CN106007720B - A kind of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics and preparation method - Google Patents
A kind of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics and preparation method Download PDFInfo
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Abstract
A kind of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics and preparation method; according to the mass fraction; 60~90 parts of silicon carbide micro-powder, 5~25 parts of zeroth order iron powder, 1~5 part of glass powder, carbon dust 3~20,1~8 part of graphite, 0.1~0.5 part of ethylene glycol, 0.1~0.5 part of ammonium polyacrylate, 2~10 parts of polyvinyl alcohol and water are uniformly mixed first; then mist projection granulating; remanufacture green body; finally under nitrogen protection; it is down to room temperature after being sintered 1 hour at 1350~1400 DEG C, obtains sewage disposal silicon carbide compound Zero-valent Iron porous ceramics.Ceramic Composite Zero-valent Iron, Zero-valent Iron is due to having many advantages, such as less toxic, cheap, easy to operate and environmentally friendly not will produce secondary pollution.Present invention process is simple, of low cost, is produced on a large scale and is applied to actual sewage processing item, overcome in the prior art treatment effect unobvious, be not thorough, cause the problem of secondary pollution.
Description
Technical field
The invention belongs to environment-friendly materials preparing technical fields, and it is porous to be related to a kind of sewage disposal silicon carbide compound Zero-valent Iron
Ceramics and preparation method.
Background technology
Silicon carbide has the characteristics that low-density, high intensity, anticorrosive, anti-oxidant, good thermal conductivity, high temperature resistant, zeroth order
Iron, which can be relatively easy to, loses electronics, has good reproducibility.Two kinds of Material claddings, which are formed in a kind of internal structure, to be had very
After mushy new function material, wide application can be obtained in sewage treatment field.
Prepare carborundum porous ceramics have kinds of processes method, including fiber draw technique, Foam dipping method,
Chemical deposition process etc., but these methods are more complicated, it is not easy to extensive progress industrialized production is carried out, cost is higher.
Traditional wastewater processing and contaminated soil processing, need the series such as filtering, neutralization reaction, resin adsorption, chemical settling multiple
Miscellaneous process, heavy workload, treatment effect unobvious are not thorough, or even cause secondary pollution,
Invention content
The purpose of the present invention is to provide a kind of sewage disposal preparation method of silicon carbide compound Zero-valent Iron porous ceramics,
This method is simple for process, can be carried out continuously industrialized production, at low cost.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics first will according to the mass fraction
60~90 parts of silicon carbide micro-powder, 5~25 parts of zeroth order iron powder, 1~5 part of glass powder, carbon dust 3~20,1~8 part of graphite, ethylene glycol
0.1~0.5 part, 0.1~0.5 part of ammonium polyacrylate, 2~10 parts of polyvinyl alcohol and water are uniformly mixed, then mist projection granulating, then
Manufacture green body is finally under nitrogen protection down to room temperature after being sintered 1 hour at 1350~1400 DEG C, obtains sewage disposal use
Silicon carbide compound Zero-valent Iron porous ceramics.
The mass ratio of water and silicon carbide micro-powder is 1:1.
Being uniformly mixed is realized by ball milling in the ball mill.
Ball-milling Time is 48 hours.
It is warming up to 1350~1400 DEG C with the heating rate of 2 DEG C/min.
Sintering carries out in vacuum sintering furnace.
When mist projection granulating, inlet temperature is 200~230 DEG C, and outlet temperature is 180~200 DEG C.
Manufacture green body is carried out at 200MPa.
A kind of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics, carbon in the silicon carbide compound Zero-valent Iron porous ceramics
SiClx mass percent is 50%~90%, and Zero-valent Iron mass percent is 5%~25%, and porosity is 5%~70%.
Compared with prior art, beneficial effects of the present invention：The present invention is with silicon carbide micro-powder, zeroth order iron powder, glass powder, carbon
Powder, graphite, ethylene glycol, polyvinyl alcohol and water are principle, and it is porous to be sintered preparation silicon carbide compound Zero-valent Iron using normal-pressure vacuum
Ceramics, the porous ceramics are equipped with high-activity biological catalyst carbon SiClx, since the excellent absorption of silicon carbide in liquid medium is micro-
Wave performance, orientation cause high energy consumption, in addition the ceramics so that catalyst temperature raising without whole heated waste water or contaminated soil
It is compounded with Zero-valent Iron, Zero-valent Iron is due to having less toxic, cheap, easy to operate and environmentally friendly not will produce secondary pollution etc. excellent
Point.And since Zero-valent Iron chemical property is active, electronegativity is very big, and electrode potential is -0.44V, has stronger reducing power,
Row in metal activity series table can be come out and be deposited on iron surface in metal replacement thereafter, it can also be stronger by oxidisability
Ion or compound and the reduction of certain organic matters, so making it in water pollution control using more and more extensive.Present invention process
Simply, of low cost, it is produced on a large scale and is applied to actual sewage processing item, overcome in the prior art that treatment effect is not
Obviously, it is not thorough, causes the problem of secondary pollution.
