CN108298576A - A kind of preparation method of antibacterial granule activated carbon - Google Patents
A kind of preparation method of antibacterial granule activated carbon Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of antibacterial granule activated carbon.Include the following steps：(1) solid phase reaction prepares nano-ZnO；(2) Powdered Activated Carbon is prepared using agriculture and forestry waste as raw material；(3) it pelletizes：After mixing by nano-ZnO and Powdered Activated Carbon, mixture is added in binder and stirs evenly, and the mixing pug stirred evenly is put into roto-granulato, forms the uniform bead that grain diameter is 4 6mm, and drying obtains antibacterial granule activated carbon after cooling.The present invention prepares activated carbon using agriculture and forestry waste as raw material; and it loads nano-ZnO and obtains antibacterial granule activated carbon; not only adsorption capacity is strong; intensity is high; antibiotic property is high, and of low cost, economizes on resources; it solves the problem of environmental pollution of agriculture and forestry waste together simultaneously, and the improvement such as air, water pollution can be used for.
Description
Technical field
The present invention relates to a kind of preparation methods of antibacterial granule activated carbon.
Background technology
The grain size of nano-ZnO is small, is a kind of novel high function fine inorganic product geared to the 21st century, good surface activity,
Has the function of sterilizing.Nano ZnO powder is carried in environment-friendly materials, materials'use function is considerably increased.At present
There are many kinds of the methods for preparing nano ZnO material, such as vapour deposition process, sol-gel method, the precipitation method, combustion method, water (solvent)
Hot method, template etc..Above method Shortcomings：Generate reactant and byproduct in the process, need cumbersome washing procedure with
Remove impurity；Technique is cumbersome, and device category is more, and working hour is long, and manpower consumption is big, is unfavorable for industrial production and cost-effective.It obtains
Zinc oxide nano rod material diameter it is thicker, specific surface area is smaller, and size is inhomogenous, dispersibility it is also not good enough, influence
The application performance of nano zine oxide nanometer.
Activated carbon is by making raw material containing the substance based on charcoal, through high temperature carbonization and activation hydrophobic adsorbent obtained.It is living
Property charcoal contain a large amount of micropores, there is huge specific surface area, production practices show that activated carbon has micro quantity organic pollutant in water
There is remarkable adsorptivity, it has good absorption to waste water such as drink water purifying, dye chemical industry, food processing and organic chemical industries
Effect.Activated carbon is a kind of good adsorbent material with abundant internal voids structure and higher specific surface area, but it is former
Material is mainly the carbonaceous materials such as coal and timber, and cost is higher.There are many antibacterial granule method for preparation of active carbon at present, but prepare
Granular activated carbon there are adsorption capacities it is weak, intensity is not high, antibacterial is weak the shortcomings of, particle is especially be easy to cause in water process
Dispersion is lost in, influences wastewater treatment efficiency etc..
Agriculture and forestry waste (agriculturalresidue) refers to being generated with process in agricultural and production of forestry
Byproduct, enormous amount, have it is renewable, the regeneration period is short, biodegradable, environmental-friendly many advantages, such as, be important
Biomass resource.Mainly there are bark, shell, sawdust, stalk, bagasse etc..However, the utilization of China's agriculture and forestry waste at present
Rate is but very low or even does not utilize.Therefore, on the one hand agricultural wastes become maximum and shelve one of resource, on the other hand again at
For huge pollution sources.
To sum up, the prior art is primarily present problems with：(1) currently used for prepare the method and process of nano-ZnO it is complicated, at
This height.(2) the existing activated carbon prepared using coal and timber is of high cost.(3) existing activated carbon preparation is to prepare powder mostly
Granular activated carbon, in use be easy be lost in, it is not easy to recycle, it is weak there are anti-microbial property the problems such as.(4) existing particle
Activated carbon intensity is not high.
Invention content
The technical problems to be solved by the invention are to provide a kind of preparation method of antibacterial granule activated carbon, utilize agriculture
Forestry waste prepares activated carbon as raw material, and loads nano-ZnO and obtain antibacterial granule activated carbon.
