CN106925216A - One kind carries silver TiO2Modification bamboo charcoal material and preparation method thereof - Google Patents
One kind carries silver TiO2Modification bamboo charcoal material and preparation method thereof Download PDFInfo
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- CN106925216A CN106925216A CN201710207131.0A CN201710207131A CN106925216A CN 106925216 A CN106925216 A CN 106925216A CN 201710207131 A CN201710207131 A CN 201710207131A CN 106925216 A CN106925216 A CN 106925216A
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- bamboo charcoal
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- 239000011425 bamboo Substances 0.000 title claims abstract description 73
- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 71
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 71
- 241001330002 Bambuseae Species 0.000 title claims abstract description 71
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 71
- 239000003610 charcoal Substances 0.000 title claims abstract description 69
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000004332 silver Substances 0.000 title claims abstract description 35
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000012986 modification Methods 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 18
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 15
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 230000033228 biological regulation Effects 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 230000004048 modification Effects 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 23
- 230000000694 effects Effects 0.000 abstract description 11
- 238000013016 damping Methods 0.000 abstract description 8
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 239000011941 photocatalyst Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 230000001954 sterilising effect Effects 0.000 abstract description 4
- 230000000295 complement effect Effects 0.000 abstract description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 14
- 238000001035 drying Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 239000008187 granular material Substances 0.000 description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 8
- 229910017604 nitric acid Inorganic materials 0.000 description 8
- 230000005764 inhibitory process Effects 0.000 description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000005352 clarification Methods 0.000 description 4
- 239000000693 micelle Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 235000016588 Rosa centifolia Nutrition 0.000 description 2
- 244000052585 Rosa centifolia Species 0.000 description 2
- -1 Titanium alkoxides Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000001143 conditioned effect Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000000452 restraining effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000013265 porous functional material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007614 solvation Methods 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B01J35/39—
Abstract
Silver TiO is carried the present invention relates to one kind2Modification bamboo charcoal material and preparation method thereof, described load silver TiO2Modification bamboo charcoal material is made up of following steps：(1) weigh butyl titanate to mix with a part of absolute ethyl alcohol, add silver nitrate crystal, pH is to 4~5 for regulation, obtains mixed liquor A；(2) remainder absolute ethyl alcohol and deionized water mixing are weighed, pH is to 1 2.5 for regulation, obtains mixed liquid B；(3) it is stirred vigorously down, mixed liquid B is added in mixed liquor A, stir to transparent clear sol is formed, add bamboo-carbon powder, stirring reaction is to forming gel；(4) gel that obtains step (3) is aging, dry, calcining, and the load silver TiO is obtained after cooling2Modification bamboo charcoal material.Compared with prior art, porous adsorption function and silver-carrying nano TiO of the composite of the invention with bamboo charcoal2Visible light catalytic sterilizing function, both can act synergistically, have complementary advantages so that composite has excellent absorption damping and photo-catalyst effect etc..
Description
Technical field
The present invention relates to a kind of modification bamboo charcoal material, silver TiO is carried more particularly, to one kind2Modification bamboo charcoal material and its preparation
Method.
Background technology
With the improvement of people ' s living standards, environmental protection and health are increasingly becoming the topic of people's common concern, and people are to ring
The requirement of border comfort level also more and more higher, therefore the development and application of types of functionality material also has become a focus.Bamboo charcoal
It is a kind of porous functional material, because its pore structure is flourishing, high adsorption capacity, thus it is widely used in air and water quality is net
Change, environment damping etc..TiO2It is a kind of nano-photocatalyst, is acted on good photo-catalyst, but it is only capable of absorbing profit
With ultraviolet light, the utilization rate to visible ray is extremely low, additionally, TiO2Poor adsorptivity, easy reunion are also there is when directly using, is returned
Receive the shortcomings of recycling difficult.By by bamboo charcoal and nano-TiO2It is compound, in combination with TiO2Load pale rose colour move modification technology, then may be used
To solve these problems well, one side bamboo charcoal can solve nano-TiO2Adsorption capacity is poor, be easy to the problems such as reuniting, another
Aspect nano-TiO2Photocatalysis Decomposition effect can solve the problems, such as the adsorption saturation of bamboo charcoal, therefore both can act synergistically,
Have complementary advantages.So that not only there is composite good absorption damping to act on, and it is sterilized with good visible light catalytic
Effect, Related product can be used for purification of air, restraining and sterilizing bacteria and environment damping etc. in architecture indoor, with well using preceding
Scape.