Silicon carbide accounting 50%~90% (mass percent) in the composite material of the present invention, Zero-valent Iron accounting 5%~
25% (mass percent), porosity are 5%~70%.
Specific implementation mode
Below by specific embodiment to the present invention will be described.
Embodiment 1
By deionized water 100Kg, silicon carbide micro-powder 100Kg, zeroth order iron powder 10Kg, glass powder 2Kg, carbon dust 5Kg, graphite
5Kg, ethylene glycol 500mL, polyvinyl alcohol 3.5Kg, polyacrylic acid aqueous ammonium (mass fraction 20%) 600mL are put into ball mill
Middle ball milling 48 hours, filtering, mist projection granulating (inlet temperature is 200~230 DEG C, and outlet temperature is 180~200 DEG C) are used
200MPa press pressing blanks, are put into vacuum sintering furnace, while being passed through high-purity argon gas, gradually with the heating rate of 2 DEG C/min
1350 DEG C are warming up to, and room temperature is down to after being kept for 1 hour, it is porous to ultimately form the silicon carbide compound Zero-valent Iron that porosity is 35%
Ceramics.
Embodiment 2
By deionized water 150Kg, silicon carbide micro-powder 150Kg, zeroth order iron powder 10Kg, glass powder 3Kg, carbon dust 10Kg, graphite
15Kg, ethylene glycol 750mL, polyvinyl alcohol 10Kg, polyacrylic acid aqueous ammonium (mass fraction 20%) 950mL are put into ball mill
Middle ball milling 48 hours, filtering, mist projection granulating is put into 200MPa press pressing blanks in vacuum sintering furnace, while being passed through high-purity
Argon gas is gradually warming up to 1350 DEG C with the heating rate of 2 DEG C/min, and is down to room temperature after being kept for 1 hour, ultimately forms porosity
For 45% silicon carbide compound Zero-valent Iron porous ceramics.
Embodiment 3
By deionized water 150Kg, silicon carbide micro-powder 150Kg, zeroth order iron powder 15Kg, glass powder 5Kg, carbon dust 10Kg, graphite
10Kg, ethylene glycol 800mL, polyvinyl alcohol 12Kg, polyacrylic acid aqueous ammonium (mass fraction 20%) 1000mL are put into ball milling
Ball milling 48 hours in machine, filtering, mist projection granulating are put into vacuum sintering furnace, while being passed through height with 200MPa press pressing blanks
Pure argon is gradually warming up to 1350 DEG C with the heating rate of 2 DEG C/min, and is down to room temperature after being kept for 1 hour, ultimately forms hole
The silicon carbide compound Zero-valent Iron porous ceramics that rate is 57%.
Embodiment 4
According to the mass fraction, first by 80 parts of silicon carbide micro-powder, 5 parts of zeroth order iron powder, 5 parts of glass powder, 15 parts of carbon dust, graphite
1 part, 0.1 part of ethylene glycol, mass fraction be 20% polyacrylic acid aqueous ammonium (in polyacrylic acid aqueous ammonium contain 0.5 part
Ammonium polyacrylate), 80 parts of 2 parts of polyvinyl alcohol and deionized water ball milling 48h in the ball mill, be uniformly mixed, then spray
It is granulated, inlet temperature is 200 DEG C when mist projection granulating, and outlet temperature is 200 DEG C；Green body is manufactured under 200MPa, finally in nitrogen
Under gas shielded, after being warming up to 1350 DEG C with the heating rate of 2 DEG C/min in vacuum sintering furnace and being sintered 1 hour at such a temperature
It is down to room temperature, obtains sewage disposal silicon carbide compound Zero-valent Iron porous ceramics.The porosity of the ceramics is 5%.
