CN103768869A - Composite active carbon ultrafiltration element and preparation method thereof - Google Patents
Composite active carbon ultrafiltration element and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a composite active carbon ultrafiltration element and preparation method of the composite active carbon ultrafiltration element, and relates to water purification. The filter element comprises the following components in parts by weight: 50-65 parts of active carbon, 5-10 parts of diatomite, 29.8-35 parts of kaolin, 0.1-0.5 part of an antibacterial agent, 0-3 of a metal ion additive and 0.1-1.5 parts of graphene microchip. The preparation method comprises the following steps: placing the graphene microchip in N-methyl pyrrolidone aqueous solution to be dispersed into 2-25g/L graphene microchip dispersion liquid; ball-milling the diatomite, the kaolin, the active carbon, the antibacterial agent, the metal ion additive and the graphene microchip dispersion liquid, taking out the slurry, curing to obtain the slurry for slip casting, pouring into a cavity of a plaster mold, pouring out the non-adsorbed flowing slurry to obtain a hollow filter element blank body after the thickness of the blank body adsorbed on the inner wall of the plaster mold is 8-15mm, taking out the filter element blank body from the plaster mold to obtain a filter element green body after degassing, drying, sintering, reducing and cooling to obtain the composite active carbon ultrafiltration element.
Description
Technical field
The present invention relates to water and purify, especially relate to a kind of composite activated carbon ultra-filtration element and preparation method thereof.
Background technology
The rare carbon atom of being arranged by one deck two dimensional surface of graphite forms, and wherein carbon atom connects with sp2 hydridization, is monatomic carbon-coating because graphite is rare, and therefore it has great specific area, and its theoretical value can reach 2600m
2/ g, it has very high absorption property and special efficacy.
At present, no matter be the active carbon stick filter core that adopts extrusion moulding or sinter molding to prepare, except it has excellent physical absorption effect, its filtering accuracy is generally all at 0.5～10 μ m.Accomplish that filtering accuracy is at 0.05～0.1 μ m, said method all cannot be realized.
Chinese patent 201210437472 is open a kind of containing multi-walled carbon nano-tubes, low-temperature sintering, high-intensity diatomite base composite ceramic filter core and preparation method thereof, this composite ceramic filter core is made up of following mass fraction raw material: 60～80 parts of terra silicea purificatas, 12～20 parts of active carbons, 4.5～9 parts of dispersants, 2～6 parts of sintering aids, 1～3 part of antiseptic, 0.5～2 part of CNT.The carbon nanotubes low-temperature sintering high strength diatomite base composite ceramic filter core of this invention, because of its inner equally distributed multi-walled carbon nano-tubes, can improve the mechanical performance of ceramic element; Meanwhile, multi-walled carbon nano-tubes has meso-hole structure, effectively heavy metal ion in Adsorption water.In addition, reduce sintering temperature (<950 ℃) by adding micron order metallic aluminium powder, retain diatomite natural nano micropore, and further improved the mechanical strength (compression strength >0.5GPa) of ceramic element.
Chinese patent 201310255456 discloses a kind of composite ceramic filter core and preparation method thereof, and diatomite 12～14, active carbon 36～38, CNT 2～3, silver nitrate 1～2, Coconut Fatty Acid Monoethanolamide 4～5, sodium metasilicate 7～9, propane diols 8～10, starch 3～5, carbonic hydroammonium 3～4, modified alta-mud 20～25, water are appropriate.The carbon nanotubes of this invention, can improve the mechanical performance of ceramic element; Meanwhile, multi-walled carbon nano-tubes has meso-hole structure, effectively heavy metal ion in Adsorption water.This invention can for the air filtration of air handling system, also can be for water filtration, can also be used for the air-breathing filtration of automobile filter, be applicable to the severe place of various environment.
