CN110074102A - A kind of nano-silver biological matter charcoal composite bactericidal material and its preparation method and application - Google Patents
A kind of nano-silver biological matter charcoal composite bactericidal material and its preparation method and application Download PDFInfo
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- CN110074102A CN110074102A CN201810074296.XA CN201810074296A CN110074102A CN 110074102 A CN110074102 A CN 110074102A CN 201810074296 A CN201810074296 A CN 201810074296A CN 110074102 A CN110074102 A CN 110074102A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/22—Improving land use; Improving water use or availability; Controlling erosion
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
Abstract
The invention proposes a kind of nano-silver biological matter charcoal composite bactericidal materials and its preparation method and application, are related to the technical field of sterilization material.Composite bactericidal material of the invention comprises the following components in parts by weight: 0.8-1.2 parts of biomass carbon, 1.0-1.5 parts of nano-Ag particles；The composite bactericidal material is that silver ion is obtained with biomass carbon by hydrothermal synthesis method under the action of reducing agent and protective agent；The present invention gives the preparation method of above-mentioned composite bactericidal material, at 90-120 DEG C, reacts 12-24h, obtains by filtering, cleaning and drying.Biomass carbon and nano-Ag particles of the present invention are compound by hydrothermal synthesis method, the aperture of biomass carbon is big, specific surface area is high, biomass carbon and nano silver form stable chemical bond, the release for slowing down silver ion, substantially increases the bacteriostasis property of composite bactericidal material, and bacteriostasis rate is high, the antibacterial period is long, long service life.
Description
Technical field
The present invention relates to the technical field of sterilization material, particularly relate to a kind of nano-silver biological matter charcoal composite bactericidal material and
Preparation method and application.
Background technique
With the continuous development of China's economy, environmental damage is got worse, especially the pollution of tap water.Now, originally
The pollution of water is divided into three aspects: first is that source is polluted, according to the ASSOCIATE STATISTICS of environment department, the river in China has eighty per cant to exist not
With the pollution situation of degree；In water system at home, be not suitable for doing the water source of drinking water close to four one-tenth of rivers；By way of city
Section, be not suitable for being used as drinking water source close to eighty per cant；About half of Urban Underground water source is contaminated.Second is that tap water
The pollution of transfer canal, tap water subsidiary company come out reach user family in, by way of pipeline it is very long very complicated, in addition to pipeline is also wanted
By water tower, water tank etc., during transmission, many polluters can be dissolved in, such as: sludge, heavy metal ion, bacterium
Deng these pollutants probably mutually chemically react, and can generate many toxic, carcinogenic chemical substances, and there are also cities
The facilities such as the water tower in city, inspection, cleaning work are not in place, will directly affect the weight of tap water, send out according to the detection of relevant departments
Existing, in 35 main cities, water quality is not up to standard close to eighty per cant.Third is that being added caused by disinfection chemical component in water
Potential pollution, present Running-water Company still use pervious water treatment technology, and the method for precipitating, disinfection, which are used, when such as filtering adds
The method of chlorine, in chlorination, chlorine can be chemically reacted with organic substance, the humic substance in water, generate some such as tetrachloros
The stronger pollutant component of the toxicity such as methane, monoxone, these ingredients are cancer, cardiopathic principal causative substance, if people
The tap water containing these substances is drunk, it will seriously endanger the health for arriving body.
Nano silver as one kind can effectively sterilize with antibacterial substance, can be used as the sterilization material of water process, nanometer
The partial size of silver is usually in several nanometers to hundreds of nanometers；In general, the bactericidal effect mechanism of nano silver is, ultra-fine state
Nano silver meets water or following reaction: Ag → Ag occurs in aqueous solution since its surface area is very big++e-；So nano silver
Bactericidal effect is mainly related with silver ion.Largely the study found that nano silver or silver ion can be with the zymoproteins in thallus
Matter or DNA base combine, and so that enzyme is lost activity, bacterium DNA replication Disability, so as to cause germ inactivation.From nano silver
Mechanism of action in it is not difficult to find out that, nano silver is consumption process in sterilization, during sterilization, with releasing for silver ion
It puts, bactericidal property constantly declines.
Active carbon has huge specific surface area and flourishing pore structure, it is easy to the pathogenic microorganism in adsorbed water body；
But during deepling purification of drinking water, the pathogenic microorganism in water body is easily numerous in the activated carbon surface of absorption organic matter
It grows, and is dissolved in water, and then microorganism concn in water body is caused to increase；Further, since work of the itrogenous organic substance in microorganism
It under, is digested in activated carbon surface, content of nitrite greatly increases in water.Therefore, will usually have in the prior art
The substance of bactericidal property --- nano-silver loaded is in activated carbon surface, to eliminate microbial reproduction during drinking water deep purification
Brought secondary pollution.Currently, active carbon/nano silver composite material preparation method mainly includes infusion process, doping method, electricity
Chemical deposition and reduction method etc., Chinese patent CN106958140A disclose a kind of loading nano silvery activated carbon fibre and its
Preparation method carries out load simple substance nanometer using the strong adsorptivity of activated carbon fibre in the surface of activated carbon fibre and micropore
Silver and keeps higher sterilizing efficiency to reduce the loss of silver, in drinking water coloration and chlorine residue etc. improve,
To play the dual function of absorption and sterilizing to drinking water, silver carrying amount is adjustable in the activated carbon fibre of the loading nano silvery, single
Matter silver ion diameter be 10-20nm, can be used for filtering and the process for sterilizing of drinking water, in water body Escherichia coli and golden yellow
Staphylococcus, which has, efficiently to be killed except effect；But in preparation process, the activated carbon fibre of this loading nano silvery, use
It is the solution reaction at 60-80 DEG C, this preparation method will cause that nano-Ag particles partial size is uneven, nano-Ag particles are in work
Property the disadvantages of carbon fiber surface is unevenly distributed, nano-Ag particles and activated carbon fibre surface binding force are small, so as to cause this
The antibacterial time of the activated carbon fibre of kind loading nano silvery is short, and bacteriostasis rate needs to be further increased, moreover, this active carbon
Fiber cost is higher, is unfavorable for industrial production and application.