Embodiment 5
According to the mass fraction, first by 90 parts of silicon carbide micro-powder, 12 parts of zeroth order iron powder, 1 part of glass powder, 20 parts of carbon dust, stone
3 parts of ink, 0.2 part of ethylene glycol, the polyacrylic acid aqueous ammonium that mass fraction is 20% (contain 0.4 in polyacrylic acid aqueous ammonium
Part ammonium polyacrylate), 60 parts of 4 parts of polyvinyl alcohol and deionized water ball milling 48h in the ball mill, be uniformly mixed, then spray
Mist is granulated, and inlet temperature is 210 DEG C when mist projection granulating, and outlet temperature is 190 DEG C；Green body is manufactured under 200MPa, is finally existed
Under nitrogen protection, 1400 DEG C are warming up to the heating rate of 2 DEG C/min in vacuum sintering furnace and be sintered 1 hour at such a temperature
After be down to room temperature, obtain sewage disposal silicon carbide compound Zero-valent Iron porous ceramics.The porosity of the ceramics is 70%.
Embodiment 6
According to the mass fraction, first by 60 parts of silicon carbide micro-powder, 25 parts of zeroth order iron powder, 2 parts of glass powder, 9 parts of carbon dust, graphite
5 parts, 0.4 part of ethylene glycol, mass fraction be 20% polyacrylic acid aqueous ammonium (in polyacrylic acid aqueous ammonium contain 0.3 part
Ammonium polyacrylate), 90 parts of 7 parts of polyvinyl alcohol and deionized water ball milling 48h in the ball mill, be uniformly mixed, then spray
It is granulated, inlet temperature is 220 DEG C when mist projection granulating, and outlet temperature is 180 DEG C；Green body is manufactured under 200MPa, finally in nitrogen
Under gas shielded, after being warming up to 1360 DEG C with the heating rate of 2 DEG C/min in vacuum sintering furnace and being sintered 1 hour at such a temperature
It is down to room temperature, obtains sewage disposal silicon carbide compound Zero-valent Iron porous ceramics.The porosity of the ceramics is 20%.
Embodiment 7
According to the mass fraction, first by 70 parts of silicon carbide micro-powder, 3 parts of zeroth order iron powder, 4 parts of glass powder, 20 parts of carbon dust, graphite
8 parts, 0.5 part of ethylene glycol, mass fraction be 20% polyacrylic acid aqueous ammonium (in polyacrylic acid aqueous ammonium contain 0.1 part
Ammonium polyacrylate), 70 parts of 10 parts of polyvinyl alcohol and deionized water ball milling 48h in the ball mill, be uniformly mixed, then spray
It is granulated, inlet temperature is 230 DEG C when mist projection granulating, and outlet temperature is 185 DEG C；Green body is manufactured under 200MPa, finally in nitrogen
Under gas shielded, after being warming up to 1380 DEG C with the heating rate of 2 DEG C/min in vacuum sintering furnace and being sintered 1 hour at such a temperature
It is down to room temperature, obtains sewage disposal silicon carbide compound Zero-valent Iron porous ceramics.The porosity of the ceramics is 55%.
Sewage disposal prepared by the present invention is with silicon carbide mass percent in silicon carbide compound Zero-valent Iron porous ceramics
50%~90%, Zero-valent Iron mass percent is 5%~25%, and porosity is 5%~70%.
The invention discloses a kind of sewage disposal preparation methods of silicon carbide compound Zero-valent Iron ceramics, including following step
Suddenly：First by deionized water, silicon carbide micro-powder, zeroth order iron powder, glass powder, carbon dust, graphite, ethylene glycol, polyvinyl alcohol, polypropylene
Sour ammonium is put into ball milling 48 hours in ball mill, filtering, mist projection granulating, and green body makes, is put into vacuum sintering furnace, while being passed through height
Pure argon is gradually warming up to 1350~1400 DEG C with the warm rate of 2 DEG C/min, and is down to room temperature after being kept for 1 hour, ultimately forms
Silicon carbide compound Zero-valent Iron porous ceramics.This method is simple for process, can continuous industrial production.
For traditional wastewater processing and contaminated soil processing, filtering, neutralization reaction, resin adsorption, chemical settling etc. is needed to be
Row complex process, heavy workload, treatment effect unobvious, the problem of being not thorough, or even cause secondary pollution, the present invention is using normal
It presses vacuum-sintering to prepare silicon carbide compound Zero-valent Iron porous ceramics, high-activity biological catalyst is carried, due to carbon in liquid medium
The excellent absorption microwave property of SiClx, orientation cause so that catalyst temperature raising without whole heated waste water or contaminated soil
High energy consumption, other Ceramic Composite Zero-valent Iron, Zero-valent Iron due to have it is less toxic, cheap, easy to operate and also it is environmentally friendly not
The advantages that will produce secondary pollution.It is set to be applied in water pollution control more and more extensive, Zero-valent Iron chemical property is active.Electricity is negative
Property is very big.Electrode potential Eo (Fe2+/Fe)=- 0.44V has stronger reducing power, can will be arranged in metal activity series table
Metal replacement in thereafter comes out and is deposited on iron surface, can also be by the stronger ion of oxidisability or compound and certain organic
Object restores.Simple process and low cost is honest and clean, is produced on a large scale and is applied to actual sewage processing item.
