas
The problem of porosity is 87.5%, and compression strength reaches 2.12MPa, can solve solid-liquid phase change material phase transition process partial amorphism.
Example 3
It weighs 400g kaolin, 300g mullite, 250g red mud and 250g river sand and is put into ore milling after mixing
In machine, composite ore soil powder is obtained to cross 200 meshes after 80kW power grinding 30min；It is in mass ratio 1:8 by aluminium metaphosphate and
Above-mentioned composite ore soil powder is fitted into ceramic pot together, then the poultry of composite ore soil total powder quality 1/2 is added into ceramic pot
Excrement methane-generating pit biogas slurry at the middle and upper levels obtains pureed after mixing evenly with stirring rod and expects and be transferred to the pros that side length is 5cm
In mould, it is put into baking oven dry 50min at 200 DEG C after suppressing 20min with hydraulic press with the pressure pressure maintaining of 6MPa, is obtained pre-
Green body；Above-mentioned pre- green body is wrapped with gauze and is placed on jar for picking vegetable bottom, covers altar after cow dung is filled into altar, by jar for picking vegetable
It is placed in 40 DEG C of greenhouses heat-preservation fermentation 3 weeks, takes out the pre- green body of gauze package, put it into Muffle furnace, burnt with 400 DEG C of temperature
It takes out, is cooled to room temperature after 2h processed, obtain ceramic body；Above-mentioned ceramic body is immersed in 8 times of deionized waters of its volume, with super
Sound oscillation instrument makes the deionized water immersed in green body hole freeze after impregnating 14h with 300W oscillation of power with liquid nitrogen flash freezer 2min,
To its spontaneous recovery to room temperature after quick-frozen, make the ice-out in hole, by it is aforementioned immersion, it is quick-frozen, melt the step of repeatedly
Operation 5 times obtains ceramic matrix crude product after dry；Ceramic matrix crude product obtained above is put into tube type resistance furnace, first with 5
DEG C/min rate program is warming up to 500 DEG C of heat preservations calcining 2h, then is warming up to 700 DEG C with 3 DEG C/min rate and continues to go out after calcining 4h
Material, up to homogeneous porous ceramics accumulation of heat basis material after demoulding.
Application method of the invention：Solid-liquid phase change is loaded using homogeneous porous ceramics accumulation of heat basis material produced by the present invention
It is wrapped up after material with epoxy resin, can be prepared by phase change heat storage material, through detecting, accumulation of heat basis material produced by the present invention shows gas
The problem of porosity is 89.9%, and compression strength reaches 2.20MPa, can solve solid-liquid phase change material phase transition process partial amorphism.
Claims (1)
1. a kind of preparation method of homogeneous porous ceramics accumulation of heat basis material, it is characterised in that specifically preparation step is：
（1）Weigh 300~400g kaolin, 250~300g mullite, 200~250g red mud and the mixing of 220~250g river sand
It is put into ore flour mill after uniformly, obtains composite ore soil powder to cross 200 meshes after 70~80kW power grinding, 20~30min
End；
（2）It is in mass ratio 1:8 are fitted into aluminium metaphosphate and above-mentioned composite ore soil powder in ceramic pot together, then into ceramic pot
The fowl and animal excrement methane-generating pit biogas slurry at the middle and upper levels of composite ore soil total powder quality 1/2 is added, obtains mud after mixing evenly with stirring rod
Shape is expected simultaneously to be transferred in the square mould that side length is 5cm, with hydraulic press with the pressure pressure maintaining of 4~6MPa compacting 15~
It is put into baking oven dry 40~50min at 180~200 DEG C after 20min, obtains pre- green body；
（3）Above-mentioned pre- green body is wrapped with gauze and is placed on jar for picking vegetable bottom, covers altar after cow dung is filled into altar, by pickle
Altar is placed in 30~40 DEG C of greenhouses heat-preservation fermentation 2~3 weeks, is taken out the pre- green body of gauze package, is put it into Muffle furnace, with
300~400 DEG C of temperature are taken out after firing 1~2h, are cooled to room temperature, obtain ceramic body；
（4）Above-mentioned ceramic body is immersed in 5~8 times of deionized waters of its volume, with sonic oscillation instrument with the vibration of 200~300W power
Swing makes the deionized water immersed in green body hole freeze after 12~14h of dipping with 1~2min of liquid nitrogen flash freezer, it is quick-frozen after to it
Spontaneous recovery makes the ice-out in hole to room temperature, by aforementioned immersion, it is quick-frozen, melt the step of operate repeatedly 3~5 times, it is dry
After obtain ceramic matrix crude product；
（5）Ceramic matrix crude product obtained above is put into tube type resistance furnace, is first warming up to 400 with 5 DEG C/min rate program
1~2h are calcined in~500 DEG C of heat preservations, then with 3 DEG C/min rate be warming up to 600~700 DEG C continue 2~4h of calcining after discharge, demoulding
Afterwards up to homogeneous porous ceramics accumulation of heat basis material.
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| CN107032759B (en) * | 2017-02-28 | 2021-03-16 | 沈阳理工大学 | Method for preparing carbon-loaded porous ceramic and slow-release compound fertilizer by using livestock and poultry manure |
| CN106747641B (en) * | 2017-02-28 | 2021-03-16 | 沈阳理工大学 | Method for preparing foam liquid and porous ceramic for foam concrete by using cow dung |
| CN107043242B (en) * | 2017-02-28 | 2021-03-16 | 沈阳理工大学 | Method for preparing porous ceramic composite material and foam liquid by using sludge and cow dung |
| CN107032758B (en) * | 2017-02-28 | 2021-03-16 | 沈阳理工大学 | Method for preparing gas purification porous ceramic by using sludge and cow dung |
| CN106892671A (en) * | 2017-03-31 | 2017-06-27 | 美科特种材料股份有限公司 | A kind of large dosage river sand makes the production technology of hollow foam ceramics |
| CN108164251A (en) * | 2018-01-10 | 2018-06-15 | 和县明生环保材料有限责任公司 | A kind of production method of ceramic thermal insulation materials for wall |
| CN111454696B (en) * | 2020-05-20 | 2021-02-26 | 温州大学 | Hexadecylamine/aluminum phosphate composite shape-stabilized phase change material and preparation method thereof |
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| CN104136874A (en) * | 2011-12-22 | 2014-11-05 | 法商圣高拜欧洲实验及研究中心 | Regenerator with composite insulating wall |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104136874A (en) * | 2011-12-22 | 2014-11-05 | 法商圣高拜欧洲实验及研究中心 | Regenerator with composite insulating wall |
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