The present invention specifically comprises the following steps：
(1) solid phase reaction prepares nano-ZnO：By the ZnCl of solid2Or ZnSO4, with NaOH mixed grindings or ball milling 5min-
Then filtering, drying, grinding as nano-ZnO after deionized water is mixed evenly is added in 10min.
(2) Powdered Activated Carbon is prepared：Using agriculture and forestry waste as raw material, using ZnCl2Powder activity is produced for activator
Charcoal；
(3) it pelletizes：After mixing by nano-ZnO and Powdered Activated Carbon, mixture is added in binder and stirs evenly, and stirs
It mixes uniform mixing pug to be put into roto-granulato, is granulated, drying, antibacterial granule activated carbon is obtained after cooling.
Specifically：
ZnCl in step (1)2Or ZnSO4With molar ratio=1 of NaOH:(2-2.5).
Step (2) the agriculture and forestry waste includes bark, shell, sawdust, stalk, bagasse.
Step (2) production activated carbon condition be：Activator ZnCl2The quality of 1~3mol/L of concentration, raw material and activator
Than being 1:(1-2) impregnates in 70-90 DEG C of water-bath, stirs 0.5h-1h, 450~650 DEG C of reaction temperature, reaction time 30-
60min。
More specifically, the Powdered Activated Carbon for preparing includes the following steps：
A, agriculture and forestry waste preprocessing process：After agriculture and forestry waste is crushed, with activator ZnCl2Uniformly mixing,
It impregnated in 70-90 DEG C of water-bath, stir 0.5h-1h, filtered, drying is spare.
B, the particle that will have been dried in A is put into electron tubes type atmosphere furnace, with nitrogen as protection gas, with 5-10 DEG C/min
Heating rate, be warming up to 450~650 DEG C, after keeping the temperature 30-60min, cooled to room temperature obtains Powdered Activated Carbon.
The mass ratio that nano-ZnO accounts for mixture in step (3) is 0.5%-1%.
Step (3) described binder is Ludox.The mass ratio of mixture and Ludox is 1：(0.25-0.35).As
Ludox, there is no particular limitation, including well known Ludox, can be widely used.
Step (3) described granulation forms the uniform bead that grain diameter is 4-6mm.
The Powdered Activated Carbon that the nano-ZnO that the present invention is prepared using solid phase reaction is produced with agriculture and forestry waste is as raw material
Antibacterial granule activated carbon is prepared, not only adsorption capacity is strong, and intensity is high, and antibiotic property is high, and of low cost, economizes on resources, simultaneously
It solves the problem of environmental pollution of agriculture and forestry waste together, and the improvement such as air, water pollution can be used for.
The invention has the advantages that：
(1) by by ZnCl2Or ZnSO4It is made by grinding or ball milling (solid phase reaction) with both sodium hydroxide solid particles
Standby nano-ZnO, this is simple for process, and the nano-ZnO purity obtained is more than 97%, and grain size is between 5-30nm, crystal form knot
Structure is hexagonal structure, as shown in Figure 1.
(2) granular activated carbon is prepared using agriculture and forestry waste, activated carbon SEM figures are as shown in Fig. 2, not only reduce agricultural
The influence that industry waste generates environment, and water body, the air etc. of pollution can effectively be administered, realize that solid is useless
The higher value application of gurry.Raw material utilize waste, derive from a wealth of sources, it is of low cost, take it is be easy, conveniently, can realize recycling
It utilizes.
(3) present invention using Ludox as binder, to improve the intensity of granular activated carbon, not only intensity height,
Antibiotic property is high, and adsorption effect is good.
(4) the antibacterial active carbon grain diameter that the present invention prepares is controlled in 4-6mm, as shown in figure 3, for air, dirt
Processing cannot be easily caused particle dispersion in water, not influence to handle quality, and be easy convenient for recycling, regeneration.
(5) simple for process, it is easy to operate.
Description of the drawings
The present invention is further illustrated in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 is nano-ZnO XRD diagram.