As number of patent application is a kind of for the Chinese patent application of " 200410037684.9 " is disclosed can antibacterial be degerming receives
Rice modification bamboo charcoal, it mainly with bamboo charcoal, nano titanium oxide and nano titanium dioxide anti-bacterial agent as raw material, it is blended, stirring,
The series of process such as evaporation, dry is made, and the method is a kind of physical method, is not related to chemical reaction, therefore not strong for load solid,
Combined efficiency is not high, and red shift modification of the titanium dioxide without absorption spectrum in the nano modified bamboo charcoal sterilization material, its
Bactericidal effect under visible light is weaker.
For another example number of patent application for " 201210250146.2 " Chinese patent application disclose a kind of modifying titanium dioxide/
Bamboo charcoal composite material and preparation method thereof, it prepares TiO using sol-gel process first2Colloidal sol, then sonicated, high temperature
Calcining and other processes first obtain TiO2- bamboo charcoal composite material, finally recycles silver nitrate to see that the characteristics of light is decomposed loads elemental silver
On titanium dioxide-bamboo charcoal, nano-TiO is finally obtained2/ Ag/ bamboo charcoal composite materials.The method is by TiO2With bamboo charcoal it is compound with
Silver-carrying modified substep is carried out, and there is complex technical process, relatively costly defect, and the patent concern is primarily with composite
The effect of degradable organic pollutant, is not directed to its sterilized and damping effect.
The content of the invention
The purpose of the present invention is exactly that a kind of load silver TiO is provided for the defect for overcoming above-mentioned prior art to exist2It is modified
Bamboo charcoal material and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
One kind carries silver TiO2Modification bamboo charcoal material, including with mass ratio 3-10:100 compound load silver TiO2Component and bamboo charcoal
Component, described load silver TiO2In component, silver-colored and TiO2Mass ratio be 2-5:100.
Carry silver TiO2The preparation method of modification bamboo charcoal material, comprises the following steps：
(1) weigh butyl titanate to mix with a part of absolute ethyl alcohol, add silver nitrate crystal, pH is to 4~5 for regulation,
Obtain mixed liquor A；
(2) remainder absolute ethyl alcohol and deionized water mixing are weighed, pH is to 1-2.5 for regulation, obtains mixed liquid B；
(3) it is stirred vigorously down, mixed liquid B is added in mixed liquor A, stir to transparent clear sol is formed, adds
Bamboo-carbon powder, stirring reaction is to forming gel；
(4) gel that obtains step (3) is aging, dry, calcining, and the load silver TiO is obtained after cooling2Modification bamboo charcoal
Material.
Preferably, in step (1) and step (2)：The mol ratio of absolute ethyl alcohol, deionized water and butyl titanate is (12
~15)：(30~50)：1, the mass ratio of silver nitrate and butyl titanate is (0.75~1.85)：100, wherein, in step (1)
The absolute ethyl alcohol of addition is (1-2) with the volume ratio of the absolute ethyl alcohol of addition in step (2)：1.
Preferably, the bamboo-carbon powder particle diameter for being added in step (3) is 100~400 mesh, and specific surface area is more than 100m2·g-1。
Preferably, bamboo-carbon powder and the mass ratio of butyl titanate are (2.5~8)：1.
Preferably, the calcine technology condition in step (4) is：Calcining heat be 400 DEG C~600 DEG C, calcination time be 2~
3h。
Preferably, also by pretreatment before bamboo-carbon powder is added in step (3), the pretreatment is specially：By pending bamboo
Charcoal boils in adding deionized water, then cleans filtering, so repeatedly.
Preferably, mixing speed is 800~1000rpm in step (3), and mixed liquid B feed postition is disposable all fast
Speed is added in mixed liquor A.
Be dispersed in Titanium alkoxides in anhydrous ethanol solvent form presoma first, so by the present invention in preparation process
The reaction dissolvents such as deionized water are added afterwards, make solute that the series reactions such as hydrolysis or alcoholysis, polycondensation and complexing occur with solvent, it is raw
Particle being gathered into thing and forming colloidal sol, colloidal sol is dried by evaporation and is changed into gel, gel is thermally treated again to obtain composite wood
Material.And bamboo charcoal particle can be as the carrier of nano-particle, for it provides attachment site, therefore both can realize combining closely,
Synergy.
