CN110105058A - A kind of foamed ceramics and its application in the treatment of waste water - Google Patents
A kind of foamed ceramics and its application in the treatment of waste water Download PDFInfo
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- CN110105058A CN110105058A CN201910477087.4A CN201910477087A CN110105058A CN 110105058 A CN110105058 A CN 110105058A CN 201910477087 A CN201910477087 A CN 201910477087A CN 110105058 A CN110105058 A CN 110105058A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
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Abstract
The present invention provides a kind of foamed ceramics, by weight, preparation method is the following steps are included: by diatomite, kaolin, quartz, straw biological charcoal and α-Al for ingredient2O3Micro mist mixed grinding;Add water for ball milling, dries to obtain mixed powder;Gelatin solution is added, prepares slurry, mixing and ball milling;Vacuum outgas is injected in mold, sealing and curing;It is demoulded after drying;It is placed in supercritical carbon dioxide foaming device and foams;Roasting;It is laid in after cooling in low-temperature plasma processing unit and handles to obtain modified foamed ceramics;Take Al (NO3)3·9H2O and distilled water stirring and dissolving, are heated at reflux, aluminium powder are added to react;Obtain colorless and transparent colloidal sol;Polyethylene glycol, lanthanum nitrate and barium nitrate, stirring and dissolving is added;Modified foamed ceramics is immersed, is taken out after vacuum impregnation, it is dry;It is roasted after taking-up to obtain the final product.Foamed ceramics provided by this law all has extraordinary treatment effect for COD and ammonia nitrogen, can be effectively applied to wastewater treatment.
Description
Technical field
Application the present invention relates to a kind of foamed ceramics and its in the treatment of waste water.
Background technique
Foamed ceramics be it is fast-developing in recent years get up there is specific function with one kind that stomata is main composition part
Ceramic material, be as components such as aggregate, pore creating material and binders by made of high temperature sintering.It can be divided according to pore size
Are as follows: large pore material, mesoporous material and poromerics.Good chemical stability that foam ceramic material has, high mechanical strength and
The advantages that high temperature resistant.Meanwhile also there is large specific surface area, the features such as porosity is high.Its flourishing microcellular structure, big ratio table
Area is conducive to the growth and breeding of microorganism;There is in water treatment procedure retention suspended solid simultaneously, improve water-gas distribution
Effect.Remold it is modified can effectively be used in wastewater treatment, new development side is provided for wastewater treatment
To.
Summary of the invention
Technical problems to be solved: a kind of foamed ceramics and its application in the treatment of waste water, gained foamed ceramics are provided
All there is extraordinary treatment effect for COD and ammonia nitrogen, wastewater treatment can be effectively applied to.
Technical solution: a kind of foamed ceramics, ingredient by weight, preparation method the following steps are included:
(1) by 20-30 parts of diatomite, 20-30 parts of kaolin, 10-20 parts of quartz, 5-10 parts of straw biological charcoals and 5-10 parts of α-
Al2O3Micro mist mixing, is ground to fineness < 0.1mm;
(2) plus water polo is milled to partial size≤2 μm, dries to obtain mixed powder;
(3) gelatin solution is added, prepares the slurry that total solid content is 40-45%, mixing and ball milling 5-10min;
(4) it by vacuum outgas after slurry magnetic agitation, injects in mold, is placed in sealing and curing 1h in 85 DEG C of thermostatic drying chambers;
(5) it is transferred in 50 DEG C of drying boxes and is demoulded after drying;
(6) it is placed in the autoclave of supercritical carbon dioxide foaming device, is first filled with low pressure CO 2 for air displacement in kettle
Completely, it is re-filled with high-pressure carbon dioxide, 10-20min is swollen at 50-80 DEG C of temperature, pressure 10-20MPa, is quickly unloaded in 2s
Pressure;
(7) it is put into Muffle furnace, roasts 4h at 1300-1350 DEG C of temperature;
(8) it is equably laid on the ground electrode in low-temperature plasma processing unit after cooling, in supply frequency 10-15kHz, work
Processing 10-15min must be modified foamed ceramics under the conditions of making voltage 20kV, discharge power 70-80W;
(9) 200-250 parts of Al (NO are taken3)3·9H2O and 600-650 parts of distilled water stirring and dissolving, is put into water-bath, at 90 DEG C
Under be heated at reflux, be slowly added into the reaction of 35-40 parts of aluminium powders, the pH value that solution is controlled in reaction process is 3.0-4.0;
(10) bottom gray precipitate is removed after being centrifugated, and obtains colorless and transparent colloidal sol;
(11) 20-25 parts of polyethylene glycol, 3-6 parts of lanthanum nitrates and 4-8 parts of barium nitrates are added, it is molten that stirring and dissolving obtains pale yellow transparent
Glue;
(12) modified foamed ceramics is immersed in pale yellow transparent colloidal sol, takes out, is put into drying box after vacuum impregnation 0.5-1h
It is dry;
(13) it is put into Muffle furnace after taking out and roasts 5h at 500-800 DEG C up to foamed ceramics.
