CN108719320A - A kind of graphene oxide sterilization material of Bengal rose red functionalization and preparation method thereof - Google Patents

A kind of graphene oxide sterilization material of Bengal rose red functionalization and preparation method thereof Download PDF

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Publication number
CN108719320A
CN108719320A CN201810742837.1A CN201810742837A CN108719320A CN 108719320 A CN108719320 A CN 108719320A CN 201810742837 A CN201810742837 A CN 201810742837A CN 108719320 A CN108719320 A CN 108719320A
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China
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graphene oxide
rose red
bengal rose
pdda
sterilization material
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CN201810742837.1A
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Chinese (zh)
Inventor
毛昌杰
迟芬萍
陈鹏鹏
陈京帅
吴明元
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Anhui University
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Anhui University
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N59/00Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds

Abstract

The invention discloses a kind of graphene oxide sterilization materials of Bengal rose red functionalization and preparation method thereof, wherein the sterilization material is made of following component:Graphene oxide, diallyl dimethyl ammoniumchloride and Bengal rose red.Synthesis technology of the present invention is simple, low processing cost is easily grasped, safety and environmental protection, it is low to human toxicity, on the one hand bactericidal liquid processing preparation work efficiency can be effectively improved, raising bactericidal liquid is killed to microbial activities such as bacterium, viruses and inhibiting effect, another aspect material can generate a large amount of active oxygens (ROS) under light, active oxygen is a kind of strong oxidizer, microbial action, including bacterium, brood cell, virus, fungi etc., 600-3000 times fast compared with chlorine of killing rate are killed with extensive.

