CN105289497A - High nanometer sliver loading active carbon and preparation method thereof - Google Patents
High nanometer sliver loading active carbon and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to high nanometer sliver loading active carbon and a preparation method thereof. A purpose of the present invention is to provide a simple nanometer sliver loading active carbon preparation method suitable for industrial production, and nanometer sliver loading active carbon prepared through the method. According to the present invention, the preparation process is divided into four modules such as nanometer silver medium preparation, active carbon pretreatment, silver supporting adsorption, and separation and purification, such that the modular preparation process is achieved, and the quality management control and the efficiency improving are easily achieved; with the method, the nanometer sliver loading active carbons having different uses can be prepared by using different specifications of the active carbon and different particle sizes of the nanometer silver mediums, the combination is diverse, and the control is flexible; the active carbon is pre-treated, such that the number and the density of the nanometer sliver adsorption groups on the surface and the inner wall can be improved so as to improve the silver loading amount (100-10000 ppm) and reduce the silver loss; and with the method, a variety of nanometer silver loading active carbons can be prepared, the silver loading amount and the nanometer silver particle size can be adjusted, and the wide application values are provided.
Description
Technical field
The present invention relates to a kind of high capacity nano-silver active carbon and preparation method thereof, specifically, is the preparation method that a kind of technique is simple, cost is low, security is high, is applicable to industrial production; Different size carrying nano silver active carbon can be prepared with satisfied different demand, can be used for preparation sewage disposal, exhaust-gas treatment, antibacterially to keep a public place clean, environmental protection and the Related product such as purification, chemical catalysis, have a extensive future.
Background technology
Reform and opening-up three during the last ten years, China's economy and society achieve continuously and healthily with deep development.In this process, along with industrial manufacturing industry and agriculture fast development, environmental problem is on the rise.Wherein, water quality deterioration and atmosphere pollution serious threat is to the health of people and productive life.How effectively administering water and atmosphere pollution, the water that the protection mankind depend on for existence and Air resource, realize the sustainable development of economic society, just becomes more and more urgent and important.
In many water and atmospheric treatment technology, active carbon adsorption technology is a kind of getting instant result and cheap method.But also there is its drawback in active carbon adsorption technology, such as, hydrophobic due to activated carbon surface, add huge specific area, effectively to remove in water body while organic compound and part inorganic impurity, also for the breeding of the microorganisms such as bacterium provides hotbed, make active carbon itself also become pollution sources, cause the secondary pollution of water body and affect purifying water effect.In order to overcome this defect, we consider to carry out carrying silver process to active carbon, become carrying nano silver active carbon after activated carbon-carried nano silver.Carrying nano silver active carbon not only can keep the function of organic compound in adsorbed water and part inorganic matter, and its Nano Silver carried also can effectively anti-bacteria, the mould even microbial growth of virus be bred.Research finds, carrying nano silver active carbon is compared with normal activated carbon, and the speed of not only decontamination removal of impurities is accelerated, and efficiency also gets a promotion greatly, and effectively can suppress microbial reproduction, prevents active carbon from becoming secondary pollution source.
In the active carbon of all multiple types, we have selected that specific area is large, hole is flourishing and the active carbon of good mechanical property is carrier, and the moisture wherein contained by shell activated carbon and ash content are all lower, thus preferably shell activated carbon as Nano Silver carrier.On the other hand, research shows, the bactericidal ability of carrying nano silver active carbon is relevant with Nano Silver particle diameter to silver carrying amount.The silver carrying amount of active carbon is higher, and Nano Silver particle diameter is less, and bactericidal and bacteriostatic effect is better.Therefore the present invention increases activated carbon surface by the method activated active carbon and silver carrying amount is improved in intrapore year silver-colored site.Meanwhile, we are pre-synthesis is no more than the nano-Ag particles of 200nm, it can be used as Nano Silver medium.