In preparation process, preparation condition is to TiO2The performances such as crystalline structure, the particle diameter of crystal and composite pattern, hole
The influence such as structure is very big.When wherein absolute ethyl alcohol addition is very few, Titanium alkoxides excessive concentration, hydrolytie polycondensation production concentration is too high,
Easily cause aggregation or the precipitation of particle, addition is excessive, and gel time can be extended again；Amount of water is few, then hydrolysis of alkoxide speed
Slowly, gel time is long, influences the structure of product, and amount of water can excessively reduce the concentration of condensation polymer so that between monomer
Collision probability reduction, also causes gel time long；The pH value of solution is lower, and micelle surface charge is more, between micelle
Repulsive force is also bigger, colloidal sol just relatively stablize, gel time is also more long, and pH value it is excessive when, reduce the solvation of sol surface
Layer, micelle surface charge is reduced, and the repulsive force between micelle diminishes, TiO2The gelling time of colloidal sol shortens, and colloidal sol is more unstable；
To TiO when silver carrying amount is too low2The raising DeGrain of photocatalytic activity, bactericidal effect is also weak, and silver particles are simultaneously when too high
It is likely to turn into TiO2Light induced electron and the complex centre in hole, reduce TiO2Photo-catalyst activity, while also not enough warp
Ji；For carrying silver TiO2The selection of load capacity on bamboo charcoal, if when very few, bactericidal effect is not obvious, because bamboo charcoal is deposited when too high
In load saturation problem so that nano-particle is easily reunited, activity is reduced, it is also possible to block bamboo charcoal hole, reduces specific surface area；For
The selection of bamboo charcoal particle diameter, if particle diameter is excessive, specific surface area is smaller, and saturation load capacity is small, and combines not firm enough；Particle diameter is too small
When, particle is easy to reunite, and reduces specific surface area, and same composite effect is undesirable；Finally for the control of calcining heat and time,
If calcining heat is too low or during the too short time, TiO2Photocatalytic activity highest anatase crystal can not be more changed into；Forge
When burning too high temperature or overlong time, TiO2Crystal formation may be converted into relatively low rutile-type of photocatalytic activity etc. again.Therefore, with
Upper each reactant consumption and technological parameter must be controlled in rational scope.
This patent is related to a kind of load silver TiO with sterilized, humidity under visible ray2The preparation of-bamboo charcoal composite material
Method, the absorption humidity and load silver TiO of composite prepared by the method with bamboo charcoal2Visible light catalytic bactericidal properties
Can, architecture indoor is can be applied to for environment damping, purification of air, restraining and sterilizing bacteria etc., with good application prospect.In addition originally
Technical process can be by nano-TiO2Silver-carrying modified and its load on bamboo charcoal disposably complete, technical process is simple, prepares
Cycle is shorter, and cost is relatively low.
Compared with prior art, the present invention is by by bamboo charcoal and nano-TiO2It is compound, take full advantage of the porous suction of bamboo charcoal
Attached performance and nano-TiO2Photocatalysis performance, in combination with nano-TiO2Load pale rose colour move modification technology, improve nanometer
TiO2To the utilization rate of visible ray, make it that also there is good photo-catalyst effect under visible light.Additionally, bamboo charcoal is used as load
Body can well solve nano-TiO2Adsorption capacity is poor, be easy to the problems such as reuniting, on the other hand using load silver TiO2Photocatalysis
Decomposition can rapidly decompose the organic matter that bamboo Charcoal Adsorption comes, and the adsorption saturation of bamboo charcoal is solved the problems, such as well, because
Both can act synergistically for this, have complementary advantages, and give play to effect of maximum so that not only there is composite good absorption to adjust
Wet effect, and with good visible light catalytic bactericidal effect.
Brief description of the drawings
Fig. 1 is preparation flow figure of the invention；
Fig. 2 is the Bactericidal test comparative result figure of embodiment 1；
Fig. 3 is the Bactericidal test comparative result figure of embodiment 2.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
Bamboo charcoal is pre-processed：From 400 mesh bamboo charcoals, bamboo charcoal is boiled 30 minutes with deionized water first, then it is clear with deionized water
Wash, filter, be so repeated 3 times, it is standby after being dried in thermostatic drying chamber at 105 DEG C.
8ml butyl titanate liquid is taken, after adding 12ml absolute ethyl alcohols well mixed, 0.12g silver nitrate crystals is added,
The pH that mixed liquor is adjusted with nitric acid is 5.0, is uniformly mixing to obtain mixed liquor A；It is another to take 8ml ethanol solutions, add 18ml to go
Ionized water, it is 2.0 to adjust pH value of solution with nitric acid, is uniformly mixing to obtain mixed liquid B；It is under violent stirring, mixed liquid B is quick
It is added in mixed liquor A, persistently stirs some time, the colloidal sol until forming transparent clarification is subsequently adding 25g after pretreatment
Bamboo-carbon powder, then be sufficiently stirred for until formed gel；Above-mentioned gel is placed in air and is spontaneously dried aging 1 day, then with perseverance
Warm drying box in drying 1 day at 105 DEG C, finally by xerogel it is levigate after, be put into high temperature furnace the anoxybiotic under 450 DEG C of calcining heats
Calcining 2h, obtains carrying silver-colored TiO after cooling2Modification bamboo charcoal composite granule.
