CN108503921A - A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material - Google Patents
A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material Download PDFInfo
- Publication number
- CN108503921A CN108503921A CN201810498244.5A CN201810498244A CN108503921A CN 108503921 A CN108503921 A CN 108503921A CN 201810498244 A CN201810498244 A CN 201810498244A CN 108503921 A CN108503921 A CN 108503921A
- Authority
- CN
- China
- Prior art keywords
- graphene
- thiocarbamide
- nano
- preparation
- functionalized nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2321/00—Characterised by the use of unspecified rubbers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Wood Science & Technology (AREA)
- Plant Pathology (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to chemical fields, are related to a kind of preparation method of Thiourea antibiotic property nano-graphene material, include the following steps, step 1：Organic acid obtains nano-graphene after reacting 1 10h at a temperature of 150 300 DEG C；Step 2：Thiocarbamide functionalized nano graphene is obtained by the reaction with Thiourea organic amino antiseptic under the action of catalyst in nano-graphene；Step 3：Thiocarbamide functionalized nano graphene polymerize with high molecular material to be prepared high-molecular anti-bacteria composite membrane or directly carries out antibacterial test.Nano-graphene produced by the present invention possesses the abundant functional group such as carboxyl, hydroxyl, amino, and strong antibacterial, safety is more preferable, easy to use.
Description
Technical field
The invention belongs to chemical fields, are related to a kind of preparation method of Thiourea antibiotic property nano-graphene material.
Background technology
Graphene has unusual excellent properties in mechanics, electricity, calorifics and magnetics, is widely used in electrochemistry
Sensor, nano material prepare and all various aspects such as bio-imaging.Currently, the preparation method of graphene mainly has micromechanics separation
Method, epitaxial growth method, chemical vapour deposition technique（CVD）, oxidation-reduction method and solvent-thermal method etc..The original substantially of micromechanics partition method
Reason is to overcome using mechanicals efforts the Van der Waals force of graphite layers to finally obtain one to make graphene be detached
The single-layer graphene of fraction.The method detaches known most thin material using mechanical force, it is desirable that charcoal material precursor has to
There is good cleavage fissure.Epitaxial growth method refers to utilizing Lattice Matching, and another crystal is grown on a crystal structure
Method, but the condition that this method requires is harsh.CVD method is to make it in Metal Substrate using carbon compounds such as methane as presoma
Body surface face occurs pyrolytic and generates pyrolytic carbon, and the method preparation process is simple, and gained graphene is of high quality, it can be achieved that large area
Growth, and be relatively easy to be transferred on various matrixes.It is so far most widely used one that graphite oxide reduction method, which prepares graphene,
The method that kind prepares graphene, the method is as a kind of low cost, the method that graphene batch production can be achieved.Solvent-thermal method has
Process is relatively easy, be easy to control, reaction temperature is low, does not need catalyst, the advantages that yield is high.In recent years, high quality and big
The synthetic method that batch nano-graphene manufactures and green is harmless becomes research hotspot.
With the fast development of society and the continuous improvement of industrial manufacturing level, from daily life to processing and manufacturing
Industry all fights Cordycepps and proposes increasingly higher demands.At the same time, caused to environment can not for the intensification of industrialization degree
The damage of reverse, and the growth and sprawling for harmful pico- biology such as encouraged bacterium, mould in most cases, make equipment
It is proposed acid test with protection." antibacterial " refer to inhibit within a certain period of time bacterium, the growth of microorganisms such as fungi,
Breeding and survival；Antibiotic method mainly has two class of physical method and chemical method.Antiseptic is divided into inorganic antiseptic and organic anti-
Microbial inoculum two major classes, wherein organic antibacterial agent are divided into as natural, low molecule and macromolecule organic antibacterial agent.However, in order to inhibit thin
Bacterium grows, and reduces harm of the bacterium to the mankind, and various novel anti-biotic materials continue to bring out out.Anti-biotic material refers to itself tool
There is killing or inhibits a kind of new function material of microbial function.Nano anti-biotic material is by more extensive concern.Although
Have some materials they itself possess the performance of antibacterial, but it is a certain amount of by being added still to have many anti-biotic materials all now
Antiseptic realize and improve their anti-microbial property.
Invention content
The present invention is intended to provide a kind of preparation method of Thiourea antibiotic property nano-graphene material, designs synthesizing thiourea
Class nano-graphene anti-biotic material, strong antibacterial, safety is more preferable, easy to use.