The disclosed method of Chinese patent " active carbon of loading nano silvery and preparation method thereof " (publication number: CN103232035A) is, rice hull active carbon is added in deionized water, adjust ph is 9 ~ 11, add valence state silver compound and a complexing agent again, add chemical reducing agent after being uniformly mixed, fully after reaction, namely obtain the active carbon of loading nano silvery.The method is after the complex compound of charcoal absorption one valence state silver, use reducing agent again, the complex compound of the valence state silver that active carbon adsorbs is reduced, obtain carrying nano silver active carbon, but the nano-Ag particles on carrying nano silver active carbon is reunited serious, distribution of particles is uneven, and Nano Silver is mainly distributed in activated carbon surface, the distribution of internal void Nano Silver is less, and finally cause silver carrying amount low, the sterilization anti-microbial property of carrying nano silver active carbon is had a greatly reduced quality.On the other hand, although last handling process still have passed through take out steps such as washing oven dry, but due to the superpower adsorptivity of active carbon, cause the impurity compound of active carbon inside absorption and ion etc. residual serious, this can affect water treatment efficiency, and the complex compound that these impurity compounds and ion are all reduction one valence state silver is brought into.
Chinese patent " preparation method of antibacterial fibre of activated carbon containing nano silver particles " (publication number: CN1376822) disclosed method method disclosed with " active carbon of loading nano silvery and preparation method thereof " (publication number: CN103232035A) in principle is the same, difference is, the complex compound of what NACF directly adsorbed is not a valence state silver, but directly adsorb a valence state silver, then the reproducibility of NACF is utilized, one valence state silver of absorption is at high temperature reduced, becomes carrying nano silver active carbon.Although do not add other reducing agents and complexometric reagent, but the NACF that phosphoric acid dip is crossed is to the limited sorption capacity of a valence state silver, silver carrying amount can be affected, and Nano Silver domain size distribution after reduction uneven with, mainly also be distributed in activated carbon surface, be difficult to be formed and stablize lasting absorption and antibacterial bacteriostatic effect.
Chinese patent " a kind of method making coconut palm charcoal nano-silver active carbon " (publication number: CN104190357A) is although disclosed method adopts the cocoanut active charcoal of high-ratio surface sum porosity, before implantation Nano Silver, simple chlorohydric acid pickling is done to NACF, this can only play the effect of necessarily dredging active carbon hole and pipeline, the hydrophily of active carbon is transformed, increasing specific surface area and pore volume without obvious effect, therefore effect is very limited in raising silver carrying amount.The improvements of this invention allow the preparation process of Nano Silver and charcoal adsorption process independent, obtain highly purified nano-Ag particles, allow active carbon can adsorb Nano Silver in the system of relative " totally ", effectively prevent the interference of other impurity compounds and ion, but because nano-Ag particles not being configured to the nano-class silver colloidal solution of more stable uniform, make nano-Ag particles can not better fully compatible with activated carbon fiber with to contact and Blang is diffused in hole, final absorption mainly rests on activated carbon surface, have impact on silver carrying amount, also be unfavorable for that reducing silver runs off.
Through long-time investigation, we find, current commercially available active carbon loading silver, Argent grain mainly relies on model ylid bloom action power in the absorption of activated carbon surface, this chemical interactions is very weak, is difficult to improve silver carrying amount and resist silver run off, therefore is difficult to form lasting absorption and bactericidal and bacteriostatic effect.The more important thing is, the silver carrying amount of this kind of active carbon loading silver is generally ppm level, and from tens to hundreds of ppm, and particle diameter mostly is hundreds of nanometer, and sterilizing ability is very limited.
Be summed up, object of the present invention is just intended to solve four problems: the first, improves activated carbon silver carrying amount; The second, reduce carrying nano silver grain diameter; 3rd, reduce silver and run off; 4th, strict impurity and other ion residues controlling carrying nano silver active carbon, prevent it from becoming secondary pollution source.