Summary of the invention
The present invention proposes a kind of nano-silver biological matter charcoal composite bactericidal material and its preparation method and application, solves existing
The activated carbon fibre bacteriostasis rate of loading nano silvery low and antibacterial time short problem in technology.
A kind of nano-silver biological matter charcoal composite bactericidal material of the invention, technical solution is achieved in that described multiple
It closes sterilization material to comprise the following components in parts by weight: 0.8-1.2 parts of biomass carbon, 1.0-1.5 parts of nano-Ag particles；It is described compound
Sterilization material is that silver ion is obtained with biomass carbon by hydrothermal synthesis method under the action of reducing agent and protective agent.
Biomass carbon is general carbon containing mainly by aromatic hydrocarbon and simple substance carbon or the carbon with graphite-like structure forms in the present invention
60% or more, other elements are mainly H, O, N, S and other ash elements；The solubility of biomass carbon is extremely low, melts boiling point pole
Height has height carboxylic esterification, aromatization and aliphatic chain structure in alkalinity or strong basicity；In its preparation process, protozoa
The micropore structure of matter is preferably retained in biomass carbon, therefore, with biggish specific surface area, can not only be adsorbed
The chlorine of being irritating to the skin property in water, keeps water quality softer, biomass carbon also has the function of sterilization and disinfection.It is raw in the present invention
Substance charcoal and nano-Ag particles are compound by hydrothermal synthesis method ,-OH base isoreactivity group are rich in biomass carbon, with nano silver shape
At stable chemical bond, the release of silver ion is further slowed down, substantially increases the bacteriostasis property of composite bactericidal material, gained
Composite bactericidal material bacteriostasis rate is high, and the antibacterial period is long, long service life.
Embodiment as one preferred, the particle size of the nano-Ag particles are 5-100nm.Nano silver partial size
Size will affect bactericidal effect and the sterilization service life of composite bactericidal material, since partial size is too small to be accelerated to consume, so that reducing makes
Use the service life；Partial size can then lower specific surface area greatly very much, influence its bactericidal effect；Present invention synthesis takes into account the grain for taking nano-Ag particles
Diameter size is between 5-100nm, preferably 5-9nm.
Embodiment as one preferred, the specific surface area of the biomass carbon are 1600-2500m2/ g, the biology
The pore size of matter charcoal is 3.0-6.0nm.The large specific surface area of biomass carbon, nano silver during hydrothermal synthesis directly into
Enter in the aperture structure of biomass carbon, and coat the outside of biomass carbon, comprehensive package structure is formed to biomass carbon, is avoided
Secondary pollution of the biomass carbon in drinking water purification process, meanwhile, the release of silver ion is slowed down, composite bactericidal material is extended
The service life of material.
Embodiment as one preferred, the biomass carbon the preparation method comprises the following steps: 1) take stalk, impregnate, drying is standby
With；2) distilled water is taken, is added in the resulting stalk of step 1), and add the concentrated sulfuric acid, wherein distilled water, the concentrated sulfuric acid and stalk
Mass ratio be 15-30:5-10:1-2, be uniformly mixed, at 120-200 DEG C, react 10-48h, it is cooling；3) by step 2) institute
The straw filtering obtained, is cleaned respectively using distilled water and dehydrated alcohol, dry, obtains carbonization stalk；It 4) will be obtained by step 3)
Carbonization stalk mixed with active material, the mass ratio of carbonization stalk and active material is 1-2:2-4, and grinding is uniform；It 5) will step
Rapid 4) resulting carbonization stalk and active material admixture at 700-800 DEG C, calcine 12- under inert gas shielding effect
For 24 hours, charcoal particle is obtained；6) hydrochloric acid and distilled water is respectively adopted in the resulting charcoal particle of step 5) to clean, then with washes of absolute alcohol,
Dry, grinding obtains biomass carbon.The preparation method of biomass carbon of the invention is simple, easy to operate, it is easy to accomplish industrialization,
The function admirable of gained charcoal.
Embodiment as one preferred, in the step 4), active material is sodium hydroxide, appointing in potassium hydroxide
Meaning is one or more of.Active material and carbonization stalk are subjected to mixed grinding, make active material sufficiently with carbonization stalk
With, fully ensured that carbonization after stalk aperture structure.
