CN107668032A - Antibacterial white cabon black composite and preparation method thereof - Google Patents
Antibacterial white cabon black composite and preparation method thereof Download PDFInfo
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- CN107668032A CN107668032A CN201710912271.8A CN201710912271A CN107668032A CN 107668032 A CN107668032 A CN 107668032A CN 201710912271 A CN201710912271 A CN 201710912271A CN 107668032 A CN107668032 A CN 107668032A
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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
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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
- A01N59/20—Copper
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- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
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- Environmental Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to a kind of antibacterial white cabon black composite and preparation method thereof.The antibacterial white cabon black is using graphene, white carbon as matrix, and one or both of incorporation antiseptic elements Zn, Cu, Ag, Ti element, its preparation method comprises the steps：（1）Antibacterial ion solution allocation；（2）Two step hybrid reactions；（3）Separation of solid and liquid and drying；（4）Post processing.In the present invention, the interspersed aggregation that can effectively suppress material itself mutually of graphene and white carbon, so as to obtain high degree of dispersion and white carbon be in nano-scale composite；Novel antibacterial white carbon has antibiotic property and reinforcement dual-use function, meets the needs for requiring some products of antibacterial functions；The graphene oxide solution of low ph value is used as one of reaction raw materials, the process problem for solving spent acid waste water is green.In addition, low cost of raw materials, economical cost-effective, preparation technology is simple, it is easy to accomplish industrialization production and application.
Description
Technical field
The present invention relates to the preparation field of high dispersive antimicrobial composite material, specifically a kind of antibacterial white cabon black composite
Preparation method.
Background technology
White carbon is precipitated silica, is a kind of white non-toxic, amorphous fine powder, has porous, resistance to height
The features such as warm, fire-retardant, light and chemical purity is high, with its superior chemical stability, reinforcing, thickening property, thixotropy in rubber
Glue, coating, plastics, paint, Chinese white, weaving, papermaking, agricultural chemicals, synthetic resin and food additives etc. are daily and chemical industry work
It is used widely in industry field.
The preparation method of white carbon mainly has the precipitation method, vapor phase method.In the market is most commonly used that with the white of precipitation method production
Carbon black, the method production cost is relatively low, and technique is simple, but product cut size is big, activity is relatively low, specific surface area is small, product quality is low etc..
Graphene is incorporated into precipitated silica, plays both excellent physical and chemical performances, the more excellent high score of processability
Dissipate composite.
At present, inorganic antiseptic and white carbon black product and production technology have all reached higher level.Inorganic antiseptic is
Refer to using materials such as surface area is big, good dispersion, porosity are high zeolite, silica gel, activated carbon or ceramics as carrier, by silver, copper,
Zinc and by the emperor himself plasma are attached to carrier surface and the powder body material with antibacterial functions are made.But these antiseptics are not mended because of it
Powerful, therefore cannot function as reinforcing agent and be added in the products such as rubber.Common white carbon can only be as the addition of common product
Agent or reinforcing agent are added in the products such as rubber, can not meet the needs for requiring some products of antibacterial functions.
The content of the invention
In order to solve above-mentioned existing technical problem, the present invention proposes a kind of antibacterial white cabon black composite and its preparation side
Method, the no added any surfactant of this method, obtain that dispersion effect is more preferable, purity is high, specific surface area is big and high catalytic activity,
And there is certain anti-microbial property, technique is simple, and cost is low, it is easy to accomplish industrialization production and application.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of antibacterial white cabon black composite, using white carbon, graphene complex as carrier, silver, zinc, copper, titanium one kind therein
Or two metal ion species be attached to carrier surface, antibacterial white cabon black composite is made.