Further, content of the gelatin in mixed powder is 20wt%-30wt% in the step (3).
Further, in the step (6) temperature be 65 DEG C, pressure 15MPa, swelling time 15min.
Further, supply frequency is 13kHz, discharge power 75W in the step (8).
A kind of application of foamed ceramics in the treatment of waste water.
The utility model has the advantages that
1. with supercritical CO2It foams, avoids the use of organic solvent, energy conservation and environmental protection.
2. the surface mesoporous quantity of foamed ceramics increases, and surface is more coarse after the processing of low-temperature plasma processing unit, increases and inhale
Attached performance.
3. all there is extraordinary treatment effect, after processing, COD for COD and ammonia nitrogen through foamed ceramics prepared by the present invention
It is all up to 97.2% and 92.1% respectively with the removal rate of ammonia nitrogen.
Specific embodiment
Embodiment 1
A kind of foamed ceramics, ingredient by weight, preparation method the following steps are included:
(1) by 20 parts of diatomite, 20 parts of kaolin, 10 parts of quartz, 5 parts of straw biological charcoals and 5 parts of α-Al2O3Micro mist mixing, grinds
It is milled to fineness < 0.1mm;
(2) plus water polo is milled to partial size≤2 μm, dries to obtain mixed powder;
(3) gelatin solution is added, prepares the slurry that total solid content is 40%, mixing and ball milling 5min, wherein gelatin is in mixed powder
In content be 20wt%;
(4) it by vacuum outgas after slurry magnetic agitation, injects in mold, is placed in sealing and curing 1h in 85 DEG C of thermostatic drying chambers;
(5) it is transferred in 50 DEG C of drying boxes and is demoulded after drying;
(6) it is placed in the autoclave of supercritical carbon dioxide foaming device, is first filled with low pressure CO 2 for air displacement in kettle
Completely, it is re-filled with high-pressure carbon dioxide, is swollen 10min at temperature 50 C, pressure 10MPa, the fast pressure relief in 2s;
(7) it is put into Muffle furnace, roasts 4h at 1300 DEG C of temperature;
(8) it is equably laid on the ground electrode in low-temperature plasma processing unit after cooling, in supply frequency 10kHz, work
10min is handled under the conditions of voltage 20kV, discharge power 70W must be modified foamed ceramics;
(9) 200 parts of Al (NO are taken3)3·9H2O and 600 part of distilled water stirring and dissolving, is put into water-bath, is returned at 90 DEG C
Stream heating is slowly added into 35 parts of aluminium powder reactions, and the pH value that solution is controlled in reaction process is 3.0;
(10) bottom gray precipitate is removed after being centrifugated, and obtains colorless and transparent colloidal sol;
(11) 20 parts of polyethylene glycol, 3 parts of lanthanum nitrates and 4 parts of barium nitrates, stirring and dissolving is added and obtains pale yellow transparent colloidal sol;
(12) modified foamed ceramics is immersed in pale yellow transparent colloidal sol, is taken out after vacuum impregnation 0.5h, is put into drying box and does
It is dry;
(13) it is put into Muffle furnace after taking out and roasts 5h at 500 DEG C up to foamed ceramics.