Summary of the invention
The present invention is directed to the problems referred to above, provide a whole set of solution, first, for improving activated carbon silver carrying amount, the characteristics such as first we select the active carbon being widely used in all kinds sewage such as sanitary sewage, chemical engineering sewage, medical sewage and municipal sewage and exhaust-gas treatment to be Nano Silver carrier, and the cocoanut active charcoal wherein in shell carbon has larger specific area, flourishing micro-central hole structure, adsorption capacity is large, the rate of filtration is fast; The second, the present invention devises and carries out pretreatment to active carbon, improves activated adoption radical amount and density in its surface and hole further, dredges hole.By the complexing in nano-Ag particles and modified active carbon surface and hole between activated adoption group, improve silver carrying amount to thousand ppm to ten thousand ppm levels, opposing silver runs off; 3rd, the present invention is pre-synthesis high-purity nano silver medium; 4th, we devise will carry silver and Nano Silver medium prepares the way that two processes are separated, Nano Silver is implanted in pretreated active carbon by Nano Silver medium, effectively prevent the interference of reducing agent, complex compound and foreign ion, prevent carrying nano silver active carbon from becoming secondary pollution source.5th, in the system built separately, prepare Nano Silver medium, effectively can control the domain size distribution of nano-Ag particles and surface polarity etc., be convenient to carry out separation and purification and metering to it simultaneously, improve controllability, also meet the theory of modularized production.There is not been reported for design concept disclosed by the invention and method.
The present invention is achieved through the following technical solutions:
A kind of high capacity nano-silver active carbon and preparation method thereof, its concrete steps are as follows:
The preparation of Nano Silver medium
Preferential employing chemical synthesising technology prepares Nano Silver medium, and Nano Silver particle size range is 5 ~ 500nm, is preferably 5 ~ 100nm.
Further, the pretreatment of activated carbon
The method of preferential employing oxidation modification carries out activating pretreatment to active carbon; Then separation and purification, oven dry, stand-by.
Further, the control of silver-colored process is carried
The Pre-Treatment of Activated charcoal of accurate-metering is added in a certain amount of Nano Silver medium, is equipped with certain auxiliary absorption measure, completes Nano Silver implantation process; Isolate carrying nano silver active carbon crude product.
Further, the separation and purification of carrying nano silver active carbon, oven dry and preservation
By the further separation and purification of isolated for previous step carrying nano silver active carbon crude product, dry, stand-by.
Beneficial effect:
A kind of high capacity nano-silver active carbon provided by the invention and preparation method thereof, has first prepared the high-purity nano silver medium that particle diameter less (being no more than 100nm), distribution are more even, compatibility is higher.
Activating pretreatment is carried out to active carbon, has improve nano silver active adsorption group quantity and density in activated carbon surface and hole, carrying silver with absorbent charcoal amount has been increased to thousand ppm to ten thousand ppm levels.
Nano Silver and activated adoption group are associated by complexing, more firm compared to model ylid bloom action, play slowly-releasing and reduce silver-colored effect of running off.
The adsorption loading silver process of the preparation of Nano Silver medium and active carbon is separated, decreases its impurities left.
Thinking designed according to this invention, the whole preparation process of carrying nano silver active carbon is divided into four module: the pretreatment of active carbon, the preparation of Nano Silver medium, year silver absorption, separation and purification (post processing), achieve the modularization of preparation process, contribute to quality management and control, be also conducive to enhancing productivity.
A kind of high capacity nano-silver active carbon disclosed by the invention and preparation method thereof reaches design original intention substantially.