Description

A kind of graphene oxide sterilization material of Bengal rose red functionalization and its preparation Method
Technical field
The present invention relates to a kind of graphene oxide sterilization materials of Bengal rose red functionalization and preparation method thereof, belong to life Object chemical technology field.
Background technology
Microbial contamination is a serious environmental problem.Such as bacterium can give rise to diseases, threaten human health with Socio-economic development.One of the most common bacterium is Escherichia coli, behind e. coli contamination water source, can enter people by drinking water Body gastrointestinal tract makes one to catch.If soil can be deteriorated by e. coli contamination, not only soil quality, underground water and farming Object can be also contaminated, and the health of resident can also be seriously threatened.Therefore in order to improve people to everyday tools, food and people The needs of protection and the health care of body itself, people are increasing to all kinds of sterilization material demands, especially efficient sterilizing material. It for above-mentioned present situation, needs to develop a kind of completely new efficient sterilizing liquid, to meet the needs of actual use.On the other hand, in recent years To find active oxygen for biology and the treatment for medically having great role, especially tumour, it has been found that these activity Oxygen equally can generate destruction to the institutional framework of bacterium, and bactericidal effect is apparent.Therefore a kind of a large amount of active oxygens of energy generation are developed Sterilization material peomotes the development of modern medicine.
Invention content
The present invention is intended to provide a kind of graphene oxide sterilization material of Bengal rose red functionalization and preparation method thereof. On the one hand the graphene oxide sterilization material of Bengal rose red functionalization of the present invention can effectively improve bactericidal liquid working efficiency, Raising bactericidal liquid is killed to microbial activities such as bacterium, viruses and inhibiting effect;Another aspect material can generate under photocatalysis A large amount of active oxygens (ROS), have and kill microbial action extensively.
The graphene oxide sterilization material of Bengal rose red functionalization of the present invention, is made of following component:
Graphene oxide, diallyl dimethyl ammoniumchloride (PDDA) and Bengal rose red.
Diallyl dimethyl ammoniumchloride is the coupling agent that Bengal rose red is combined on graphene oxide.
Graphene oxide and the mass ratio of diallyl dimethyl ammoniumchloride are 2:1.
Graphene oxide and the mass ratio of Bengal rose red are 1:1-4, wherein for 1:When 3, generation active oxygen is most, kills The oxidability of bacterium material is most strong.
The pattern of the graphene oxide is film-form;The graphene oxide sterilization material is sheet.
The preparation method of the graphene oxide sterilization material of Bengal rose red functionalization of the present invention, includes the following steps:
Step 1:Prepare graphene oxide
Graphene oxide is prepared using Hummers methods, is freeze-dried;
Step 2:Prepare GO/PDDA compounds
The PDDA solution of mass concentration 0.25% is added in 1mg/mL graphene oxide solutions, graphene oxide and poly- two The mass ratio of allyl dimethyl ammonium chloride is 2:8-12h is stood after 1, ultrasonic disperse 1h, viscous brown shape object is obtained after centrifugation Matter, as GO/PDDA compounds obtain GO/PDDA dispersion liquids after redistilled water ultrasonic disperse is added;
Step 3:Prepare GO/PDDA/RB composite materials
Bengal rose red is added in GO/PDDA dispersion liquids, 6h is stirred after ultrasonic disperse 2h, centrifugation to supernatant is clarified It is transparent, GO/PDDA/RB composite materials are can be obtained after freeze-drying.
In step 3, centrifugal speed 10000r/min.
On the one hand sterilization material of the present invention can effectively improve bactericidal liquid working efficiency, improve bactericidal liquid to bacterium, virus Etc. microbial activities kill and inhibiting effect;Another aspect material can generate a large amount of active oxygens under photocatalysis, and active oxygen is one Kind strong oxidizer, has and kills microbial action, including bacterium, brood cell, virus, fungi etc. extensively, killing rate is fast compared with chlorine 600-3000 times, and active oxygen cannot be only used for the treatment etc. that sterilization can be additionally used in biology and medicine aspect such as tumour Deng.
Material of the present invention has potential application value in bioanalysis and in terms of improving environmental pollution, can effectively meet and wash The demand needed even medically that the multiple products such as clean essence, hand cleanser are used in mixed way.
Synthesis technology of the present invention is simple, low processing cost, easily grasps, and safety and environmental protection is low to human toxicity.
Description of the drawings
Fig. 1 is preparation technology flow chart of the present invention.
Fig. 2 is GO/PDDA/RB composite materials stereoscan photograph of the present invention.
Fig. 3 is antibacterial experiment photo of the present invention.
Specific implementation mode
Technical solution of the present invention is further analyzed and described with reference to specific embodiment and attached drawing.
Embodiment 1:
The graphene oxide sterilization material of Bengal rose red functionalization is made of following component in the present embodiment:
Graphene oxide, diallyl dimethyl ammoniumchloride and Bengal rose red.
Wherein, graphene oxide and the mass ratio of diallyl dimethyl ammoniumchloride are 2:1, graphene oxide and Meng Jia It is 1 to draw the mass ratio of rose-red:1.
The pattern of the graphene oxide is film-form;The graphene oxide sterilization material is sheet.
The preparation method of the graphene oxide sterilization material of Bengal rose red functionalization is as follows in the present embodiment:
1, graphene oxide is prepared
Graphene oxide is prepared using Hummers methods, is freeze-dried.(Hummers methods prepare graphene oxide with reference to text It offers:Hummers W S,Offeman R E.Preparation of Graphitic Oxide.J Am Chem Soc 80: 1339[J].Journal of the American Chemical Society,1958,80(6).)
2, GO/PDDA compounds are prepared
The PDDA solution of 200mL mass concentrations 0.25% is added in the graphene oxide solution of 100mL 1mg/mL, oxygen Graphite alkene and the mass ratio of diallyl dimethyl ammoniumchloride are 2:12h is stood after 1, ultrasonic disperse 1h, by stratification Solution centrifugation afterwards three times, obtains viscous brown shape substance, as GO/PDDA compounds, redistilled water ultrasonic disperse is added 30min obtains GO/PDDA dispersion liquids;
3, GO/PDDA/RB composite materials are prepared
0.1g Bengal rose reds are added in GO/PDDA dispersion liquids, stir 6h after ultrasonic disperse 2h, 10000r/min from Heart 10min, supernatant clear can be obtained GO/PDDA/RB composite materials after freeze-drying.