Embodiment 2
A kind of foamed ceramics, ingredient by weight, preparation method the following steps are included:
(1) by 23 parts of diatomite, 22 parts of kaolin, 12 parts of quartz, 7 parts of straw biological charcoals and 7 parts of α-Al2O3Micro mist mixing, grinds
It is milled to fineness < 0.1mm;
(2) plus water polo is milled to partial size≤2 μm, dries to obtain mixed powder;
(3) gelatin solution is added, prepares the slurry that total solid content is 42%, mixing and ball milling 7min, wherein gelatin is in mixed powder
In content be 22wt%;
(4) it by vacuum outgas after slurry magnetic agitation, injects in mold, is placed in sealing and curing 1h in 85 DEG C of thermostatic drying chambers;
(5) it is transferred in 50 DEG C of drying boxes and is demoulded after drying;
(6) it is placed in the autoclave of supercritical carbon dioxide foaming device, is first filled with low pressure CO 2 for air displacement in kettle
Completely, it is re-filled with high-pressure carbon dioxide, is swollen 15min at temperature 60 C, pressure 15MPa, the fast pressure relief in 2s;
(7) it is put into Muffle furnace, roasts 4h at 1320 DEG C of temperature;
(8) it is equably laid on the ground electrode in low-temperature plasma processing unit after cooling, in supply frequency 12kHz, work
12min is handled under the conditions of voltage 20kV, discharge power 75W must be modified foamed ceramics;
(9) 220 parts of Al (NO are taken3)3·9H2O and 620 part of distilled water stirring and dissolving, is put into water-bath, is returned at 90 DEG C
Stream heating is slowly added into 36 parts of aluminium powder reactions, and the pH value that solution is controlled in reaction process is 3.5;
(10) bottom gray precipitate is removed after being centrifugated, and obtains colorless and transparent colloidal sol;
(11) 22 parts of polyethylene glycol, 4 parts of lanthanum nitrates and 5 parts of barium nitrates, stirring and dissolving is added and obtains pale yellow transparent colloidal sol;
(12) modified foamed ceramics is immersed in pale yellow transparent colloidal sol, is taken out after vacuum impregnation 0.5h, is put into drying box and does
It is dry;
(13) it is put into Muffle furnace after taking out and roasts 5h at 600 DEG C up to foamed ceramics.
Embodiment 3
A kind of foamed ceramics, ingredient by weight, preparation method the following steps are included:
(1) by 25 parts of diatomite, 25 parts of kaolin, 15 parts of quartz, 8 parts of straw biological charcoals and 8 parts of α-Al2O3Micro mist mixing, grinds
It is milled to fineness < 0.1mm;
(2) plus water polo is milled to partial size≤2 μm, dries to obtain mixed powder;
(3) gelatin solution is added, prepares the slurry that total solid content is 43%, mixing and ball milling 8min, wherein gelatin is in mixed powder
In content be 25wt%;
(4) it by vacuum outgas after slurry magnetic agitation, injects in mold, is placed in sealing and curing 1h in 85 DEG C of thermostatic drying chambers;
(5) it is transferred in 50 DEG C of drying boxes and is demoulded after drying;
(6) it is placed in the autoclave of supercritical carbon dioxide foaming device, is first filled with low pressure CO 2 for air displacement in kettle
Completely, it is re-filled with high-pressure carbon dioxide, is swollen 15min at 65 DEG C of temperature, pressure 15MPa, the fast pressure relief in 2s;
(7) it is put into Muffle furnace, roasts 4h at 1330 DEG C of temperature;
(8) it is equably laid on the ground electrode in low-temperature plasma processing unit after cooling, in supply frequency 13kHz, work
13min is handled under the conditions of voltage 20kV, discharge power 75W must be modified foamed ceramics;
(9) 230 parts of Al (NO are taken3)3·9H2O and 630 part of distilled water stirring and dissolving, is put into water-bath, is returned at 90 DEG C
Stream heating is slowly added into 38 parts of aluminium powder reactions, and the pH value that solution is controlled in reaction process is 3.5;
(10) bottom gray precipitate is removed after being centrifugated, and obtains colorless and transparent colloidal sol;
(11) 23 parts of polyethylene glycol, 5 parts of lanthanum nitrates and 6 parts of barium nitrates, stirring and dissolving is added and obtains pale yellow transparent colloidal sol;
(12) modified foamed ceramics is immersed in pale yellow transparent colloidal sol, is taken out after vacuum impregnation 1h, is put into drying box dry;
(13) it is put into Muffle furnace after taking out and roasts 5h at 650 DEG C up to foamed ceramics.