Chinese patent 201310255348 discloses a kind of carbon crystal compound micropore ceramic filter element and preparation method thereof, is made up of the raw material of following weight portion: precipitated calcium carbonate 12～14, kaolin 9～12, diatomite 7～9, bamboo charcoal powder 10～12, charcoal powder 4～6, stalk ashes 1～2, celestite powder 12～14, talcum powder 6～8, mica powder 3～5, chlorinated paraffin wax 10～12, ethanol 12～14, modified alta-mud 25～35, water are appropriate.
Chinese patent 200810006710 discloses a kind of carbon crystal compound micropore ceramic filter element and preparation method thereof, this carbon crystal compound micropore ceramic filter element is take diatomite and powdered carbon as main component, add after the other materials such as precipitated calcium carbonate, kaolin mix and blend, through slip casting or pressed compact moulding, the carbon crystal compound micropore ceramic filter element that sintering forms under reducing atmosphere, finished form can be tubulose, the shape such as tabular, hemispherical.This micropore ceramic filter element is mainly used in water treatment facilities or other filter plants; There is the several functions such as filtration, absorption and anti-bacteria breeding simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of composite activated carbon ultra-filtration element of graphene-containing microplate, high filtering precision and preparation method thereof.Utilize the special absorption property of Graphene, its surface area reaches 2600m
2/ g, and the control technology of the antibiotic and sterilizing ability of Nano Silver excellence and ultrafiltration level filtering accuracy, and obtain a kind of novel composite activated carbon ultra-filtration element, it is very effective to toxic heavy metal ion remavals such as organic matter, bacterium and lead.
Described composite activated carbon ultra-filtration element is made up of following mass fraction raw material: 50～65 parts of active carbons, 5～10 parts, diatomite, 29.8～35 parts of kaolin, 0.1～0.5 part of antiseptic, 0～3 part of metal ions addition agent, 0.1～1.5 part of Graphene microplate.
The average grain particle diameter of described active carbon raw material is 10～16 μ m, specific area BET value >1100～1500m
2/ g, iodine number is 600～1000mg/g.
The average grain particle diameter of described diatomite material is 6～10 μ m, and the average grain particle diameter of described kaolin raw material is 2～5 μ m.
Described antiseptic can adopt silver nitrate etc., and described metal ions addition agent can adopt ferric nitrate or iron chloride etc.Described Graphene microplate raw thickness is 80～100nm, and average microplate diameter is 8 μ m.
Described composite activated carbon ultra-filtration element preparation method, comprises the following steps:
1) dispersion of Graphene microplate: it is the Graphene microplate dispersion liquid that 10% 1-METHYLPYRROLIDONE aqueous solution ultrasonic wave is separated into 2～25g/L that Graphene microplate is put into volume by volume concentration;
2) preparation of the slurry that injection forming is used: by after diatomite, kaolin, active carbon, antiseptic, metal ions addition agent and Graphene microplate dispersion liquid ball milling, take out slurry, obtain the slurry that injection forming is used after slaking;
3) injection forming and the demoulding: the slurry that injection forming is used is poured in the die cavity of plaster mold, after being 8～15mm at the idiosome thickness of plaster mold inwall absorption, pour out the not mobile slurry of absorption in plaster mold, obtain hollow filter core idiosome, by after degassed plaster mold processing, filter core idiosome is deviate from plaster mold, obtained composite activated carbon ultra-filtration element green compact;
4) composite activated carbon ultra-filtration element green compact are dried and sintering: composite activated carbon ultra-filtration element green compact are dry, after sintering and reducing, take out with stove cool to room temperature, and must be loaded with the composite activated carbon ultra-filtration element of Nano Silver, Nanoscale Iron.