A kind of preparation method of antibacterial white cabon black composite, comprises the steps：
（1）Antibacterial ion solution allocation：Configuration concentration is 0.05~0.10mol/L Ag+Solution, Zn2+Solution, Cu2+Solution,
Concentration is 1.00~5.00mol/L Ti4+Solution, it is stand-by；
（2）Hybrid reaction：The graphene oxide solution of the low ph value of hummers methods preparation is taken, adds pure water, adjusts the matter of solution
It is 0.01~2% to measure concentration, and pH value is 2~5, stand-by after stirring；
（3）Hybrid reaction：According to sodium silicate：Graphene oxide is 15~1：1 mass ratio weighs sodium silicate solution, by volume
For 3:1~5:1, measure step（1）The mixed liquor of any one antibacterial ion solution or any two kinds of antibacterial ion solution, stirring
After uniformly, mixed liquor is instilled into step（2）Sulfur acid graphene oxide solution in, further according to actual conditions instill sulfuric acid or
Hydrochloric acid, the pH for adjusting mixed liquor is 4~7, continues to stir, and ultrasound 0.3~2 hour, obtains containing single antiseptic elements or contains it
In two kinds of elements colloidal solution, it is stand-by；
（4）Separation of solid and liquid and drying：By step（3）Obtained colloidal sol, after filtered, centrifuging process carries out separation of solid and liquid processing,
Obtain the antibacterial white cabon black composite predecessor of paste body shape；
（5）Post processing：By step（4）Novel antibacterial white carbon black composite material is finally made through calcination processing in obtained predecessor.
The mutually interspersed of above-mentioned technical proposal, graphene and white carbon reduces both reunions of itself, incorporation antibacterial from
Son, while increasing material activity, expand material specific surface area, there is antibiotic property, and solve hummers methods production graphene
During spent acid waste water process problem, it is green, it is energy-efficient.
Using the present invention of above-mentioned technical proposal, compared with prior art, its advantage is：
1. novel antibacterial white carbon nano particle is uniformly dispersed, there is antibiotic property and reinforcement dual-use function, satisfaction requires anti-
The needs of some products of bacterium function；
2. product particle size is controllable, and lower cost for material, economical cost-effective, preparation technology is simple, therefore is easily achieved
Industrialization production and application；
3. material realizes waste material recycling, green.
Further, preferred scheme of the present invention is：
The step（3）Middle sodium silicate is the one or more in sodium metasilicate, potassium silicate, lithium metasilicate.
The step（4）Middle centrifugal separation process reaches separation of solid and liquid purpose using various centrifuge, filter press.
The step（4）Middle drying process is divided into：1）Freeze-drying condition is：Freeze temperature maintains -50~30 DEG C, freezes
The dry h of time 10~40,1~300Pa of vacuum；2）Spray drying condition is：Inlet temperature is 100~350 DEG C, outlet temperature
For 40~150 DEG C, used dried medium is hot-air.
The step（5）Middle calcine technology is in argon hydrogen gaseous mixture（95：5）Under protective condition, 300~600 DEG C are warming up to,
2~6h is incubated, after reaction terminates, drops to room temperature in gas shield.
Embodiment
The present invention is further elaborated with reference to embodiments, but embodiment does not form any restrictions to the present invention.
Embodiment 1：
（1）Antibacterial ion solution allocation：Configuration concentration is 0.05~0.10mol/L ZnSO4It is solution, stand-by；
（2）Hybrid reaction：The graphene oxide solution of the low ph value of hummers methods preparation is taken, adds pure water, adjusts the matter of solution
It is 1% to measure concentration, and pH value is 2~5, stand-by after stirring；
（3）Hybrid reaction：According to sodium silicate：Graphene oxide is 1：1 mass ratio weighs sodium silicate solution, is by volume 3:
1~5:1, measure ZnSO4Solution, after mixing, stir, mixed liquor is instilled in the graphene oxide solution of sulfur acid, then
Sulfuric acid or hydrochloric acid are instilled according to actual conditions, the pH for adjusting mixed liquor is 4~7, continues to stir, and ultrasound 0.3~2 hour, is obtained
Colloidal solution containing zinc ion, it is stand-by；
（4）Separation of solid and liquid and drying：The colloidal sol that will be obtained, filtered, centrifuging process carry out separation of solid and liquid, the solid warp after separation
After drying process, antibacterial white cabon black composite predecessor is obtained；
（5）Post processing：By obtained predecessor in argon hydrogen gaseous mixture（95：5）Under protective condition, 400 DEG C are warming up to, is incubated 2 h,
After reaction terminates, drop to room temperature in gas shield, finally the obtained antibacterial white cabon black composite containing Zn-ef ficiency.