Embodiment 4
A kind of foamed ceramics, ingredient by weight, preparation method the following steps are included:
(1) by 28 parts of diatomite, 28 parts of kaolin, 17 parts of quartz, 9 parts of straw biological charcoals and 9 parts of α-Al2O3Micro mist mixing, grinds
It is milled to fineness < 0.1mm;
(2) plus water polo is milled to partial size≤2 μm, dries to obtain mixed powder;
(3) gelatin solution is added, prepares the slurry that total solid content is 44%, mixing and ball milling 9min, wherein gelatin is in mixed powder
In content be 28wt%;
(4) it by vacuum outgas after slurry magnetic agitation, injects in mold, is placed in sealing and curing 1h in 85 DEG C of thermostatic drying chambers;
(5) it is transferred in 50 DEG C of drying boxes and is demoulded after drying;
(6) it is placed in the autoclave of supercritical carbon dioxide foaming device, is first filled with low pressure CO 2 for air displacement in kettle
Completely, it is re-filled with high-pressure carbon dioxide, is swollen 15min at temperature 70 C, pressure 17MPa, the fast pressure relief in 2s;
(7) it is put into Muffle furnace, roasts 4h at 1340 DEG C of temperature;
(8) it is equably laid on the ground electrode in low-temperature plasma processing unit after cooling, in supply frequency 14kHz, work
14min is handled under the conditions of voltage 20kV, discharge power 75W must be modified foamed ceramics;
(9) 240 parts of Al (NO are taken3)3·9H2O and 640 part of distilled water stirring and dissolving, is put into water-bath, is returned at 90 DEG C
Stream heating is slowly added into 39 parts of aluminium powder reactions, and the pH value that solution is controlled in reaction process is 4.0;
(10) bottom gray precipitate is removed after being centrifugated, and obtains colorless and transparent colloidal sol;
(11) 24 parts of polyethylene glycol, 5 parts of lanthanum nitrates and 7 parts of barium nitrates, stirring and dissolving is added and obtains pale yellow transparent colloidal sol;
(12) modified foamed ceramics is immersed in pale yellow transparent colloidal sol, is taken out after vacuum impregnation 1h, is put into drying box dry;
(13) it is put into Muffle furnace after taking out and roasts 5h at 700 DEG C up to foamed ceramics.
Embodiment 5
A kind of foamed ceramics, ingredient by weight, preparation method the following steps are included:
(1) by 30 parts of diatomite, 30 parts of kaolin, 20 parts of quartz, 10 parts of straw biological charcoals and 10 parts of α-Al2O3Micro mist mixing,
It is ground to fineness < 0.1mm;
(2) plus water polo is milled to partial size≤2 μm, dries to obtain mixed powder;
(3) gelatin solution is added, prepares the slurry that total solid content is 45%, mixing and ball milling 10min, wherein gelatin is in mixed powder
Content in material is 30wt%;
(4) it by vacuum outgas after slurry magnetic agitation, injects in mold, is placed in sealing and curing 1h in 85 DEG C of thermostatic drying chambers;
(5) it is transferred in 50 DEG C of drying boxes and is demoulded after drying;
(6) it is placed in the autoclave of supercritical carbon dioxide foaming device, is first filled with low pressure CO 2 for air displacement in kettle
Completely, it is re-filled with high-pressure carbon dioxide, is swollen 20min at 80 DEG C of temperature, pressure 20MPa, the fast pressure relief in 2s;
(7) it is put into Muffle furnace, roasts 4h at 1350 DEG C of temperature;
(8) it is equably laid on the ground electrode in low-temperature plasma processing unit after cooling, in supply frequency 15kHz, work
15min is handled under the conditions of voltage 20kV, discharge power 80W must be modified foamed ceramics;
(9) 250 parts of Al (NO are taken3)3·9H2O and 650 part of distilled water stirring and dissolving, is put into water-bath, is returned at 90 DEG C
Stream heating is slowly added into 40 parts of aluminium powder reactions, and the pH value that solution is controlled in reaction process is 4.0;
(10) bottom gray precipitate is removed after being centrifugated, and obtains colorless and transparent colloidal sol;
(11) 25 parts of polyethylene glycol, 6 parts of lanthanum nitrates and 8 parts of barium nitrates, stirring and dissolving is added and obtains pale yellow transparent colloidal sol;
(12) modified foamed ceramics is immersed in pale yellow transparent colloidal sol, is taken out after vacuum impregnation 1h, is put into drying box dry;
(13) it is put into Muffle furnace after taking out and roasts 5h at 800 DEG C up to foamed ceramics.