Embodiment as one preferred, in the step 1), stalk is impregnated in dehydrated alcohol, when immersion
Between be 7-10d；The stalk is corn stover, broomcorn straw, catkin, petal, Enteromorpha, any one or a few in reed；
Stalk is first crushed before impregnating, and smashed stalk particle length is 0.3-0.5cm.Dehydrated alcohol impregnates stalk
Purpose be to soften stalk, the surface fibre of stalk is destroyed, to be conducive to subsequent concentrated sulfuric acid carbonization treatment；Stalk can be with
It is many kinds, chooses straw or stem tuber etc. from a wealth of sources, can be common common stalk, such as: corn stover
Core, corncob cellulose, kaoliang stalk core, reed etc., it is of course also possible to be the straw that catkin, petal, Enteromorpha etc. do not need to be crushed
Stalk；Stalk is crushed mainly to improve before immersion and impregnates effect.
In embodiment as one preferred, the step 3) and the step 6), wash number when cleaning is
3-5 times.Composite bactericidal material of the invention is for drinking water treatment, and cleaning process is all made of distilled water and dehydrated alcohol
Cleaning, avoids the comprehensive performance that its preparation process brings potential pollution to improve composite bactericidal material composite bactericidal material.
A kind of preparation method of nano-silver biological matter charcoal composite bactericidal material of the invention, technical solution are realized in
: the following steps are included: S1: taking ethylene glycol, the concentrated sulfuric acid, polyvinylpyrrolidone and silver nitrate, ethylene glycol, the concentrated sulfuric acid, poly- second
The mass ratio of alkene pyrrolidone and silver nitrate is 10-40:5-10:1-5:0.1-1, is uniformly mixed, obtains mixed solution；S2: life is taken
Substance charcoal is added in the resulting mixed solution of step S1, the mass ratio of biomass carbon and the silver in silver nitrate used in step S1
For 0.8-1.2:1.0-1.5, stirring obtains mixture；S3: by the resulting mixture of step S2, at 90-120 DEG C, 12- is reacted
For 24 hours, cooling, obtain reaction product；S4: reaction product obtained by step S3 being filtered, sediment is obtained, and distilled water and anhydrous is respectively adopted
Ethyl alcohol cleaning, is dried, and grinding obtains composite bactericidal material.
Composite bactericidal material of the invention is using silver nitrate as raw material, in reducing agent ethylene glycol and protective agent polyvinyl pyrrole
Under the action of alkanone, biomass carbon is added, is obtained in a high pressure reaction kettle by hydrothermal synthesis method；It is rich in its biomass carbon
Containing-OH base isoreactivity group, stable chemical bond is formed with nano silver, the release of silver ion is further slowed down, greatly improves
The bacteriostasis property of composite bactericidal material, gained composite bactericidal material bacteriostasis rate is high, and the antibacterial period is long, long service life.
Embodiment as one preferred, in the step S3, cooling and is cooled to by the way of natural cooling
Room temperature；In the step S4, wash number when cleaning is 3-5 times.After hydrothermal synthesis reaction, using the side of natural cooling
Formula is cooled to room temperature product, product can be made further to be formed, and keeps product shape more stable, reduces subsequent clear
Wash destruction of the journey to product morphology；The impurity of surface is removed comprehensively by being cleaned multiple times, and makes gained composite bactericidal material
Expect purer.
A kind of application of nano-silver biological matter charcoal composite bactericidal material of the invention, technical solution are achieved in that
The composite bactericidal material is used for the filtering and sterilization processing of drinking water.Composite bactericidal material of the present invention is used for the process of drinking water
And sterilization processing, bacteriostasis property is good, and bacteriostasis rate is high, and the antibacterial period is long, long service life.
Compared with prior art, the beneficial effects of the present invention are: biomass carbon and nano-Ag particles pass through water in the present invention
Thermal synthesis method is compound, and-OH base isoreactivity group is rich in biomass carbon, stable chemical bond is formed with nano silver, further subtracts
The release of silver ion is delayed；The aperture of biomass carbon is big, and specific surface area is high, and nano silver is not only direct during hydrothermal synthesis
It into the aperture structure of biomass carbon, is also coated on the outer surface of biomass carbon, package knot comprehensively is formed to biomass carbon
Structure avoids secondary pollution of the biomass carbon in drinking water purification process；Substantially increase the biocidal property of composite bactericidal material
Can, gained composite bactericidal material bacteriostasis rate is high, additionally it is possible to go the chlorine residue in water removal, keep drinking water softer, have sterilization and
The double action of disinfection, the antibacterial period is long, long service life.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the electron scanning micrograph figure of one gained biomass carbon of the embodiment of the present invention；
Fig. 2 is the transmission electron microscope photo figure of one gained biomass carbon of the embodiment of the present invention；
Fig. 3 is the specific surface area test result figure of one gained biomass carbon of the embodiment of the present invention；
Fig. 4 is the opening size test result figure of one gained biomass carbon of the embodiment of the present invention；
Fig. 5 is the electron scanning micrograph figure of one gained composite bactericidal material of the embodiment of the present invention；
Fig. 6 is the electron scanning micrograph figure of two gained biomass carbon of the embodiment of the present invention；
Fig. 7 is the electron scanning micrograph figure of two gained composite bactericidal material of the embodiment of the present invention
Fig. 8 is the electron scanning micrograph figure of three gained biomass carbon of the embodiment of the present invention；
Fig. 9 is the electron scanning micrograph figure of three gained composite bactericidal material of the embodiment of the present invention；
Figure 10 is the electron scanning micrograph figure of four gained biomass carbon of the embodiment of the present invention；
Figure 11 is the electron scanning micrograph figure of four gained composite bactericidal material of the embodiment of the present invention；
Figure 12 is the electron scanning micrograph figure of five gained composite bactericidal material of the embodiment of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
A kind of nano-silver biological matter charcoal composite bactericidal material of the invention, the composite bactericidal material includes following parts by weight
Component: 0.8-1.2 parts of biomass carbon, 1.0-1.5 parts of nano-Ag particles；The composite bactericidal material is silver ion in reducing agent
It is obtained with biomass carbon by hydrothermal synthesis method under the action of protective agent.