Claims (7)
1. a kind of sewage disposal preparation method of silicon carbide compound Zero-valent Iron porous ceramics, which is characterized in that press mass fraction
Meter, first by 60~90 parts of silicon carbide micro-powder, 5~25 parts of zeroth order iron powder, 1~5 part of glass powder, 3~20 parts of carbon dust, graphite 1~8
Part, 0.1~0.5 part of ethylene glycol, 0.1~0.5 part of ammonium polyacrylate, 2~10 parts of polyvinyl alcohol and water are uniformly mixed, and are then sprayed
Mist is granulated, and is remanufactured green body, finally under nitrogen protection, is warming up to 1350~1400 DEG C with the heating rate of 2 DEG C/min and burns
Knot is down to room temperature after 1 hour, obtains sewage disposal silicon carbide compound Zero-valent Iron porous ceramics；Wherein, water and silicon carbide micro-powder
Mass ratio be 1:1.
2. a kind of preparation method of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics according to claim 1,
It is characterized in that, being uniformly mixed is realized by ball milling in the ball mill.
3. a kind of preparation method of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics according to claim 2,
It is characterized in that, Ball-milling Time is 48 hours.
4. a kind of preparation method of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics according to claim 1,
It is characterized in that, sintering carries out in vacuum sintering furnace.
5. a kind of preparation method of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics according to claim 1,
It is characterized in that, when mist projection granulating, inlet temperature is 200~230 DEG C, and outlet temperature is 180~200 DEG C.
6. a kind of preparation method of sewage disposal silicon carbide compound Zero-valent Iron porous ceramics according to claim 1,
It is characterized in that, manufacture green body is carried out at 200MPa.
7. sewage disposal silicon carbide compound Zero-valent Iron porous ceramics prepared by a kind of method according to claim 1, special
Sign is that silicon carbide mass percent is 50%~90% in the silicon carbide compound Zero-valent Iron porous ceramics, zeroth order weight of iron hundred
Score is 5%~25%, and porosity is 5%~70%.
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| CN109304470B (en) * | 2017-07-28 | 2020-07-10 | 华中科技大学 | Surface-modified amorphous zero-valent iron, and preparation method and application thereof |
| CN107963907B (en) * | 2017-11-21 | 2020-10-16 | 浙江师范大学 | Sintered porous ceramic sheet for sewage treatment and preparation method thereof |
| CN110937900B (en) * | 2018-09-25 | 2022-04-26 | 陕西固勤材料技术有限公司 | Preparation method of large-size reaction sintered silicon carbide ceramic plate |
| CN109592762A (en) * | 2019-02-01 | 2019-04-09 | 何美英 | A kind of eutrophication water inorganic agent and preparation method thereof |
| CN109589927B (en) * | 2019-02-01 | 2022-02-15 | 广州市中绿环保有限公司 | Printing and dyeing wastewater adsorption treatment agent and preparation method thereof |
| CN110423136A (en) * | 2019-09-06 | 2019-11-08 | 东莞精陶科技有限公司 | The prilling process of porous ceramics |
| CN114436676A (en) * | 2022-01-29 | 2022-05-06 | 深圳市中科纳米科技有限公司 | Production method of carbon nano tube composite porous ceramic capable of adsorbing toxic substances |
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| CN101323524A (en) * | 2008-04-15 | 2008-12-17 | 西安交通大学 | Preparation of oriented hole silicon carbide porous ceramic |
| CN102295458A (en) * | 2011-06-10 | 2011-12-28 | 江苏大阳光辅股份有限公司 | Preparation method of reaction sinteredsilicon carbide ceramic |
| CN102718544A (en) * | 2012-06-18 | 2012-10-10 | 北京大学 | Ceramsite for heavy metal wastewater treatment, preparation method and applications thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101323524A (en) * | 2008-04-15 | 2008-12-17 | 西安交通大学 | Preparation of oriented hole silicon carbide porous ceramic |
| CN102295458A (en) * | 2011-06-10 | 2011-12-28 | 江苏大阳光辅股份有限公司 | Preparation method of reaction sinteredsilicon carbide ceramic |
| CN102718544A (en) * | 2012-06-18 | 2012-10-10 | 北京大学 | Ceramsite for heavy metal wastewater treatment, preparation method and applications thereof |
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