Foamed ceramics prepared by the present invention is carried out to the processing of sewage, the COD of sewage is 484mg/L, ammonia-nitrogen content 36.3mg/
L。
The performance indicator of the sewage after foamed ceramics is handled of table 1
Name of product | COD removal rate (%) | Ammonia nitrogen removal frank (%) |
Embodiment 1 | 96.3 | 91.2 |
Embodiment 2 | 96.7 | 91.7 |
Embodiment 3 | 97.2 | 92.1 |
Embodiment 4 | 96.8 | 91.9 |
Embodiment 5 | 96.2 | 91.5 |
Note: foamed ceramics usage amount is 3g/L
All there is extraordinary treatment effect for COD and ammonia nitrogen through foamed ceramics prepared by the present invention, after processing, COD and
The removal rate of ammonia nitrogen is all up to 97.2% and 92.1% respectively.
Claims (5)
1. a kind of foamed ceramics, it is characterised in that: ingredient by weight, preparation method the following steps are included:
(1) by diatomite, kaolin, quartz, straw biological charcoal and α-Al2O3Micro mist mixing, is ground to fineness < 0.1mm;
(2) plus water polo is milled to partial size≤2 μm, dries to obtain mixed powder;
(3) gelatin solution is added, prepares the slurry that total solid content is 40-45%, mixing and ball milling 5-10min;
(4) it by vacuum outgas after slurry magnetic agitation, injects in mold, is placed in sealing and curing 1h in 85 DEG C of thermostatic drying chambers;
(5) it is transferred in 50 DEG C of drying boxes and is demoulded after drying;
(6) it is placed in the autoclave of supercritical carbon dioxide foaming device, is first filled with low pressure CO 2 for air displacement in kettle
Completely, it is re-filled with high-pressure carbon dioxide, 10-20min is swollen at 50-80 DEG C of temperature, pressure 10-20MPa, is quickly unloaded in 2s
Pressure;
(7) it is put into Muffle furnace, roasts 4h at 1300-1350 DEG C of temperature;
(8) it is equably laid on the ground electrode in low-temperature plasma processing unit after cooling, in supply frequency 10-15kHz, work
Processing 10-15min must be modified foamed ceramics under the conditions of making voltage 20kV, discharge power 70-80W;
(9) 200-250 parts of Al (NO are taken3)3·9H2O and 600-650 parts of distilled water stirring and dissolving, is put into water-bath, at 90 DEG C
Under be heated at reflux, be slowly added into the reaction of 35-40 parts of aluminium powders, the pH value that solution is controlled in reaction process is 3.0-4.0;
(10) bottom gray precipitate is removed after being centrifugated, and obtains colorless and transparent colloidal sol;
(11) 20-25 parts of polyethylene glycol, 3-6 parts of lanthanum nitrates and 4-8 parts of barium nitrates are added, it is molten that stirring and dissolving obtains pale yellow transparent
Glue;
(12) modified foamed ceramics is immersed in pale yellow transparent colloidal sol, takes out, is put into drying box after vacuum impregnation 0.5-1h
It is dry;
(13) it is put into Muffle furnace after taking out and roasts 5h at 500-800 DEG C up to foamed ceramics.
2. a kind of foamed ceramics according to claim 1, it is characterised in that: gelatin is in mixed powder in the step (3)
In content be 20wt%-30wt%.
3. a kind of foamed ceramics according to claim 1, it is characterised in that: temperature is 65 DEG C, pressure in the step (6)
For 15MPa, swelling time 15min.
4. a kind of foamed ceramics according to claim 1, it is characterised in that: supply frequency is in the step (8)
13kHz, discharge power 75W.
5. the application of a kind of foamed ceramics described in -4 in the treatment of waste water according to claim 1.
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CN111170441A (en) * | 2020-01-19 | 2020-05-19 | 长沙凯天工研院环保服务有限公司 | Core-shell structure foam ceramic-based biofilm formation material, preparation thereof and application thereof in biofilm wastewater treatment |
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CN109574703A (en) * | 2018-11-17 | 2019-04-05 | 蒋吉平 | A kind of foamed ceramics and its application in the treatment of waste water |
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CN111170441A (en) * | 2020-01-19 | 2020-05-19 | 长沙凯天工研院环保服务有限公司 | Core-shell structure foam ceramic-based biofilm formation material, preparation thereof and application thereof in biofilm wastewater treatment |
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