Preferably, the particle size of the nano-Ag particles is 5-100nm.
Specifically, the specific surface area of the biomass carbon is 1600-2500m2The pore size of/g, the biomass carbon is
3.0-6.0nm。
Further, the biomass carbon the preparation method comprises the following steps: 1) take stalk, impregnate, drying is spare；2) pure distillation is taken
Water is added in the resulting stalk of step 1), and adds the concentrated sulfuric acid, wherein the mass ratio of distilled water, the concentrated sulfuric acid and stalk is
15-30:5-10:1-2 is uniformly mixed, and at 120-200 DEG C, reacts 10-48h, cooling；3) by the resulting stalk mistake of step 2)
Filter, is cleaned respectively using distilled water and dehydrated alcohol, dry, obtains carbonization stalk；4) by the resulting carbonization stalk of step 3)
It is mixed with active material, the mass ratio of carbonization stalk and active material is 1-2:2-4, and grinding is uniform；5) step 4) is resulting
Carbonization stalk and active material admixture at 700-800 DEG C, calcine 12-24h, obtain charcoal under inert gas shielding effect
Grain；6) hydrochloric acid and distilled water is respectively adopted in the resulting charcoal particle of step 5) to clean, then uses washes of absolute alcohol, it is dry, it grinds,
Obtain biomass carbon.
It is highly preferred that in the step 4), active material is sodium hydroxide, any one or a few in potassium hydroxide.
Further, in the step 1), stalk is impregnated in dehydrated alcohol, soaking time 7-10d；Institute
Stating stalk is corn stover, broomcorn straw, catkin, petal, Enteromorpha, any one or a few in reed；Before stalk impregnates
It is first crushed, smashed stalk particle length is 0.3-0.5cm.
More specifically, in the step 3) and the step 6), wash number when cleaning is 3-5 times.
The preparation method of a kind of nano-silver biological matter charcoal composite bactericidal material of the invention, comprising the following steps: S1: take second
Glycol, the concentrated sulfuric acid, polyvinylpyrrolidone and silver nitrate, the quality of ethylene glycol, the concentrated sulfuric acid, polyvinylpyrrolidone and silver nitrate
Than being uniformly mixed, obtaining mixed solution for 10-40:5-10:1-5:0.1-1；S2: taking biomass carbon, and it is resulting to be added to step S1
In mixed solution, the mass ratio of biomass carbon and the silver in silver nitrate used in step S1 is 0.8-1.2:1.0-1.5, and stirring obtains
Mixture；S3: by the resulting mixture of step S2, at 90-120 DEG C, reacting 12-24h, cooling, obtains reaction product；S4: will
The filtering of reaction product obtained by step S3, obtains sediment, distilled water and washes of absolute alcohol is respectively adopted, and dries, and grinding obtains compound
Sterilization material.
Preferably, in the step S3, cooling and is cooled to room temperature by the way of natural cooling；The step S4
In, wash number when cleaning is 3-5 times.
A kind of application of nano-silver biological matter charcoal composite bactericidal material of the invention, the composite bactericidal material is for drinking
The filtering and sterilization processing of water.
Embodiment one
A kind of preparation method of nano-silver biological matter charcoal composite bactericidal material of the invention, comprising the following steps:
(1) preparation of biomass carbon
1) corn stover of fresh dried is taken, core is stayed in peeling, is cut into the small pieces that length is 0.3cm, soaks using dehydrated alcohol
7d is steeped, drying is spare；
2) 1g above-mentioned steps 1 are weighed) pretreated corn stover core is added 30mL and steams in 50mL water heating kettle liner
Distilled water and the 5mL concentrated sulfuric acid are uniformly mixed, and sealing is placed in baking oven, at 180 DEG C, are reacted for 24 hours, natural cooling；
3) by above-mentioned steps 2) corn stover core filtering after resulting hydrothermal carbonization, then, it is clear that distilled water is respectively adopted
It washes, washes of absolute alcohol, each cleaning three times, is placed in baking oven dry；
4) by above-mentioned steps 3) it is dry after carbonization corn stover core, with active material, that is, potassium hydroxide (KOH) according to 1:1
Mass ratio mixing, using agate mortar, grinding is uniform；
5) by above-mentioned steps 4) in the carbonization corn stover core that is mixed with active material, be put into tube furnace, pre- logical nitrogen
(N2) 30min, to eliminate air, at 800 DEG C, calcining 12h obtains charcoal particle；
6) by above-mentioned steps 5) in calcined charcoal particle, be respectively washed three times using concentrated hydrochloric acid and distilled water, then use nothing
Water-ethanol cleans three times, dry, and grinding obtains biomass carbon.