Accompanying drawing explanation
Fig. 1 is the manufacture flow process that the present invention relates to High-efficient Water process carrying nano silver active carbon;
Fig. 2 is the carrying nano silver activated carbon surface of the embodiment of the present invention 1 preparation and the SEM*15 in cross section, 000 figure, and in figure, black particle is Nano Silver;
Fig. 3 is the carrying nano silver activated carbon surface of the embodiment of the present invention 2 preparation and the SEM*15 in cross section, 000 figure, and in figure, black particle is Nano Silver;
Fig. 4 is the carrying nano silver activated carbon surface of the embodiment of the present invention 3 preparation and the SEM*10 in cross section, 000 figure, and in figure, white particle is Nano Silver;
Fig. 5 is the carrying nano silver activated carbon surface of the embodiment of the present invention 4 preparation and the SEM*10 in cross section, 000 figure, and in figure, white particle is Nano Silver;
Fig. 6 is the carrying nano silver activated carbon surface of the embodiment of the present invention 5 preparation and the SEM*15 in cross section, 000 figure, and in figure, white particle is Nano Silver;
Fig. 7 is the carrying nano silver activated carbon surface of the embodiment of the present invention 6 preparation and the SEM*15 in cross section, 000 figure, and in figure, white particle is Nano Silver;
Fig. 8 is the SEM*150 of 10-30nm Nano Silver medium prepared by the present invention, 000 figure;
Fig. 9 is the SEM*100 of 50nm Nano Silver medium prepared by the present invention, 000 figure;
Figure 10 is the SEM*50 of 100nm Nano Silver medium prepared by the present invention, 000 figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to a kind of preparation method of carrying nano silver cocoanut active charcoal of carrying nano silver particle (20nm)
Get 1 kilogram of freshly prepd fragment shape cocoanut active charcoal, grind rear mistake 80 eye mesh screen, wash to washing lotion clear, colorless several times with 5 kilograms of pure water; Dry to constant weight, in drier, be cooled to room temperature, be denoted as cocoanut active charcoal AC-0 for 100 ~ 140 DEG C; 1 kilogram of above-mentioned cocoanut active charcoal adds in 30% hydrogen peroxide under stirring by 180rpm, and room temperature maintains stirring 5 ~ 8 hours, filters out active carbon; 5 kilograms of pure water gradation repeatedly take out be washed till washing lotion colourless and in neutrality till, now washing lotion electrical conductivity is lower than 20.0 μ s/cm; By drying to constant weight at cocoanut active charcoal 100-140 good for modification DEG C, in drier, being cooled to room temperature, being denoted as cocoanut active charcoal AC-1.
In 40-50 DEG C of environment, take silver ammino solution as presoma, maltose is reducing agent, glucan protective agent, preparation 20nm nano-Ag particles; Through high speed centrifugation, pure water 5 times, absolute ethanol washing 5 times; Then be again scattered in pure water under nano silver material being stirred, add the glucan of 5%, ultrasonic 10 seconds of ultrasound intensity 0.5W/mL(, interval 5 seconds), speed of agitator 200rpm, jitter time 2 hours, whole process control temp is no more than 40 DEG C; Finally obtain homogeneous nano-class silver colloidal solution, as Nano Silver medium A, it is 1000ppm that ICP method records Nano Silver concentration.
1 kilogram of AC-1 adds in 5 kilograms of Nano Silver medium A, holding temperature 25 ~ 30 DEG C under stirring by 180rpm; Be equipped with excusing from death and assist absorption, ultrasonic 10 seconds of ultrasound intensity 0.5W/mL(, interval 5 seconds), ultrasonic time 0.5 hour; After absorption reaches balance, 5 ~ 10 kilograms of pure water are repeatedly taken out and are washed carrying nano silver active carbon to washing lotion water white transparency, till ICP cannot detect silver; Dry to constant weight, be transferred in dry device and be cooled to room temperature, pack stand-by for 150 DEG C.