Fig. 2 is the activated carbon SEM figures undoped with nano-ZnO.
The activated carbon SEM figures that Fig. 3 is dopen Nano ZnO.
Specific implementation mode
Embodiment 1
A kind of preparation method of antibacterial granule activated carbon, includes the following steps：
(1) nano-ZnO is prepared using solid phase reaction：By the ZnCl of solid2Certain molar ratio mixed grinding is pressed with NaOH
Or ball milling 5min, n (ZnCl2):N (NaOH)=1:2, deionized water then is added after mixing, filtering, 105 DEG C of baking ovens are done
Dry 2h, grinding are nano-ZnO.
(2) agriculture and forestry waste preprocessing process：By agriculture and forestry waste (bark, shell, sawdust, stalk, bagasse etc.)
After crushing, raw material and activator ZnCl2(concentration 1mol/L) presses quality 1:1 uniformly mixing, 0.5h is heated in 70 DEG C of water-bath
(dipping, stirring), filtering, then be placed in 105 DEG C of baking ovens and dry for 24 hours.
(3) particle that will have been dried in (2), is put into electron tubes type atmosphere furnace, with nitrogen as protection gas, with 5 DEG C/min
Heating rate, be warming up to 450 DEG C, after keeping the temperature 30min, cooled to room temperature obtains Powdered Activated Carbon.
(4) after mixing by nano-ZnO and Powdered Activated Carbon (nano-ZnO mass ratio 0.5%), it is molten that silicon is added in mixture
In glue, solid-liquid mass ratio 1：0.25, it stirs evenly.
(5) the mixing pug that (4) stir evenly is put into roto-granulato, it is the uniform of 4-6mm to form grain diameter
Bead.The particle being granulated is put into 105 DEG C of vacuum drying chambers again and dries 1h, antibacterial granule activated carbon is obtained after cooling.
(6) the antibacterial granule activated carbon that will be prepared in (5), progress specific area measuring are 835m2/ g, compression strength are
The adsorptive value of 4.1Mpa, iodine are 950mg/g, and antibacterial granule activated carbon is under 5 minutes effect of sunlight, to staphylococcus aureus
Sterilizing rate is more than 98%, and the sterilizing rate of Escherichia coli is more than 99%.
Specific surface area measurement method uses《GB/T 7702.20-2008 coal quality granular activated carbon test method pore volume ratios
The measurement of surface area》；The absorption values determination method of iodine uses《GB/T 7702.7-2008 coal quality granular activated carbon test method iodine
The measurement of adsorptive value》；Mechanics performance determining method uses《GB/T20451-2006 activated carbon ball disk method strength test methods》；Suppression
Bacterium assay method uses《GB/T4989.2-2003 microbiological test of food hygiene total plate counts measure》.
Embodiment 2
A kind of preparation method of antibacterial granule activated carbon, includes the following steps：
(1) nano-ZnO is prepared using solid phase reaction：By the ZnSO of solid4Certain molar ratio mixed grinding is pressed with NaOH
Or ball milling 8min, n (ZnSO4):N (NaOH)=1:2, after deionized water mixing is then added, filtering, after drying, grinding is
Nano-ZnO.
(2) agriculture and forestry waste preprocessing process：By agriculture and forestry waste (bark, shell, sawdust, stalk, bagasse etc.)
After crushing, raw material and activator ZnCl2(concentration 2mol/L) presses quality 1:1.5 uniformly mixing, 1h is heated in 85 DEG C of water-bath
(dipping, stirring), filtering, then be placed in 105 DEG C of baking ovens and dry for 24 hours.
(3) particle that will have been dried in (2), is put into electron tubes type atmosphere furnace, with nitrogen as protection gas, with 7 DEG C/min
Heating rate, be warming up to 550 DEG C, after keeping the temperature 40min, cooled to room temperature obtains Powdered Activated Carbon.
(4) after mixing by nano-ZnO and Powdered Activated Carbon (nano-ZnO mass ratio 0.75%), silicon is added in mixture
In colloidal sol, solid-liquid mass ratio 1：0.3, it stirs evenly.