(2) preparation of nano-silver biological matter carbon composite
S1: taking 25mL ethylene glycol, the 5mL concentrated sulfuric acid, 1g polyvinylpyrrolidone (PVP), 0.2g silver nitrate, and reaction kettle is added
In, it is uniformly mixed；
S2: the biomass carbon of 0.1g above-mentioned steps (one) preparation is weighed, is placed in the reaction kettle in above-mentioned steps S1, fills
Divide stirring；
S3: the reaction kettle of above-mentioned steps S2 is placed in baking oven, at 120 DEG C, is reacted 12h, is naturally cooled to room temperature,
Obtain reaction product；
S4: the resulting reaction product of above-mentioned steps S3 is filtered, deposit is obtained, it is clear that distilled water, dehydrated alcohol is respectively adopted
It washes, respectively three times, dries, grinding obtains composite bactericidal material.
The biomass carbon that step (1) is obtained is placed in the electronic scanner microscope of the SU8000 model of Hitachi, Ltd's production
On be scanned, gained picture is as shown in Fig. 1；And the biomass carbon for obtaining step (1) is placed in FEI Co.'s production
Tecnai G2It is scanned on the transmission electron microscope of F20S-TWIN model, gained picture is as shown in Fig. 2；Then, will
The biomass carbon that step (1) obtains carries out specific surface area and pore-size distribution test experiments respectively, as a result such as 4 institute of attached drawing 3 and attached drawing
Show；The resulting composite bactericidal material of the present embodiment is placed on above-mentioned electronic scanner microscope and is scanned, gained picture is for example attached
Shown in Fig. 5.
The biomass carbon of method of the invention preparation is porous structure, inner part it can be seen from attached drawing 1 and attached drawing 2
Many ducts are furnished with, pore size is about 3.1nm, specific surface area 2125m2/ g has the smallest aperture and maximum compares table
Area.The biomass carbon even aperture distribution of method of the invention preparation it can be seen from attached drawing 3 and attached drawing 4.It can by attached drawing 5
To find out, the comprehensive package structure biomass carbon structure of composite bactericidal material nano silver of method preparation of the invention is greatly improved
The bacteriostasis property of composite bactericidal material, gained composite bactericidal material bacteriostasis rate is high, and the antibacterial period is long, long service life.
Embodiment two
A kind of preparation method of nano-silver biological matter charcoal composite bactericidal material of the invention, comprising the following steps:
(1) preparation of biomass carbon
1) broomcorn straw for taking fresh dried is cut into the small pieces that length is 0.5cm, using soaked in absolute ethyl alcohol 10d, dries
It is dry, it is spare；
2) 1g above-mentioned steps 1 are weighed) 30mL distillation is added in 50mL water heating kettle liner in pretreated broomcorn straw
Water and the 10mL concentrated sulfuric acid are uniformly mixed, and sealing is placed in baking oven, at 120 DEG C, are reacted for 24 hours, natural cooling；
3) by above-mentioned steps 2) broomcorn straw filtering after resulting hydrothermal carbonization, then, be respectively adopted distilled water cleaning,
Washes of absolute alcohol, each cleaning three times, are placed in baking oven dry；
4) by above-mentioned steps 3) it is dry after carbonization broomcorn straw, with active material, that is, sodium hydroxide (NaOH) according to 1:1
Mass ratio mixing, using agate mortar, grinding is uniform；
5) by above-mentioned steps 4) in the carbonization broomcorn straw that is mixed with active material, be put into tube furnace, pre- logical nitrogen
(N2) 30min, to eliminate air, at 700 DEG C, calcining 12h obtains charcoal particle；
6) by above-mentioned steps 5) in calcined charcoal particle, be respectively washed three times using concentrated hydrochloric acid and distilled water, then use nothing
Water-ethanol cleans three times, dry, and grinding obtains biomass carbon.
(2) preparation of nano-silver biological matter carbon composite
S1: taking 35mL ethylene glycol, the 10mL concentrated sulfuric acid, 1g polyvinylpyrrolidone (PVP), 0.2g silver nitrate, and high pressure is added
In counteracting tank, it is uniformly mixed；
S2: the biomass carbon of 0.1g above-mentioned steps (one) preparation, the high-pressure digestion tank being placed in above-mentioned steps S1 are weighed
In, it is sufficiently stirred；
S3: the high-pressure digestion tank of above-mentioned steps S2 is placed in baking oven, at 90 DEG C, is reacted 12h, is naturally cooled to room
Temperature obtains reaction product；
S4: the resulting reaction product of above-mentioned steps S3 is filtered, deposit is obtained, it is clear that distilled water, dehydrated alcohol is respectively adopted
It washes, respectively three times, dries, grinding obtains composite bactericidal material.
The resulting biomass carbon of the present embodiment step (1) and the resulting composite bactericidal material of step (2) are respectively placed in
It is scanned on electronic scanner microscope described in embodiment one, gained picture is as shown in attached drawing 6 and attached drawing 7.