The silver carrying amount that ICP records carrying nano silver active carbon is>=25mg/g; BET specific surface area>=1150m
2/ g; Iodine number>=960mg/g; PH6.5 ~ 7.5; Stereoscan photograph is as Fig. 2.
embodiment 2
The present embodiment relates to a kind of preparation method of carrying nano silver cocoanut active charcoal of carrying nano silver particle (30nm)
Get 1 kilogram of freshly prepd fragment shape cocoanut active charcoal, grind rear mistake 50 eye mesh screen, wash to washing lotion clear, colorless several times with 3 ~ 5 kilograms of pure water; Dry to constant weight, in drier, be cooled to room temperature, be denoted as cocoanut active charcoal AC-0 for 100 ~ 150 DEG C; 1 kilogram of above-mentioned cocoanut active charcoal adds in 30% hydrogen peroxide under stirring by 150rpm, and room temperature maintains stirring and spends the night (12h), filters out active carbon; 5 kilograms of pure water gradation repeatedly take out be washed till washing lotion colourless and in neutrality till, now washing lotion electrical conductivity is lower than 20.0 μ s/cm; By drying to constant weight at cocoanut active charcoal 100 ~ 150 DEG C good for modification, in drier, being cooled to room temperature, being denoted as cocoanut active charcoal AC-1.
In 40-70 DEG C of environment, take silver ammino solution as presoma, fructose is reducing agent, and polyvinylpyrrolidone (PVP) is covering and dispersant, preparation 30nm nano-Ag particles; Through high speed centrifugation, pure water 5 times, absolute ethanol washing 5 times, then 40 ~ 50 DEG C of vacuum drying obtain nano silver material in 2 hours; Then be again scattered in pure water under being stirred by nano silver material, the polyethylene glycol adding 5 ~ 10% does dispersant, ultrasonic 10 seconds of ultrasound intensity 1W/mL(, interval 5 seconds), speed of agitator 200rpm, jitter time 2 ~ 4 hours, whole process control temp is no more than 40 DEG C; Finally obtain nano-class silver colloidal solution, as Nano Silver medium A, it is 2000ppm that ICP method records Nano Silver concentration, and stereoscan photograph is as Fig. 8.
1 kilogram of AC-1 adds in 5 kilograms of Nano Silver medium A, holding temperature 25 ~ 30 DEG C under stirring by 200rpm; Be equipped with excusing from death and assist absorption, ultrasonic 10 seconds of ultrasound intensity 0.5W/mL(, interval 5 seconds), ultrasonic time 1 hour; Then, 5 ~ 10 kilograms of pure water are repeatedly taken out and are washed carrying nano silver active carbon to washing lotion water white transparency, till ICP cannot detect silver; Dry to constant weight, be transferred in dry device and be cooled to room temperature, pack stand-by for 150 DEG C.
The silver carrying amount that ICP records carrying nano silver active carbon is>=20mg/g; BET specific surface area>=1100m
2/ g; Iodine number>=950mg/g; PH6.5 ~ 7.5; Stereoscan photograph is as Fig. 3.
embodiment 3
The present embodiment relates to a kind of preparation method of carrying nano silver walnut shell active carbon of carrying nano silver particle (50nm)
Get 5 kilograms of freshly prepd fragment shape walnut shell active carbons, grind rear mistake 30 eye mesh screen, wash to washing lotion clear, colorless several times with 20 kilograms of pure water; Dry to constant weight, in drier, be cooled to room temperature, be denoted as walnut shell active carbon AC-0 for 120 DEG C; Under 180rpm stirs, add in 15 ~ 20% aqueous solution of nitric acid by 1 kilogram of above-mentioned walnut shell active carbon, soaking at room temperature 4 hours, filters out active carbon; 25 kilograms of pure water gradation repeatedly take out be washed till washing lotion colourless and in neutrality till, now washing lotion electrical conductivity is lower than 20.0 μ s/cm; Dry to constant weight at the walnut shell active carbon that nitric acid is activated 120 DEG C, in drier, be cooled to room temperature, be denoted as walnut shell active carbon AC-1.