In step 2) in, described ball milling can adopt planetary Universal ball grinding machine ball milling, diatomite, kaolin, active carbon, antiseptic and the gross mass of Graphene microplate dispersion liquid and the mass ratio of abrading-ball can be 1: 3, described abrading-ball can be made up of two kinds of different-grain diameter Ceramic Balls, wherein a kind of diameter of Ceramic Balls is 1mm, the diameter of another kind of Ceramic Balls is 2mm, diameter is that the mass ratio of 1mm Ceramic Balls and 2mm Ceramic Balls is (1～3): 1, the rotating speed of ball milling can be 1000～3000rpm, and the time of ball milling can be 8～16h; Described slaking can adopt static slaking 12～24h.
In step 3), described degassed processing can be inverted into plaster mold in the vacuum tank that vacuum is 10kPa, the degassed processing of static 2～4h.
In step 4), described dry temperature can be 102～108 ℃, and the dry time can be 12～24h; The method of described sintering and reducing can be put into vacuum reaction sintering stove by dried composite activated carbon ultra-filtration element green compact, sintering and reducing in the atmosphere of nitrogen and hydrogen, heat up according to the speed of 4～6 ℃/min, the temperature of sintering is 850～920 ℃, and the time of sintering is 1.5～3h.
Composite activated carbon ultra-filtration element prepared by the present invention carries out the clearance of mark-on test test to chlorine residue according to " GB5750-2006 drinking water standard method of inspection " standard, to plumbous clearance, adopt multi-functional aperture analyzer PSDA-20 type to carry out pore size measurement to it.Compared with prior art, the present invention has following advantages:
1, can remove efficiently, fast the heavy metal ion such as organic pollutants, DBPs, chlorine residue and lead ion, can reach 100% by the test of standard mark-on to the clearance of chlorine residue, lead ion clearance reaches 95%.
2, there is sterilization and bacteria resistance function, effectively sterilization; Meanwhile, because its filtering accuracy is high, average pore size is 0.08 μ m, therefore can tackle bacterium and virus completely.
The specific embodiment
Embodiment 1
1) dispersion of Graphene microplate: be 80～100nm by thickness, average microplate diameter is that 8 μ m Graphene microplate 15g put into the Graphene microplate dispersion liquid that volume by volume concentration is 10% the ultrasonic 25g/L of being separated into of 1-METHYLPYRROLIDONE aqueous solution 0.6L.
2) preparation of the slurry that injection forming is used: be 10 μ m active carbon 500g by average grain particle diameter, average grain particle diameter is 6 μ m diatomite 100g, average grain particle diameter is 2 μ m kaolin 350g, silver nitrate 5g, the dispersion liquid of ferric nitrate 30g and above-mentioned Graphene microplate, put into planetary Universal ball grinding machine and carry out ball milling, the mass ratio of material and abrading-ball is 1: 3, abrading-ball is made up of two kinds of different-grain diameter Ceramic Balls, wherein a kind of diameter of Ceramic Balls is 1mm, the diameter of another kind of rotating speed Ceramic Balls is 2mm, diameter is that the mass ratio of 1mm Ceramic Balls and 2mm Ceramic Balls is 3: 1.Rotational speed of ball-mill is 3000rpm, and Ball-milling Time is 8h, takes out slurry, and static slaking 24h obtains the slurry that injection forming is used.
3) injection forming and the demoulding: the slurry after slaking is poured in the die cavity of plaster mold, after being 15mm at the idiosome thickness of plaster mold inwall absorption, pour out the not mobile slurry of absorption in plaster mold, obtain hollow filter core idiosome, plaster mold is inverted in the vacuum tank that vacuum is 10kPa, the degassed processing of static 4h is deviate from filter core idiosome in plaster mold, obtains composite activated carbon ultra-filtration element green compact.
4) composite activated carbon ultra-filtration element green compact are dried and sintering: by composite activated carbon ultra-filtration element green compact dry 24h at 108 ℃, dried green compact are placed in vacuum reaction sintering stove, sintering and reducing in the atmosphere of nitrogen and hydrogen, heat up according to the speed of 4 ℃/min, sintering temperature is 920 ℃, after sintering time is 1.5h, take out with stove cool to room temperature.Can obtain the composite activated carbon ultra-filtration element that is loaded with Nano Silver, Nanoscale Iron.