The biomass carbon of of the invention method preparation is porous structure it can be seen from attached drawing 6, inside be distributed with it is very much
Aperture, pore size are about 3.5nm, specific surface area 1812m2/g.The method of the invention preparation it can be seen from attached drawing 7
Composite bactericidal material is the comprehensive wrapping biological matter carbon structure of nano silver, forms comprehensive package structure to biomass carbon, greatly improves
The bacteriostasis property of composite bactericidal material, gained composite bactericidal material bacteriostasis rate is high, and the antibacterial period is long, long service life.
Embodiment three
A kind of preparation method of nano-silver biological matter charcoal composite bactericidal material of the invention, comprising the following steps:
(1) preparation of biomass carbon
1) catkin for taking fresh dried, using soaked in absolute ethyl alcohol 7d, drying is spare；
2) 1g above-mentioned steps 1 are weighed) pretreated catkin, in 50mL water heating kettle liner, be added 30mL distilled water and
The 10mL concentrated sulfuric acid is uniformly mixed, and sealing is placed in baking oven, at 180 DEG C, is reacted for 24 hours, natural cooling；
3) by above-mentioned steps 2) then distilled water cleaning, anhydrous is respectively adopted in catkin filtering after resulting hydrothermal carbonization
Ethyl alcohol cleaning, each cleaning three times, are placed in baking oven dry；
4) by above-mentioned steps 3) it is dry after carbonization catkin, with active material, that is, potassium hydroxide (KOH) according to the quality of 1:2
Than mixing, using agate mortar, grinding is uniform；
5) by above-mentioned steps 4) in the carbonization catkin that is mixed with active material, be put into tube furnace, pre- logical argon gas (Ar)
30min, to eliminate air, at 800 DEG C, calcining for 24 hours, obtains carbon particle；
6) by above-mentioned steps 5) in calcined carbon particle, be respectively washed three times using hydrochloric acid and distilled water, then with anhydrous
Ethyl alcohol cleans three times, dry, and grinding obtains biomass carbon.
(2) preparation of nano-silver biological matter carbon composite
S1: taking 25mL ethylene glycol, the 5mL concentrated sulfuric acid, 1g polyvinylpyrrolidone (PVP), 0.2g silver nitrate, and high pressure is added and disappears
It solves in tank, is uniformly mixed；
S2: the biomass carbon of 0.1g above-mentioned steps (one) preparation, the high-pressure digestion tank being placed in above-mentioned steps S1 are weighed
In, it is sufficiently stirred；
S3: the high-pressure digestion tank of above-mentioned steps S2 is placed in baking oven, at 90 DEG C, is reacted 18h, is naturally cooled to room
Temperature obtains reaction product；
S4: the resulting reaction product of above-mentioned steps S3 is filtered, deposit is obtained, it is clear that distilled water, dehydrated alcohol is respectively adopted
It washes, respectively three times, dries, grinding obtains composite bactericidal material.
The resulting biomass carbon of the present embodiment step (1) and the resulting composite bactericidal material of step (2) are respectively placed in
It is scanned on electronic scanner microscope described in embodiment one, gained picture is as shown in Figure 8 and Figure 9.
The biomass carbon of of the invention method preparation is porous structure it can be seen from attached drawing 8, inside be distributed with it is very much
Aperture, pore size are about 3.7nm, specific surface area 1725m2/g.The method of the invention preparation it can be seen from attached drawing 9
Nano silver is wrapped in biomass carbon comprehensively in composite bactericidal material, and nano silver not only wraps it in the outside of biomass carbon
It wraps up in, also into being filled inside the duct of biomass carbon to it, forms comprehensive package structure of biomass carbon.
Example IV
A kind of preparation method of nano-silver biological matter charcoal composite bactericidal material of the invention, comprising the following steps:
(1) preparation of biomass carbon
1) reed for taking fresh dried is cut into the segment that length is 0.4cm, and using soaked in absolute ethyl alcohol 8d, drying is standby
With；
2) 1g above-mentioned steps 1 are weighed) pretreated reed, in 50mL water heating kettle liner, be added 40mL distilled water and
The 5mL concentrated sulfuric acid is uniformly mixed, and sealing is placed in baking oven, at 200 DEG C, is reacted for 24 hours, natural cooling；
3) by above-mentioned steps 2) then distilled water cleaning, anhydrous is respectively adopted in reed filtering after resulting hydrothermal carbonization
Ethyl alcohol cleaning, each cleaning three times, are placed in baking oven dry；
4) by above-mentioned steps 3) it is dry after carbonization reed, with active material, that is, sodium hydroxide (NaOH) according to the matter of 1:4
Amount is than mixing, and using agate mortar, grinding is uniform；
5) by above-mentioned steps 4) in the carbonization reed that is mixed with active material, be put into tube furnace, pre- helium injection gas (He)
30min, to eliminate air, at 700 DEG C, calcining for 24 hours, obtains carbon particle；
6) by above-mentioned steps 5) in calcined carbon particle, be respectively washed three times using hydrochloric acid and distilled water, then with anhydrous
Ethyl alcohol cleans three times, dry, and grinding obtains biomass carbon.