In 40 ~ 70 DEG C of environment, take silver ammino solution as presoma, glucose is reducing agent, and gelatin is dispersant, preparation 50nm nano-Ag particles; Through centrifugal, pure water 5 times, absolute ethanol washing 5 times, then 30 ~ 50 DEG C of vacuum drying obtain nano silver material in 2 hours; Then be again scattered in pure water under being stirred by nano silver material, the polyvinylpyrrolidone (PVP) adding 5 ~ 10% does dispersant, ultrasonic 5 seconds of ultrasound intensity 0.8W/mL(, interval 5 seconds), speed of agitator 200rpm, jitter time 4 hours, whole process control temp is no more than 40 DEG C; Finally obtain homogeneous nano-class silver colloidal solution, as Nano Silver medium A, it is 5000ppm that ICP method records Nano Silver concentration, and stereoscan photograph is as Fig. 9.
1 kilogram of AC-1 adds in 5 kilograms of Nano Silver medium A, holding temperature 25 ~ 30 DEG C under stirring by 150rpm; Be equipped with excusing from death and assist absorption, ultrasonic 5 seconds of ultrasound intensity 1.0W/mL(, interval 5 seconds), ultrasonic time 1.5 hours; After absorption reaches balance, 5 ~ 10 kilograms of pure water are repeatedly taken out and are washed carrying nano silver active carbon to washing lotion water white transparency, till ICP cannot detect silver; Dry to constant weight, be transferred in dry device and be cooled to room temperature, pack stand-by for 120 DEG C.
The silver carrying amount that ICP records carrying nano silver active carbon is>=15mg/g; BET specific surface area>=950m
2/ g; Iodine number>=900mg/g; PH7.0 ~ 7.5; Stereoscan photograph is as Fig. 4.
embodiment 4
The present embodiment relates to a kind of preparation method of carrying nano silver active fruit shell carbon of carrying nano silver particle (100nm)
Get 10 kilograms of freshly prepd crushed particles shape active fruit shell carbons, grind rear mistake 30 eye mesh screen, wash to washing lotion clear, colorless several times with 40 ~ 50 kilograms of pure water; Dry to constant weight, in drier, be cooled to room temperature, be denoted as active fruit shell carbon AC-0 for 115 DEG C; Under 180rpm stirs, add in 10% oxalic acid aqueous solution by 5 kilograms of above-mentioned active fruit shell carbons, soaking at room temperature 8 hours, filters out active carbon; 25 kilograms of pure water gradation repeatedly take out be washed till washing lotion colourless and in neutrality till, now washing lotion electrical conductivity is lower than 20.0 μ s/cm; Dry to constant weight at the active fruit shell carbon that oxalic acid is activated 120 DEG C, in drier, be cooled to room temperature, be denoted as active fruit shell carbon AC-1.
In 40 ~ 60 DEG C of environment, take silver oxalate as presoma, hydrazine hydrate is reducing agent, and soluble starch is dispersant, preparation 100nm nano-Ag particles; Through centrifugal, pure water 5 times, absolute ethanol washing 5 times, then 40 ~ 50 DEG C of vacuum drying obtain nano silver material in 2 hours; Then be again scattered in pure water under being stirred by nano silver material, the soluble starch adding 5 ~ 10% is cooked dispersant, ultrasonic 5 seconds of ultrasound intensity 1.5W/mL(, interval 5 seconds), speed of agitator 250rpm, jitter time 5 hours, whole process control temp is no more than 40 DEG C; Finally obtain uniform nano silver suspending liquid, as Nano Silver medium A, it is 500ppm that ICP method records Nano Silver concentration, and stereoscan photograph is as Figure 10.
5 kilograms of AC-1 add in 20 kilograms of Nano Silver medium A, holding temperature 20-30 DEG C under stirring by 100rpm; Be equipped with excusing from death and assist absorption, ultrasonic 5 seconds of ultrasound intensity 1.0W/mL(, interval 5 seconds), ultrasonic time 2.5 hours; After absorption reaches balance, 30 kilograms of pure water are repeatedly taken out and are washed carrying nano silver active carbon to washing lotion water white transparency, till ICP cannot detect silver; Dry to constant weight, be transferred in dry device and be cooled to room temperature, pack stand-by for 115 DEG C.