Obtained load silver TiO2The conditioned performance test of modification bamboo charcoal composite granule, it is flat under 50% relative humidities
Weighing apparatus water capacity is 6% or so, and the equilibrium moisture content under 90% relative humidities is 10% or so, and damping works well.
Composite granule is under visible light to the bactericidal property of Escherichia coli through inhibition zone method test result below figure 2, it is seen that
Pure bamboo charcoal there is no bactericidal effect, not have inhibition zone around it, and composite granule has stronger bactericidal property, around it
It is observed that there is obvious inhibition zone.
Embodiment 2
Bamboo charcoal is pre-processed：From 500 mesh bamboo charcoals, bamboo charcoal is boiled 30 minutes with deionized water first, then it is clear with deionized water
Wash, filter, be so repeated 3 times, it is standby after being dried in thermostatic drying chamber at 105 DEG C.
8ml butyl titanate liquid is taken, after adding 12ml absolute ethyl alcohols well mixed, 0.1g silver nitrate crystals is added,
The pH that mixed liquor is adjusted with nitric acid is 4.5, is uniformly mixing to obtain mixed liquor A；It is another to take 8ml ethanol solutions, add 18ml to go
Ionized water, it is 2.0 to adjust pH value of solution with nitric acid, is uniformly mixing to obtain mixed liquid B；It is under violent stirring, mixed liquid B is quick
It is added in mixed liquor A, persistently stirs some time, the colloidal sol until forming transparent clarification is subsequently adding 40g after pretreatment
Bamboo-carbon powder, then be sufficiently stirred for until formed gel；Above-mentioned gel is placed in air and is spontaneously dried aging 1 day, then with perseverance
Warm drying box in drying 1 day at 105 DEG C, finally by xerogel it is levigate after, be put into high temperature furnace the anoxybiotic under 550 DEG C of calcining heats
Calcining 2.5h, obtains carrying silver-colored TiO after cooling2Modification bamboo charcoal composite granule.
Obtained load silver TiO2The conditioned performance test of modification bamboo charcoal composite granule, it is flat under 50% relative humidities
Weighing apparatus water capacity is 7% or so, and the equilibrium moisture content under 90% relative humidities is 12% or so, and damping works well.
Composite granule is under visible light to the bactericidal property of Escherichia coli through inhibition zone method test result below figure 3：It can be seen that
Pure bamboo charcoal there is no bactericidal effect, not have inhibition zone around it, and composite granule has stronger bactericidal property, around it
It is observed that there is obvious inhibition zone.
Embodiment 3
Bamboo charcoal is pre-processed：From 400 mesh bamboo charcoals, bamboo charcoal is boiled 30 minutes with deionized water first, then it is clear with deionized water
Wash, filter, be so repeated 3 times, it is standby after being dried in thermostatic drying chamber at 105 DEG C.
0.02mol butyl titanate liquid is taken, after adding 0.12mol absolute ethyl alcohols well mixed, 0.051g nitre is added
Sour silver crystal, the pH that mixed liquor is adjusted with nitric acid is 5.0, is uniformly mixing to obtain mixed liquor A；Separately take 0.12mol absolute ethyl alcohols molten
Liquid, adds 0.6mol deionized waters, and it is 2.5 to adjust pH value of solution with nitric acid, is uniformly mixing to obtain mixed liquid B；In violent stirring
Under, mixed liquid B is added rapidly in mixed liquor A, some time is persistently stirred, the colloidal sol until forming transparent clarification, then
17.016g bamboo-carbon powders after pretreatment are added, then is sufficiently stirred for until forming gel；Above-mentioned gel is placed in air certainly
So dry aging 1 day, then with thermostatic drying chamber at 105 DEG C drying 1 day, finally by xerogel it is levigate after, be put into high temperature furnace
Anoxybiotic calcining 2h, obtains carrying silver-colored TiO after cooling under 450 DEG C of calcining heats2Modification bamboo charcoal composite granule.
Embodiment 4
Bamboo charcoal is pre-processed：From 400 mesh bamboo charcoals, bamboo charcoal is boiled 30 minutes with deionized water first, then it is clear with deionized water
Wash, filter, be so repeated 3 times, it is standby after being dried in thermostatic drying chamber at 105 DEG C.