The Compound Ultrafiltration filter core obtaining carries out the clearance of mark-on test test to chlorine residue according to " GB5750-2006 drinking water standard method of inspection " standard, to plumbous clearance, adopts multi-functional aperture analyzer PSDA-20 type to carry out pore size measurement to it.Test by standard mark-on, lead ion clearance reaches 95.6%, chlorine residue clearance 100%.Multi-functional aperture analyzer PSDA-20 test result shows, the average pore size of composite activated carbon ultra-filtration element is 0.08 μ m.Chlorine residue performance test data is referring to table 1.
Table 1
| Chlorine residue life test | Initial concentration (mg/L) | Concentration (mg/L) after filter | Clearance (%) |
| After water flowing 5min | 2.36 | 0 | 100 |
| After water flowing 5t | 2.43 | 0 | 100 |
| After water flowing 10t | 2.84 | 0.02 | 99.1 |
| After water flowing 15t | 2.23 | 0.04 | 98.4 |
| After water flowing 20t | 2.59 | 0.13 | 94.9 |
Lead ion mark-on clearance is referring to table 2.
Table 2
Embodiment 2
1) dispersion of Graphene microplate: be 80～100nm by thickness, average microplate diameter is that to put into volume by volume concentration be the Graphene microplate dispersion liquid that 10% 1-METHYLPYRROLIDONE aqueous solution 0.5L ultrasonic wave is separated into 2g/L to 8 μ m Graphene microplate 1g.
2) preparation of the slurry that injection forming is used: be 16 μ m active carbon 650g by average grain particle diameter, average grain particle diameter is 10 μ m diatomite 50g, average grain particle diameter is 5 μ m kaolin 298g, silver nitrate 1g, dispersion liquid with above-mentioned Graphene microplate, put into planetary Universal ball grinding machine and carry out ball milling, the mass ratio of material and abrading-ball is 1: 3, abrading-ball is made up of two kinds of different-grain diameter Ceramic Balls, wherein a kind of diameter of Ceramic Balls is 1mm, the diameter of another kind of rotating speed Ceramic Balls is 2mm, and diameter is that the mass ratio of 1mm Ceramic Balls and 2mm Ceramic Balls is 1: 1.Rotational speed of ball-mill is 1000rpm, and Ball-milling Time is 16h, takes out slurry, and static slaking 12h obtains the slurry that injection forming is used.
3) injection forming and the demoulding: the slurry after slaking is poured in the die cavity of plaster mold, after being 8mm at the idiosome thickness of plaster mold inwall absorption, pour out the not mobile slurry of absorption in plaster mold, obtain hollow filter core idiosome, plaster mold is inverted in the vacuum tank that vacuum is 10kPa, the degassed processing of static 2h is deviate from filter core idiosome in plaster mold, obtains composite activated carbon ultra-filtration element green compact.
4) composite activated carbon ultra-filtration element green compact are dried and sintering: by composite activated carbon ultra-filtration element green compact dry 12h at 102 ℃, dried green compact are placed in vacuum reaction sintering stove, sintering and reducing in the atmosphere of nitrogen and hydrogen, heat up according to the speed of 6 ℃/min, sintering temperature is 850 ℃, after sintering time is 3h, take out with stove cool to room temperature.Can obtain the composite activated carbon ultra-filtration element that is loaded with Nano Silver, Nanoscale Iron.
The Compound Ultrafiltration filter core obtaining carries out the clearance of mark-on test test to chlorine residue according to " GB5750-2006 drinking water standard method of inspection " standard, to plumbous clearance, adopts multi-functional aperture analyzer PSDA-20 type to carry out pore size measurement to it.Test by standard mark-on, lead ion clearance reaches 93.8%, chlorine residue clearance 100%.Multi-functional aperture analyzer PSDA-20 test result shows, the average pore size of composite activated carbon ultra-filtration element is 0.15 μ m.Chlorine residue performance test data is referring to table 3.