The silver carrying amount that ICP records carrying nano silver active carbon is>=5mg/g; BET specific surface area>=750m
2/ g; Iodine number>=800mg/g; PH6.5 ~ 7.5; Stereoscan photograph is as Fig. 5.
embodiment 5
The present embodiment relates to a kind of preparation method of carrying nano silver wood activated charcoal of carrying nano silver particle (70nm)
Get 10 kilograms of column wood activated charcoals, wash to washing lotion clear, colorless several times with 50 ~ 60 kilograms of pure water; Dry to constant weight, in drier, be cooled to room temperature, be denoted as wood activated charcoal AC-0 for 120 DEG C; Under 180rpm stirs, add in 5% aqueous sodium hypochlorite solution by 10 kilograms of above-mentioned wood activated charcoals, stirred overnight at room temperature, filters out active carbon; 50 kilograms of pure water are repeatedly taken out several times and are washed till that washing lotion is colourless and in neutral, washing lotion electrical conductivity is lower than till 20.0 μ s/cm; By drying to constant weight at the wood activated charcoal 120 DEG C activated, be denoted as wood activated charcoal AC-1 stand-by.
In 40 ~ 60 DEG C of environment, take silver nitrate as presoma, glucose is reducing agent, and CMC is dispersant, preparation 70nm nano-Ag particles; Through centrifugal, pure water 5 times, absolute ethanol washing 5 times, then 45 DEG C of vacuum drying obtain nano silver material in 4 hours; Then be again scattered in pure water under being stirred by nano silver material, the CMC adding 3% does dispersant, ultrasonic 5 seconds of ultrasound intensity 0.5W/mL(, interval 5 seconds), speed of agitator 250rpm, jitter time 2 hours, whole process control temp is no more than 50 DEG C; Finally obtain dispersed Nano Silver suspension preferably, as Nano Silver medium A, it is 1000 ~ 1200ppm that ICP method records Nano Silver concentration.
5 kilograms of AC-1 add in 25 kilograms of Nano Silver medium A, holding temperature 30 ~ 35 DEG C under stirring by 200rpm; After absorption reaches balance, 30 kilograms of pure water are repeatedly taken out and are washed carrying nano silver active carbon to washing lotion water white transparency, till ICP cannot detect silver; Dry to constant weight, be cooled to room temperature, pack stand-by for 135 DEG C.
The silver carrying amount that ICP records carrying nano silver active carbon is>=2mg/g; BET specific surface area>=550m
2/ g; Iodine number>=650mg/g; PH7.0 ~ 7.5; Stereoscan photograph is as Fig. 6;
embodiment 6
The present embodiment relates to a kind of preparation method of carrying nano silver wood activated charcoal of carrying nano silver particle (150 ~ 200nm)
Get 2 kilograms of sheet cocoanut active charcoals, wash to washing lotion clear, colorless several times with 10 kilograms of pure water; Dry to constant weight, be denoted as cocoanut active charcoal AC-0 for 120 DEG C; 1 kilogram of above-mentioned cocoanut active charcoal is added 0.1% potassium permanganate solution soaked overnight, filters out active carbon; 5 kilograms of pure water are repeatedly taken out several times and are washed till that washing lotion is colourless and in neutral, washing lotion electrical conductivity is lower than till 20.0 μ s/cm; By drying to constant weight at the cocoanut active charcoal 120 DEG C activated, be denoted as cocoanut active charcoal AC-1 stand-by.
Take silver nitrate as presoma, hydrazine hydrate is reducing agent, and CMC is dispersant, preparation 150 ~ 200nm nano-Ag particles; Through centrifugal, pure water, ethanol washing, then 45 DEG C of vacuum drying obtain nano silver material in 4 ~ 6 hours; Then be again scattered in pure water under being stirred by nano silver material, the CMC adding 1% does dispersant, high-speed stirred (rotating speed 800rpm) jitter time 2 hours; Finally obtain Nano Silver suspension, as Nano Silver medium A, it is 1500ppm that ICP method records Nano Silver concentration.