(5) the mixing pug that (4) stir evenly is put into roto-granulato, it is the uniform of 4-6mm to form grain diameter
Bead.The particle being granulated is put into 105 DEG C of vacuum drying chambers again and is dried 1-2 hours, obtaining antibacterial granule after cooling lives
Property charcoal.
(6) the antibacterial granule activated carbon that will be prepared in (5), progress specific area measuring are 936m2/ g, the adsorptive value of iodine
For 1176mg/g, compression strength 4.8Mpa, antibacterial granule activated carbon is under 5 minutes effect of sunlight, to staphylococcus aureus
Sterilizing rate be more than 98%, the sterilizing rates of Escherichia coli is more than 99%.
Embodiment 3
A kind of preparation method of antibacterial granule activated carbon, includes the following steps：
(1) nano-ZnO is prepared using solid phase reaction：By the ZnSO of solid4Certain molar ratio mixed grinding is pressed with NaOH
Or ball milling 5min-10min, n (ZnSO4):N (NaOH)=1:2.5, after deionized water mixing is then added, filtering, after drying,
Grinding is nano-ZnO.
(2) agriculture and forestry waste preprocessing process：By agriculture and forestry waste (bark, shell, sawdust, stalk, bagasse etc.)
After crushing, raw material and activator ZnCl2(concentration 3mol/L) presses quality 1:2 uniformly mixing, heat 1h (leachings in 90 DEG C of water-bath
Stain, stirring), filtering, then be placed in 105 DEG C of baking ovens and dry for 24 hours.
(3) particle that will have been dried in (2), is put into electron tubes type atmosphere furnace, with nitrogen as protection gas, with 10 DEG C/min
Heating rate, be warming up to 650 DEG C, after keeping the temperature 60min, cooled to room temperature obtains Powdered Activated Carbon.
(4) after mixing by nano-ZnO and Powdered Activated Carbon (nano-ZnO mass ratio 1%), Ludox is added in mixture
In, solid-liquid mass ratio 1：0.35, it stirs evenly.
(5) the mixing pug that (4) stir evenly is put into roto-granulato, it is the uniform of 4-6mm to form grain diameter
Bead.The particle being granulated is put into 105 DEG C of vacuum drying chambers again and is dried 1-2 hours, obtaining antibacterial granule after cooling lives
Property charcoal.
(6) the antibacterial granule activated carbon that will be prepared in (5), progress specific area measuring are 1001m2/ g, compression strength
Adsorptive value for 5.2Mpa, iodine is 1212mg/g, and antibacterial granule activated carbon is under 5 minutes effect of sunlight, to Staphylococcus aureus
The sterilizing rate of bacterium is more than 98%, and the sterilizing rate of Escherichia coli is more than 99%.
Although specific embodiments of the present invention have been described above, those familiar with the art should manage
Solution, we are merely exemplary described specific embodiment, rather than for the restriction to the scope of the present invention, it is familiar with this
The technical staff in field modification and variation equivalent made by the spirit according to the present invention, should all cover the present invention's
In scope of the claimed protection.
Claims (8)
1. a kind of preparation method of antibacterial granule activated carbon, it is characterised in that：Include the following steps：
(1) solid phase reaction prepares nano-ZnO：By the ZnCl of solid2Or ZnSO4, with NaOH mixed grindings or ball milling 5min-
Then filtering, drying, grinding as nano-ZnO after deionized water is mixed evenly is added in 10min；
(2) Powdered Activated Carbon is prepared：Using agriculture and forestry waste as raw material, using ZnCl2Powdered Activated Carbon is produced for activator；
(3) it pelletizes：After mixing by nano-ZnO and Powdered Activated Carbon, mixture is added in binder and stirs evenly, and stirring is equal
Even mixing pug is put into roto-granulato, is granulated, drying, and antibacterial granule activated carbon is obtained after cooling.
2. the preparation method of antibacterial granule activated carbon according to claim 1, it is characterised in that：ZnCl in step (1)2Or
ZnSO4With molar ratio=1 of NaOH:2-2.5.