Embodiment 2:
The graphene oxide sterilization material of Bengal rose red functionalization is made of following component in the present embodiment:
Graphene oxide, diallyl dimethyl ammoniumchloride and Bengal rose red.
Wherein, graphene oxide and the mass ratio of diallyl dimethyl ammoniumchloride are 2:1, graphene oxide and Meng Jia It is 1 to draw the mass ratio of rose-red:2.
The pattern of the graphene oxide is film-form;The graphene oxide sterilization material is sheet.
The preparation method of the graphene oxide sterilization material of Bengal rose red functionalization is as follows in the present embodiment:
1, graphene oxide is prepared
Graphene oxide is prepared using Hummers methods, is freeze-dried.(Hummers methods prepare graphene oxide with reference to text It offers:Hummers W S,Offeman R E.Preparation of Graphitic Oxide.J Am Chem Soc 80: 1339[J].Journal of the American Chemical Society,1958,80(6).)
2, GO/PDDA compounds are prepared
The PDDA solution of 200mL mass concentrations 0.25% is added in the graphene oxide solution of 100mL 1mg/mL, oxygen Graphite alkene and the mass ratio of diallyl dimethyl ammoniumchloride are 2:12h is stood after 1, ultrasonic disperse 1h, by stratification Solution centrifugation afterwards three times, obtains viscous brown shape substance, as GO/PDDA compounds, redistilled water ultrasonic disperse is added 30min obtains GO/PDDA dispersion liquids;
3, GO/PDDA/RB composite materials are prepared
0.2g Bengal rose reds are added in GO/PDDA dispersion liquids, stir 6h after ultrasonic disperse 2h, 10000r/min from Heart 10min, supernatant clear can be obtained GO/PDDA/RB composite materials after freeze-drying.
Embodiment 3:
The graphene oxide sterilization material of Bengal rose red functionalization is made of following component in the present embodiment:
Graphene oxide, diallyl dimethyl ammoniumchloride and Bengal rose red.
Wherein, graphene oxide and the mass ratio of diallyl dimethyl ammoniumchloride are 2:1, graphene oxide and Meng Jia It is 1 to draw the mass ratio of rose-red:3.
The pattern of the graphene oxide is film-form;The graphene oxide sterilization material is sheet.
The preparation method of the graphene oxide sterilization material of Bengal rose red functionalization is as follows in the present embodiment:
1, graphene oxide is prepared
Graphene oxide is prepared using Hummers methods, is freeze-dried.(Hummers methods prepare graphene oxide with reference to text It offers:Hummers W S,Offeman R E.Preparation of Graphitic Oxide.J Am Chem Soc 80: 1339[J].Journal of the American Chemical Society,1958,80(6).)
2, GO/PDDA compounds are prepared
The PDDA solution of 200mL mass concentrations 0.25% is added in the graphene oxide solution of 100mL 1mg/mL, oxygen Graphite alkene and the mass ratio of diallyl dimethyl ammoniumchloride are 2:12h is stood after 1, ultrasonic disperse 1h, by stratification Solution centrifugation afterwards three times, obtains viscous brown shape substance, as GO/PDDA compounds, redistilled water ultrasonic disperse is added 30min obtains GO/PDDA dispersion liquids;
3, GO/PDDA/RB composite materials are prepared
0.3g Bengal rose reds are added in GO/PDDA dispersion liquids, stir 6h after ultrasonic disperse 2h, 10000r/min from Heart 10min, supernatant clear can be obtained GO/PDDA/RB composite materials after freeze-drying.
Embodiment 4:
The graphene oxide sterilization material of Bengal rose red functionalization is made of following component in the present embodiment:
Graphene oxide, diallyl dimethyl ammoniumchloride and Bengal rose red.
Wherein, graphene oxide and the mass ratio of diallyl dimethyl ammoniumchloride are 2:1, graphene oxide and Meng Jia It is 1 to draw the mass ratio of rose-red:4.
The pattern of the graphene oxide is film-form;The graphene oxide sterilization material is sheet.
The preparation method of the graphene oxide sterilization material of Bengal rose red functionalization is as follows in the present embodiment:
1, graphene oxide is prepared
Graphene oxide is prepared using Hummers methods, is freeze-dried.(Hummers methods prepare graphene oxide with reference to text It offers:Hummers W S,Offeman R E.Preparation of Graphitic Oxide.J Am Chem Soc 80: 1339[J].Journal of the American Chemical Society,1958,80(6).)
2, GO/PDDA compounds are prepared
The PDDA solution of 200mL mass concentrations 0.25% is added in the graphene oxide solution of 100mL 1mg/mL, oxygen Graphite alkene and the mass ratio of diallyl dimethyl ammoniumchloride are 2:12h is stood after 1, ultrasonic disperse 1h, by stratification Solution centrifugation afterwards three times, obtains viscous brown shape substance, as GO/PDDA compounds, redistilled water ultrasonic disperse is added 30min obtains GO/PDDA dispersion liquids;
3, GO/PDDA/RB composite materials are prepared
0.4g Bengal rose reds are added in GO/PDDA dispersion liquids, stir 6h after ultrasonic disperse 2h, 10000r/min from Heart 10min, supernatant clear can be obtained GO/PDDA/RB composite materials after freeze-drying.
Embodiment 5:Antibacterial experiment
Antibacterial experiment selects Escherichia coli for model microorganism.Each sample disperses two after sterilization under ultrasonication In secondary distilled water, each sample solution (1ml) mixes with bacterial suspension (100 μ L), wherein the blank control for not being loaded product uses Physiological saline (1mL) is respectively added in LB liquid medium (25 mL), and at 37 DEG C, rotating speed is the water bath with thermostatic control of 220r/min It is cultivated in oscillator.After the contact of certain time, reaction suspension is diluted successively, then takes 100 μ L of each culture solution It is applied on LB agar plates, tablet is placed in 37 DEG C of bio-incubator and cultivates 24 h, record the bacterium on each material plates Number is fallen, experiment is at least in triplicate.Concrete outcome is see Fig. 3 and following table.
Blank control RB GO GO/PDDA/RB
Viable count 34 13 7 0
Viable bacteria rate 1 0.3824 0.2059 0
Synthesis technology of the present invention is simple, low processing cost, easily grasps, safety and environmental protection is low to human toxicity, on the one hand may be used The effective bactericidal liquid that improves processes preparation work efficiency, improves bactericidal liquid and the microbial activities such as bacterium, virus are killed and inhibited Effect, another aspect material can generate a large amount of active oxygens (ROS) under light, and active oxygen is a kind of strong oxidizer, have and kill extensively Microorganism killing acts on, including bacterium, brood cell, virus, fungi etc., 600-3000 times fast compared with chlorine of killing rate.And active oxygen It cannot be only used for the treatment etc. that sterilization can be additionally used in biology and medicine aspect such as tumour.The material in bioanalysis and There is potential application value in terms of improving environmental pollution, can effectively meet what the multiple products such as liquid detergent, hand cleanser were used in mixed way Need demand even medically.