1 kilogram of AC-1 adds in 5 kilograms of Nano Silver medium A under stirring by 300rpm under room temperature; After 24 hours, 10 kilograms of pure water are repeatedly taken out and are washed carrying nano silver active carbon to washing lotion water white transparency, till ICP cannot detect silver; Dry to constant weight, be cooled to room temperature, pack stand-by for 135 DEG C.
The silver carrying amount that ICP records carrying nano silver active carbon is >=12mg/g; BET specific surface area >=850m2/g; Iodine number >=870mg/g; PH7.0 ~ 7.5; Stereoscan photograph is as Fig. 7.
Claims (10)
1. high capacity nano-silver active carbon and preparation method thereof, is characterized in that:
(1) Nano Silver medium and Pre-Treatment of Activated charcoal is prepared; (2) Nano Silver is implanted in pretreated active carbon, and be equipped with certain auxiliary absorption measure; (3) carrying nano silver active carbon is isolated; Purifying, oven dry.
2. a kind of high capacity nano-silver active carbon according to claim 1 and preparation method thereof, is characterized in that: the preparation method of described Nano Silver medium comprises the one in chemical synthesis, Physical, biological synthesis process, is wherein preferably chemical synthesis.
3. a kind of high capacity nano-silver active carbon according to claim 2 and preparation method thereof, it is characterized in that: described Nano Silver medium, for the one in nano-class silver colloidal solution, Nano Silver suspension, nano-Ag particles suspension, nano silver powder etc., be wherein preferably nano-class silver colloidal solution.
4. a kind of high capacity nano-silver active carbon according to claim 3 and preparation method thereof, is characterized in that: contained by described Nano Silver medium, the particle size range of nano-Ag particles is 5 ~ 500nm, is preferably 5 ~ 100nm.
5. a kind of high capacity nano-silver active carbon according to claim 1 and preparation method thereof, it is characterized in that: described active carbon comprises one or more in active fruit shell carbon, wood activated charcoal, coal mass active carbon, petroleum-type active carbon, regenerated carbon etc., be wherein preferably active fruit shell carbon.
6. a kind of high capacity nano-silver active carbon according to claim 5 and preparation method thereof, it is characterized in that: described fruit shell carbon comprises one or more in cocos active carbon, apricot shell active carbon, walnut shell active carbon, rice hull active carbon etc., be wherein preferably cocoanut active charcoal.
7. a kind of high capacity nano-silver active carbon according to claim 1 and preparation method thereof, is characterized in that: the preprocess method of described active carbon is that fragmentation is sieved, washed, sour modification, alkali modification, oxidation modification, modified with reduction, high temperature modified in one or more; Preferably sieve, wash and add oxidation modification.
8. a kind of high capacity nano-silver active carbon according to claim 7 and preparation method thereof, it is characterized in that: the reagent that described oxidation modification is used comprises the one in nitric acid, phosphoric acid, sulfuric acid, acetic acid, citric acid, oxalic acid, hydrogen peroxide and other peroxide, permanganic acid and salt thereof, dichromic acid and salt, hypochlorous acid and salt thereof, chloric acid and salt, perchloric acid and salt, ozone etc., be wherein preferably hydrogen peroxide.
9. a kind of high capacity nano-silver active carbon according to claim 1 and preparation method thereof, is characterized in that: described auxiliary absorption measure be stir, ultrasonic, shake, rock, leave standstill, extra electric field, magnetic field, light radiation, one or more in physics ray etc.; Be preferably stir and ultrasonic.
10. according to carrying nano silver active carbon prepared by method described in claim 1 ~ 9, can be used for preparation sewage disposal, exhaust-gas treatment, antibacterially to keep a public place clean, environmental protection and purification, chemical catalysis, the Related product such as daily.
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