3. the preparation method of antibacterial granule activated carbon according to claim 1, it is characterised in that：Step (2) described agricultural
Industry waste includes bark, shell, sawdust, stalk, bagasse.
4. the preparation method of antibacterial granule activated carbon according to claim 1, it is characterised in that：Step (2) production activity
The condition of charcoal is：Activator ZnCl2The mass ratio of 1~3mol/L of concentration, raw material and activator is 1:In 1-2,70-90 DEG C of water-baths
Dipping, stirring 0.5h-1h, 450~650 DEG C of reaction temperature, reaction time 30-60min.
5. the preparation method of antibacterial granule activated carbon according to claim 1, it is characterised in that：The preparation powder activity
Charcoal specifically includes following steps：
A, agriculture and forestry waste preprocessing process：After agriculture and forestry waste is crushed, with activator ZnCl2Uniformly mixing, in 70-
It impregnated in 90 DEG C of water-bath, stir 0.5h-1h, filtered, drying is spare；
B, the particle that will have been dried in step A is put into electron tubes type atmosphere furnace, with nitrogen as protection gas, with 5-10 DEG C/min
Heating rate, be warming up to 450~650 DEG C, after keeping the temperature 30-60min, cooled to room temperature obtains Powdered Activated Carbon.
6. the preparation method of antibacterial granule activated carbon according to claim 1, it is characterised in that：Nano-ZnO in step (3)
The mass ratio for accounting for mixture is 0.5%-1%.
7. the preparation method of antibacterial granule activated carbon according to claim 1, it is characterised in that：Step (3) described bonding
Agent is Ludox, and the mass ratio of the mixture and Ludox is 1：0.25-0.35.
8. the preparation method of antibacterial granule activated carbon according to claim 1, it is characterised in that：Step (3) described granulation,
Form the uniform bead that grain diameter is 4-6mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113087097A (en) * | 2019-12-23 | 2021-07-09 | 江苏嘉恒环境科技有限公司 | High-efficiency composite filter material for water body disinfection and preparation process thereof |
| CN115490287A (en) * | 2022-05-30 | 2022-12-20 | 浙江大学 | Porous interpenetrating 3D zinc oxide/activated carbon gel spheres and preparation method and application thereof |
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| CN102757047A (en) * | 2012-05-31 | 2012-10-31 | 北京林业大学 | Method for preparing cylindrical sludge-based activated carbon |
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| CN106241796A (en) * | 2016-07-14 | 2016-12-21 | 旌德县龙强净化材料厂 | A kind of method utilizing Exocarpium cocois (Cocos nucifera L) to prepare activated carbon |
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|---|---|---|---|---|
| CN1548376A (en) * | 2003-05-09 | 2004-11-24 | 新疆大学 | One-step solid reaction process of preparing nano zinc oxide ball and rod at near room temperature condition |
| CN101759145A (en) * | 2010-01-22 | 2010-06-30 | 湘潭大学 | Preparation method of ZnO/TiO2 composite nanoparticles |
| CN102757047A (en) * | 2012-05-31 | 2012-10-31 | 北京林业大学 | Method for preparing cylindrical sludge-based activated carbon |
| CN106241796A (en) * | 2016-07-14 | 2016-12-21 | 旌德县龙强净化材料厂 | A kind of method utilizing Exocarpium cocois (Cocos nucifera L) to prepare activated carbon |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113087097A (en) * | 2019-12-23 | 2021-07-09 | 江苏嘉恒环境科技有限公司 | High-efficiency composite filter material for water body disinfection and preparation process thereof |
| CN115490287A (en) * | 2022-05-30 | 2022-12-20 | 浙江大学 | Porous interpenetrating 3D zinc oxide/activated carbon gel spheres and preparation method and application thereof |
| CN115490287B (en) * | 2022-05-30 | 2023-11-17 | 浙江大学 | Porous interpenetrating 3D zinc oxide/activated carbon gel ball and preparation method and application thereof |
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