Table 3
Lead ion mark-on clearance is referring to table 4.
Table 4
Embodiment 3
1) Graphene microplate disperses: be 80～100nm by thickness, average microplate diameter is that to put into volume by volume concentration be the Graphene microplate dispersion liquid that 10% 1-METHYLPYRROLIDONE aqueous solution 0.5L ultrasonic wave is separated into 16g/L to 8 μ m Graphene microplate 8g.
2) preparation of the slurry that injection forming is used: be 13 μ m active carbon 600g by average grain particle diameter, average grain particle diameter is 8 μ m diatomite 60g, average grain particle diameter is 5 μ m kaolin 310g, silver nitrate 3g, the dispersion liquid of iron chloride 19g and above-mentioned Graphene microplate, put into planetary Universal ball grinding machine and carry out ball milling, the mass ratio of material and abrading-ball is 1: 3, abrading-ball is made up of two kinds of different-grain diameter Ceramic Balls, wherein a kind of diameter of Ceramic Balls is 1mm, the diameter of another kind of rotating speed Ceramic Balls is 2mm, diameter is that the mass ratio of 1mm Ceramic Balls and 2mm Ceramic Balls is 2: 1.Rotational speed of ball-mill is 2000rpm, and Ball-milling Time is 12h, takes out slurry, and static slaking 16h obtains the slurry that injection forming is used.
3) injection forming and the demoulding: the slurry after slaking is poured in the die cavity of plaster mold, after being 10mm at the idiosome thickness of plaster mold inwall absorption, pour out the not mobile slurry of absorption in plaster mold, obtain hollow filter core idiosome, plaster mold is inverted in the vacuum tank that vacuum is 10kPa, the degassed processing of static 3h is deviate from filter core idiosome in plaster mold, obtains composite activated carbon ultra-filtration element green compact.
4) composite activated carbon ultra-filtration element green compact are dried and sintering: by composite activated carbon ultra-filtration element green compact dry 15h at 105 ℃, dried green compact are placed in vacuum reaction sintering stove, sintering and reducing in the atmosphere of nitrogen and hydrogen, heat up according to the speed of 5 ℃/min, sintering temperature is 910 ℃, after sintering time is 2.5h, take out with stove cool to room temperature.Can obtain the composite activated carbon ultra-filtration element that is loaded with Nano Silver, Nanoscale Iron.
The Compound Ultrafiltration filter core obtaining carries out the clearance of mark-on test test to chlorine residue according to " GB5750-2006 drinking water standard method of inspection " standard, to plumbous clearance, adopts multi-functional aperture analyzer PSDA-20 type to carry out pore size measurement to it.Test by standard mark-on, lead ion clearance reaches 94.8%, chlorine residue clearance 100%.Multi-functional aperture analyzer PSDA-20 test result shows, the average pore size of composite activated carbon ultra-filtration element is 0.11 μ m.
Table 5
Table 6
Chlorine residue performance test data is referring to table 5, and lead ion mark-on clearance is referring to table 6.
Claims (10)
1. a composite activated carbon ultra-filtration element, is characterized in that its raw material composition with quality than content is: active carbon 50～65, diatomite 5～10, kaolin 29.8～35, antiseptic 0.1～0.5, metal ions addition agent 0～3, Graphene microplate 0.1～1.5.
2. a kind of composite activated carbon ultra-filtration element as claimed in claim 1, the average grain particle diameter that it is characterized in that described active carbon is 10～16 μ m, specific area BET value is 1100～1500m
2/ g, iodine number is 600～1000mg/g.