Claims (7)

1. a kind of graphene oxide sterilization material of Bengal rose red functionalization, it is characterised in that the sterilization material is by following Component is constituted:
Graphene oxide, diallyl dimethyl ammoniumchloride and Bengal rose red.
2. the graphene oxide sterilization material of Bengal rose red functionalization according to claim 1, it is characterised in that:
Graphene oxide and the mass ratio of diallyl dimethyl ammoniumchloride are 2:1.
3. the graphene oxide sterilization material of Bengal rose red functionalization according to claim 1, it is characterised in that:
Graphene oxide and the mass ratio of Bengal rose red are 1:1-4.
4. the graphene oxide sterilization material of Bengal rose red functionalization according to claim 3, it is characterised in that:
Graphene oxide and the mass ratio of Bengal rose red are 1:3.
5. the graphene oxide sterilization material of Bengal rose red functionalization according to claim 1, it is characterised in that:
The pattern of the graphene oxide is film-form;The graphene oxide sterilization material is sheet.
6. the preparation side of the graphene oxide sterilization material of any Bengal rose red functionalization in a kind of claim 1-5 Method, it is characterised in that include the following steps:
Step 1:Prepare graphene oxide
Graphene oxide is prepared using Hummers methods, is freeze-dried;
Step 2:Prepare GO/PDDA compounds
The PDDA solution of mass concentration 0.25% is added in 1mg/mL graphene oxide solutions, 8- is stood after ultrasonic disperse 1h 12h obtains viscous brown shape substance, as GO/PDDA compounds after centrifugation, obtained after redistilled water ultrasonic disperse is added GO/PDDA dispersion liquids;
Step 3:Prepare GO/PDDA/RB composite materials
Bengal rose red is added in GO/PDDA dispersion liquids, 6h is stirred after ultrasonic disperse 2h, centrifugation is saturating to supernatant clarification It is bright, GO/PDDA/RB composite materials are can be obtained after freeze-drying.
7. preparation method according to claim 6, it is characterised in that:
In step 3, centrifugal speed 10000r/min.
CN201810742837.1A 2018-07-09 2018-07-09 A kind of graphene oxide sterilization material of Bengal rose red functionalization and preparation method thereof Pending CN108719320A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112191025A (en) * 2020-09-29 2021-01-08 南通大学 Individual protection filter material capable of being sterilized under driving of sunlight and preparation method

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WO2016106173A1 (en) * 2014-12-22 2016-06-30 Titlebaum Richard System and method for introducing photosensitive dyes via an insert into a root canal in a tooth, method for producing said dye impregnated insert and method of using said dye-impregnated insert
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CN103613773A (en) * 2013-11-07 2014-03-05 常州大学 Preparation method of flexible transparent conducting polymer thin film with antibacterial properties
WO2016106173A1 (en) * 2014-12-22 2016-06-30 Titlebaum Richard System and method for introducing photosensitive dyes via an insert into a root canal in a tooth, method for producing said dye impregnated insert and method of using said dye-impregnated insert
CN106744890A (en) * 2015-11-18 2017-05-31 青岛智信生物科技有限公司 The preparation method of diallyl dimethyl ammoniumchloride functionalization graphene

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Publication number Priority date Publication date Assignee Title
CN112191025A (en) * 2020-09-29 2021-01-08 南通大学 Individual protection filter material capable of being sterilized under driving of sunlight and preparation method

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Application publication date: 20181102