Embodiment 2：
（1）Antibacterial ion solution allocation：Configuration concentration is 0.05~0.10mol/L CuSO4It is solution, stand-by；
（2）Hybrid reaction：The graphene oxide solution of the low ph value of hummers methods preparation is taken, adds pure water, adjusts the matter of solution
It is 1% to measure concentration, and pH value is 2~5, stand-by after stirring；
（3）Hybrid reaction：According to sodium silicate：Graphene oxide is 1：1 mass ratio weighs sodium silicate solution, is by volume 3:
1~5:1, measure CuSO4Solution, after mixing, stir, mixed liquor is instilled in the graphene oxide solution of sulfur acid, then
Sulfuric acid or hydrochloric acid are instilled according to actual conditions, the pH for adjusting mixed liquor is 4~7, continues to stir, and ultrasound 0.3~2 hour, is obtained
The colloidal solution of copper ions, it is stand-by；
（4）Separation of solid and liquid and drying：The colloidal sol that will be obtained, filtered, centrifuging process carry out separation of solid and liquid, the solid warp after separation
After drying process, antibacterial white cabon black composite predecessor is obtained；
（5）Post processing：By obtained predecessor in argon hydrogen gaseous mixture（95：5）Under protective condition, 400 DEG C are warming up to, is incubated 2 h,
After reaction terminates, drop to room temperature in gas shield, finally the obtained antibacterial white cabon black composite containing copper.
Embodiment 3：
（1）Antibacterial ion solution allocation：Configuration concentration is 0.05~0.10mol/L ZnSO4Solution and CuSO4Solution, by two
The ZnSO of the same concentration of kind4Solution and CuSO4Solution presses 1:1 ratio mixing is stand-by；
（2）Hybrid reaction：The graphene oxide solution of the low ph value of hummers methods preparation is taken, adds pure water, adjusts the matter of solution
It is 1% to measure concentration, and pH value is 2~5, stand-by after stirring；
（3）Hybrid reaction：According to sodium silicate：Graphene oxide is 1：1 mass ratio weighs sodium silicate solution, is by volume 3:
1~5:1, measure above-mentioned configured good Zn2+-Gu2+Antibacterial ion mixed liquor, after mixing, stir, mixed liquor is instilled
In the graphene oxide solution of sulfur acid, sulfuric acid or hydrochloric acid are instilled further according to actual conditions, the pH for adjusting mixed liquor is 4~7, after
Continuous stirring, ultrasound 0.3~2 hour, obtains the colloidal solution of the ion containing Zn-Cu, stand-by；
（4）Separation of solid and liquid and drying：The colloidal sol that will be obtained, filtered, centrifuging process carry out separation of solid and liquid, the solid warp after separation
After drying process, antibacterial white cabon black composite predecessor is obtained；
（5）Post processing：By obtained predecessor in argon hydrogen gaseous mixture（95：5）Under protective condition, 400 DEG C are warming up to, is incubated 2 h,
After reaction terminates, drop to room temperature in gas shield, finally the obtained antibacterial white cabon black of plyability containing Zn-Cu.
It the above is only the preferred embodiments of the present invention, it is noted that although having made in detail to the present invention with reference to preferred embodiment
Describe in detail it is bright, to those of ordinary skill in the art, any improvement in the present invention, in product of the present invention each raw material etc.
Effect replacement, modification of embodiment etc., all fall within protection scope of the present invention.
Claims (6)
- A kind of 1. antibacterial white cabon black composite, it is characterised in that：Using white carbon, graphene complex as carrier, silver, zinc, copper, Titanium one or two kinds of metal ions therein are attached to carrier surface, and antibacterial white cabon black composite is made.