3. a kind of composite activated carbon ultra-filtration element as claimed in claim 1, is characterized in that described diatomaceous average grain particle diameter is 6～10 μ m, and described kaolinic average grain particle diameter is 2～5 μ m.
4. a kind of composite activated carbon ultra-filtration element as claimed in claim 1, is characterized in that described antiseptic adopts silver nitrate, and described metal ions addition agent can adopt ferric nitrate or iron chloride; Described Graphene microplate thickness is 80～100nm, and average microplate diameter is 8 μ m.
5. as the preparation method of composite activated carbon ultra-filtration element as described in arbitrary in claim 1～4, it is characterized in that comprising the following steps:
1) dispersion of Graphene microplate: it is the Graphene microplate dispersion liquid that 10% 1-METHYLPYRROLIDONE aqueous solution ultrasonic wave is separated into 2～25g/L that Graphene microplate is put into volume by volume concentration;
2) preparation of the slurry that injection forming is used: by after diatomite, kaolin, active carbon, antiseptic, metal ions addition agent and Graphene microplate dispersion liquid ball milling, take out slurry, obtain the slurry that injection forming is used after slaking;
3) injection forming and the demoulding: the slurry that injection forming is used is poured in the die cavity of plaster mold, after being 8～15mm at the idiosome thickness of plaster mold inwall absorption, pour out the not mobile slurry of absorption in plaster mold, obtain hollow filter core idiosome, by after degassed plaster mold processing, filter core idiosome is deviate from plaster mold, obtained composite activated carbon ultra-filtration element green compact;
4) composite activated carbon ultra-filtration element green compact are dried and sintering: composite activated carbon ultra-filtration element green compact are dry, after sintering and reducing, take out with stove cool to room temperature, and must be loaded with the composite activated carbon ultra-filtration element of Nano Silver, Nanoscale Iron.
6. the preparation method of composite activated carbon ultra-filtration element as claimed in claim 5, it is characterized in that in step 2) in, described ball milling adopts planetary Universal ball grinding machine ball milling, diatomite, kaolin, active carbon, the gross mass of antiseptic and Graphene microplate dispersion liquid and the mass ratio of abrading-ball can be 1: 3, described abrading-ball can be made up of two kinds of different-grain diameter Ceramic Balls, wherein a kind of diameter of Ceramic Balls is 1mm, the diameter of another kind of Ceramic Balls is 2mm, diameter is that the mass ratio of 1mm Ceramic Balls and 2mm Ceramic Balls is (1～3): 1, the rotating speed of ball milling can be 1000～3000rpm, the time of ball milling can be 8～16h.
7. the preparation method of composite activated carbon ultra-filtration element as claimed in claim 5, is characterized in that in step 2) in, described slaking adopts static slaking 12～24h.
8. the preparation method of composite activated carbon ultra-filtration element as claimed in claim 5, is characterized in that in step 3), described degassed processing is that plaster mold is inverted in the vacuum tank that vacuum is 10kPa, the degassed processing of static 2～4h.
9. the preparation method of composite activated carbon ultra-filtration element as claimed in claim 5, is characterized in that in step 4), described dry temperature is 102～108 ℃, and the dry time is 12～24h.
10. the preparation method of composite activated carbon ultra-filtration element as claimed in claim 5, it is characterized in that in step 4), the method of described sintering and reducing is that dried composite activated carbon ultra-filtration element green compact are put into vacuum reaction sintering stove, sintering and reducing in the atmosphere of nitrogen and hydrogen, heat up according to the speed of 4～6 ℃/min, the temperature of sintering is 850～920 ℃, and the time of sintering is 1.5～3h.
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Address after: Tianfeng road in Jimei District of Xiamen City, Fujian Province, No. 69 361000 Patentee after: Xiamen Jian Lin health home Limited by Share Ltd Address before: Tianfeng road in Jimei District of Xiamen City, Fujian Province, No. 69 361021 Patentee before: Xiamen Runner Industrial Corporation |