(2) preparation of nano-silver biological matter carbon composite
S1: taking 35mL ethylene glycol, the 5mL concentrated sulfuric acid, 1.5g polyvinylpyrrolidone (PVP), 0.2g silver nitrate, and high pressure is added
In counteracting tank, it is uniformly mixed；
S2: the biomass carbon of 0.1g above-mentioned steps (one) preparation, the high-pressure digestion tank being placed in above-mentioned steps S1 are weighed
In, it is sufficiently stirred；
S3: the high-pressure digestion tank of above-mentioned steps S2 is placed in baking oven, at 120 DEG C, is reacted 12h, is naturally cooled to room
Temperature obtains reaction product；
S4: the resulting reaction product of above-mentioned steps S3 is filtered, deposit is obtained, it is clear that distilled water, dehydrated alcohol is respectively adopted
It washes, respectively three times, dries, grinding obtains composite bactericidal material.
The resulting biomass carbon of the present embodiment step (1) and the resulting composite bactericidal material of step (2) are respectively placed in
It is scanned on electronic scanner microscope described in embodiment one, gained picture is as shown in attached drawing 10 and attached drawing 11.
The biomass carbon of of the invention method preparation is porous structure it can be seen from attached drawing 10, inside be distributed with very
Multiple aperture, pore size are about 4.2nm, specific surface area 1688m2/g.The method of the invention preparation it can be seen from attached drawing 11
Composite bactericidal material be made of biomass carbon and nano silver, nano silver forms thicker one on the surface of biomass carbon
Layer.
Embodiment five
A kind of preparation method of nano-silver biological matter charcoal composite bactericidal material of the invention, comprising the following steps:
S1: ethylene glycol, the concentrated sulfuric acid, polyvinylpyrrolidone and silver nitrate, ethylene glycol, the concentrated sulfuric acid, polyvinylpyrrolidine are taken
The mass ratio of ketone and silver nitrate is 25:7:2:1, is uniformly mixed, obtains mixed solution；
S2: taking biomass carbon, is added in the resulting mixed solution of step 1), silver nitrate used in biomass carbon and step 1)
In silver mass ratio be 0.8:1.0, stirring, obtain mixture；
S3: by the resulting mixture of step S2, at 110 DEG C, reaction is for 24 hours, cooling, obtains reaction product；
S4: reaction product obtained by step S3 being filtered, sediment is obtained, distilled water and washes of absolute alcohol is respectively adopted, and is dried
Dry, grinding obtains composite bactericidal material.
The resulting composite bactericidal material of the present embodiment is placed on electronic scanner microscope described in embodiment one and is swept
It retouches, gained picture is as shown in Fig. 12.
The composite bactericidal material of method of the invention preparation is by biomass carbon and nano silver group it can be seen from attached drawing 12
At nano silver is grown in the surface of biomass carbon, to wrap up biomass carbon.
The embodiment of the present invention one to the resulting composite bactericidal material of embodiment five and three control samples are carried out respectively antibacterial
Experiment, experimental procedure are as follows: the strain of Escherichia coli is linked by (a) activated in LB liquid medium after, be transferred to constant temperature
It is shaken for 24 hours at 37 DEG C in concussion case；(b) it takes a certain amount of bacterium solution to be placed in sterile beaker, the nano-silver biological matter of 0.1mg is added
Charcoal composite bactericidal material or control sample；(c) it by the bacterium solution containing nano-silver biological matter charcoal composite bactericidal material and does not contain respectively
The bacterium solution of nano-silver biological matter carbon composite, to identical multiple, then, is placed in constant temperature and humidity using normal saline dilution
15h is cultivated in case；(d) observation statistics is carried out using colony counting method, and data is counted using sterilizing rate formula；Experiment
The results are shown in Table 1.Three control samples are respectively bactericidal nano-silver material, biomass carbon sterilization material and nano silver and activity
Charcoal composite bactericidal material.
The antibacterial result statistical form of the different sterilization materials of table 1
| Sterilization material | Bacteriostasis rate (%) | Antibacterial long-term effect (d) |
| Embodiment one | 99.80 | >60 |
| Embodiment two | 99.70 | 40-50 |
| Embodiment three | 99.60 | 30-45 |
| Example IV | 98.20 | 20-35 |
| Embodiment five | 98.10 | 15-30 |
| Nano silver | 90.30 | 10-25 |
| Biomass carbon | 50.10 | >60 |
| Nano-silver active carbon composite bactericidal material | 95.00 | 10-15 |
As can be seen from Table 1, the bacteriostasis rate of the obtained nano-silver biological matter charcoal composite bactericidal material of method of the invention
Three control samples are significantly better than that with long-term effect effect, this is because-OH isoreactivity the group and nanometer that are rich in biomass carbon
Silver forms stable chemical bond, slows down the release of silver ion, increases the service life of composite bactericidal material.Meanwhile this hair
The aperture of the biomass carbon of bright method preparation is big, and specific surface area is high, and the specific surface area of biomass carbon is bigger, the knot with nano silver
It is better to close effect, can more promote the fungistatic effect of composite bactericidal material.