- 2. a kind of preparation method of antibacterial white cabon black composite as claimed in claim 1, it is characterised in that including following steps Suddenly：（1）Antibacterial ion solution allocation：Configuration concentration is 0.05~0.10mol/L Ag+Solution, Zn2+Solution, Cu2+Solution is dense Spend the Ti for 1.00~5.00mol/L4+Solution, it is stand-by；（2）Hybrid reaction：The graphene oxide solution containing low ph value for taking hummers methods to prepare, pure water is added, adjusts solution Mass concentration is 0.01~2%, and pH value is 2~5, stand-by after stirring；（3）Hybrid reaction：According to sodium silicate：Graphene oxide is 15~1：1 mass ratio weighs sodium silicate solution, by volume For 3:1~5:1, measure step（1）The mixed liquor of any one antibacterial ion solution or any two kinds of antibacterial ion solution, stirring After uniformly, mixed liquor is instilled into step（2）Sulfur acid graphene oxide solution in, further according to actual conditions instill sulfuric acid or Hydrochloric acid, the pH for adjusting mixed liquor is 4~7, continues to stir, and ultrasound 0.3~2 hour, obtains containing single antiseptic elements or contains it In two kinds of elements colloidal solution, it is stand-by；（4）Separation of solid and liquid and drying：By step（3）Obtained colloidal sol, after filtered, centrifuging process carries out separation of solid and liquid processing, Obtain the antibacterial white cabon black composite predecessor of paste body shape；（5）Post processing：By step（4）Novel antibacterial white carbon black composite material is finally made through calcination processing in obtained predecessor.
- 3. the preparation method of antibacterial white cabon black composite according to claim 2, it is characterised in that the step（3） Middle sodium silicate is the one or more in sodium metasilicate, potassium silicate, lithium metasilicate.
- 4. the preparation method of antibacterial white cabon black composite according to claim 2, it is characterised in that the step（4） Middle centrifugal separation process reaches separation of solid and liquid purpose using various centrifuge, filter press.
- 5. the preparation method of antibacterial white cabon black composite according to claim 2, it is characterised in that the step（4） Middle drying process is divided into：1）Freeze-drying condition is：Freeze temperature maintains -50~30 DEG C, the h of freeze-drying time 10~40, vacuum Spend 1~300Pa；2）Spray drying condition is：Inlet temperature is 100~350 DEG C, and outlet temperature is 40~150 DEG C, is used Dried medium be hot-air.
- 6. the preparation method of antibacterial white cabon black composite according to claim 2, it is characterised in that the step（5） Middle calcine technology is in argon hydrogen gaseous mixture（95：5）Under protective condition, 300~600 DEG C are warming up to, is incubated 2~6h, reaction terminates Afterwards, room temperature is dropped in gas shield.
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| CN201710912271.8A CN107668032A (en) | 2017-09-29 | 2017-09-29 | Antibacterial white cabon black composite and preparation method thereof |
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| CN201710912271.8A CN107668032A (en) | 2017-09-29 | 2017-09-29 | Antibacterial white cabon black composite and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325591A (en) * | 2017-07-20 | 2017-11-07 | 安徽盛华管业有限公司 | A kind of preparation method of the high temperature resistant copper type antibacterial white cabon black of fire-fighting CPVC water pipes |
| WO2022055459A3 (en) * | 2020-09-09 | 2022-09-01 | Gaziantep Universitesi Rektorlugu | Method of producing metal particles having metal oxide nanostructures for antimicrobial applications |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5236142A (en) * | 1975-09-18 | 1977-03-19 | Hitachi Cable Ltd | Sanitary rubber, plastic products |
| CN1535574A (en) * | 2003-04-04 | 2004-10-13 | 鞍山科技大学 | Antibacterial white cabon black and its preparation method |
| CN107057112A (en) * | 2017-05-31 | 2017-08-18 | 唐山建华科技发展有限责任公司 | The preparation method of graphene/white carbon black composite material |
-
2017
- 2017-09-29 CN CN201710912271.8A patent/CN107668032A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5236142A (en) * | 1975-09-18 | 1977-03-19 | Hitachi Cable Ltd | Sanitary rubber, plastic products |
| CN1535574A (en) * | 2003-04-04 | 2004-10-13 | 鞍山科技大学 | Antibacterial white cabon black and its preparation method |
| CN107057112A (en) * | 2017-05-31 | 2017-08-18 | 唐山建华科技发展有限责任公司 | The preparation method of graphene/white carbon black composite material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107325591A (en) * | 2017-07-20 | 2017-11-07 | 安徽盛华管业有限公司 | A kind of preparation method of the high temperature resistant copper type antibacterial white cabon black of fire-fighting CPVC water pipes |
| WO2022055459A3 (en) * | 2020-09-09 | 2022-09-01 | Gaziantep Universitesi Rektorlugu | Method of producing metal particles having metal oxide nanostructures for antimicrobial applications |
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Application publication date: 20180209 |
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