0.02mol butyl titanate liquid is taken, after adding 0.2mol absolute ethyl alcohols well mixed, 0.1259g nitre is added
Sour silver crystal, the pH that mixed liquor is adjusted with nitric acid is 4, is uniformly mixing to obtain mixed liquor A；0.1mol ethanol solutions separately are taken,
1mol deionized waters are added, it is 1 to adjust pH value of solution with nitric acid, is uniformly mixing to obtain mixed liquid B；Under violent stirring, will be mixed
Close liquid B to be added rapidly in mixed liquor A, persistently stir some time, the colloidal sol until forming transparent clarification is subsequently adding
54.45g bamboo-carbon powders after pretreatment, then be sufficiently stirred for until forming gel；Above-mentioned gel is placed in air and is done naturally
Dry aging 1 day, then with thermostatic drying chamber in drying 1 day at 105 DEG C, finally by xerogel it is levigate after, be put into high temperature furnace 450
Anoxybiotic calcining 2h, obtains carrying silver-colored TiO after cooling under DEG C calcining heat2Modification bamboo charcoal composite granule.
The above-mentioned description to embodiment is to be understood that and use invention for ease of those skilled in the art.
Person skilled in the art obviously can easily make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to above-described embodiment, ability
Field technique personnel announcement of the invention, does not depart from improvement that scope made and modification all should be of the invention
Within protection domain.
Claims (9)
1. it is a kind of to carry silver TiO2The preparation method of modification bamboo charcoal material, it is characterised in that comprise the following steps：
(1) weigh butyl titanate to mix with a part of absolute ethyl alcohol, add silver nitrate crystal, pH is to 4~5 for regulation, obtains
Mixed liquor A；
(2) remainder absolute ethyl alcohol and deionized water mixing are weighed, pH is to 1-2.5 for regulation, obtains mixed liquid B；
(3) it is stirred vigorously down, mixed liquid B is added in mixed liquor A, stir to transparent clear sol is formed, adds bamboo charcoal
Powder, stirring reaction is to forming gel；
(4) gel that obtains step (3) is aging, dry, calcining, and the load silver TiO is obtained after cooling2Modification bamboo charcoal material.
2. one kind according to claim 1 carries silver TiO2The preparation method of modification bamboo charcoal material, it is characterised in that step (1)
In step (2)：The mol ratio of absolute ethyl alcohol, deionized water and butyl titanate is (12~15)：(30~50)：1, silver nitrate
It is (0.75~1.85) with the mass ratio of butyl titanate：100.
3. one kind according to claim 2 carries silver TiO2The preparation method of modification bamboo charcoal material, it is characterised in that step (1)
The absolute ethyl alcohol of middle addition is (1-2) with the volume ratio of the absolute ethyl alcohol of addition in step (2)：1.
4. one kind according to claim 1 carries silver TiO2The preparation method of modification bamboo charcoal material, it is characterised in that step (3)
The bamboo-carbon powder particle diameter of middle addition is 100~400 mesh, and specific surface area is more than 100m2·g-1。
5. one kind according to claim 1 carries silver TiO2The preparation method of modification bamboo charcoal material, it is characterised in that bamboo charcoal powder
Body is (2.5~8) with the mass ratio of butyl titanate：1.
6. one kind according to claim 1 carries silver TiO2The preparation method of modification bamboo charcoal material, it is characterised in that step (4)
In calcine technology condition be：Calcining heat is 400 DEG C~600 DEG C, and calcination time is 2~3h.
7. one kind according to claim 1 carries silver TiO2The preparation method of modification bamboo charcoal material, it is characterised in that step (3)
Middle bamboo-carbon powder also passes through pretreatment before adding, and the pretreatment is specially：Boiled during pending bamboo charcoal is added into deionized water, then
Cleaning filtering, so repeatedly.
8. one kind according to claim 1 carries silver TiO2The preparation method of modification bamboo charcoal material, it is characterised in that step (3)
Middle mixed liquid B feed postition is all quickly adding into mixed liquor A for disposable, while do not stop stirring, mixing speed is 800~
1000rpm。
9. the load silver TiO being made of the preparation method as described in claim 1-8 is any2Modification bamboo charcoal material, it is characterised in that its
Including with mass ratio 3-10:100 compound load silver TiO2Component and bamboo charcoal component, described load silver TiO2In component, silver-colored and TiO2
Mass ratio be 2-5:100.
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Application publication date: 20170707 |