Therefore, compared with prior art, the beneficial effects of the present invention are: biomass carbon and nano-Ag particles pass through in the present invention
It is compound to cross hydrothermal synthesis method ,-OH base isoreactivity group is rich in biomass carbon, stable chemical bond is formed with nano silver, into one
Step slows down the release of silver ion；The aperture of biomass carbon is big, and specific surface area is high, nano silver during hydrothermal synthesis not only
It is directly entered in the aperture structure of biomass carbon, is also coated on the outer surface of biomass carbon, comprehensive packet is formed to biomass carbon
Structure is wrapped up in, secondary pollution of the biomass carbon in drinking water purification process is avoided；Substantially increase the suppression of composite bactericidal material
Bacterium performance, gained composite bactericidal material bacteriostasis rate are high, additionally it is possible to go the chlorine residue in water removal, keep drinking water softer, have and kill
The double action of bacterium and disinfection, the antibacterial period is long, long service life.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of nano-silver biological matter charcoal composite bactericidal material, it is characterised in that: the composite bactericidal material includes following weight
The component of part: 0.8-1.2 parts of biomass carbon, 1.0-1.5 parts of nano-Ag particles；
The composite bactericidal material is that silver ion passes through hydrothermal synthesis method with biomass carbon under the action of reducing agent and protective agent
And it obtains.
2. nano-silver biological matter charcoal composite bactericidal material according to claim 1, it is characterised in that:
The particle size of the nano-Ag particles is 5-100nm.
3. nano-silver biological matter charcoal composite bactericidal material according to claim 1, it is characterised in that:
The specific surface area of the biomass carbon is 1600-2500m2/ g, the pore size of the biomass carbon are 3.0-6.0nm.
4. nano-silver biological matter charcoal composite bactericidal material according to claim 1, it is characterised in that: the biomass carbon
The preparation method comprises the following steps:
1) stalk is taken, is impregnated, drying is spare；
2) distilled water is taken, is added in the resulting stalk of step 1), and add the concentrated sulfuric acid, wherein distilled water, the concentrated sulfuric acid and stalk
Mass ratio be 15-30:5-10:1-2, be uniformly mixed, at 120-200 DEG C, react 10-48h, it is cooling；
3) it by the resulting straw filtering of step 2), is cleaned respectively using distilled water or dehydrated alcohol, it is dry, obtain carbonization straw
Stalk；
4) the resulting carbonization stalk of step 3) is mixed with active material, the mass ratio of carbonization stalk and active material is 1-2:2-
4, grinding is uniform；
5) by the resulting carbonization stalk of step 4) and active material admixture, under inert gas shielding effect, in 700-800 DEG C
Under, 12-24h is calcined, charcoal particle is obtained；
6) concentrated hydrochloric acid and distilled water is respectively adopted in the resulting charcoal particle of step 5) to clean, then uses washes of absolute alcohol, dried, grind
Mill, obtains biomass carbon.
5. nano-silver biological matter charcoal composite bactericidal material according to claim 4, it is characterised in that:
In the step 4), active material is sodium hydroxide, any one or a few in potassium hydroxide.
6. nano-silver biological matter charcoal composite bactericidal material according to claim 5, it is characterised in that:
In the step 1), stalk is impregnated in dehydrated alcohol, soaking time 7-10d；
The stalk is corn stover, broomcorn straw, catkin, petal, Enteromorpha, any one or a few in reed；
Stalk is first crushed before impregnating, and smashed stalk particle length is 0.3-0.5cm.
7. nano-silver biological matter charcoal composite bactericidal material according to claim 5, it is characterised in that:
In the step 3) and the step 6), wash number when cleaning is 3-5 times.
8. the preparation method of nano-silver biological matter charcoal composite bactericidal material according to any one of claims 1-7,
It is characterized in that: the following steps are included:
S1: taking ethylene glycol, the concentrated sulfuric acid, polyvinylpyrrolidone and silver nitrate, ethylene glycol, the concentrated sulfuric acid, polyvinylpyrrolidone and
The mass ratio of silver nitrate is 10-40:5-10:1-5:0.1-1, is uniformly mixed, obtains mixed solution；
S2: taking biomass carbon, is added in the resulting mixed solution of step S1, in silver nitrate used in biomass carbon and step S1
The mass ratio of silver is 0.8-1.2:1.0-1.5, and stirring obtains mixture；
S3: by the resulting mixture of step S2, at 90-120 DEG C, reacting 12-24h, cooling, obtains reaction product；
S4: reaction product obtained by step S3 being filtered, sediment is obtained, distilled water and washes of absolute alcohol is respectively adopted, and is dried, is ground
Mill, obtains composite bactericidal material.
9. the preparation method of nano-silver biological matter charcoal composite bactericidal material according to claim 8, it is characterised in that:
In the step S3, cooling and is cooled to room temperature by the way of natural cooling；In the step S4, when cleaning
Wash number is 3-5 times.
10. the application of nano-silver biological matter charcoal composite bactericidal material according to any one of claims 1-7, feature
It is:
The composite bactericidal material is used for the filtering and sterilization processing of drinking water.
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| CN110550709A (en) * | 2019-08-29 | 2019-12-10 | 重庆大学 | Bactericidal biochar loaded with silver particles and preparation method thereof |
| CN115319090A (en) * | 2022-08-26 | 2022-11-11 | 苏州工业园区安泽汶环保技术有限公司 | Preparation method of efficient microparticle carbon-coated silver-zinc nano microsphere antibacterial material |
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| CN105753115A (en) * | 2016-04-19 | 2016-07-13 | 陈守刚 | Triple sterilizing composite and preparation method thereof |
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| CN115319090B (en) * | 2022-08-26 | 2023-12-26 | 苏州工业园区安泽汶环保技术有限公司 | Preparation method of efficient micro-granularity carbon-coated silver-zinc nano microsphere antibacterial material |
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