Technical solution according to the invention, the preparation method of the thiocarbamide functionalized nano Graphene antibiosis material, packet
Include following steps,
Step 1：Organic acid obtains nano-graphene after reacting 1-10h at a temperature of 150-300 DEG C；
Step 2：Thiocarbamide functionalized nano is obtained by the reaction with Thiourea organic amino antiseptic under the action of catalyst in nano-graphene
Graphene；
Step 3：Thiocarbamide functionalized nano graphene and the direct mixed polymerization of high molecular material prepare high-molecular anti-bacteria composite membrane or
Directly carry out antibacterial test.
Further, the organic acid in the step 1 is the carboxylic acid derivates containing carboxyl functional group.
Further, the organic acid in the step 1 is in tartaric acid, citric acid, oxalic acid, maleic acid and stearic acid
It is a kind of.
Further, the thiocarbamide functionalized nano graphene in the step 2 is the graphene of sheet.
Further, the Thiourea organic amino antiseptic in the step 2 is thiosemicarbazides, symmetric double contracting diamino sulphur
One kind in the thiosemicarbazones of urea, asymmetric double random phase encryption and metal complex.
Further, the molar ratio of nano-graphene and Thiourea organic amino antiseptic is 1 in the step 2:0.01-
1:1。
Further, the type of the high molecular material in the step 3 is rubber, plastics, fiber, hot melt adhesive and coating
In one kind.
Further, the molar ratio that nano-graphene is mixed with high molecular material in the step 3 is 0.001:1-1:1.
Further, the catalyst in the step 2 is mass ratio 1.6-2.3：1 1- ethyls -3- (3- dimethylaminos
Propyl)-carbodiimides and n-hydroxysuccinimide
The beneficial effects of the present invention are：
Strong antibacterial, compared with conventional graphite alkene, functionalized nano graphene contains abundant functional group, table because piece is small
Reveal and significantly improves antibacterial ability；
Safety is more preferable, and with inorganic nano-particle and organic anti-bacterial small molecular phase ratio, migration will not occur for nano-graphene to people
Body damages；
It is easy to use, it can avoid tradition directly with the compound carry out antibacterial of polymer composite and be modified when in use, and give
Its use is made troubles.
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
Embodiment one：
A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material, includes the following steps,
Step 1：Tartaric acid obtains nano-graphene after reacting 7h at a temperature of 150 DEG C；
Step 2：Nano-graphene is in mass ratio 2:1 1- ethyls -3- (3- dimethyl aminopropyls)-carbodiimides (EDC) and
With thiosemicarbazides with molar ratio 1 under the action of n-hydroxysuccinimide (NHS):0.01 is obtained by the reaction the thiocarbamide functionalization of sheet
Nano-graphene；
Step 3：Thiocarbamide functionalized nano graphene is with rubber with molar ratio 0.001:1 polymerization prepares high-molecular anti-bacteria composite membrane.
Embodiment two：
A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material, includes the following steps,
Step 1：Citric acid obtains nano-graphene after reacting 10h at a temperature of 200 DEG C；
Step 2：Nano-graphene is in mass ratio 1.6:With symmetrical double random phase encryption to rub under the action of 1 EDC and NHS
That ratio 1:0.08 is obtained by the reaction the thiocarbamide functionalized nano graphene of sheet；
Step 3：Thiocarbamide functionalized nano graphene is with plastics with molar ratio 0.012:1 polymerization prepares high-molecular anti-bacteria composite membrane.
Embodiment three：
A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material, includes the following steps,
Step 1：Oxalic acid obtains nano-graphene after reacting 4h at a temperature of 250 DEG C；
Step 2：Nano-graphene is in mass ratio 1.8:Under the action of 1 EDC and NHS with asymmetric double random phase encryption with
Molar ratio 1:0.24 is obtained by the reaction the thiocarbamide functionalized nano graphene of sheet；
Step 3：Thiocarbamide functionalized nano graphene is with fiber with molar ratio 0.15:1 polymerization prepares high-molecular anti-bacteria composite membrane.
Example IV：
A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material, includes the following steps,
Step 1：Maleic acid obtains nano-graphene after reacting 1h at a temperature of 300 DEG C；
Step 2：Nano-graphene is in mass ratio 2.1:Thiosemicarbazones under the action of 1 EDC and NHS with metal complex
With molar ratio 1:0.64 is obtained by the reaction the thiocarbamide functionalized nano graphene of sheet；
Step 3：Thiocarbamide functionalized nano graphene is with hot melt adhesive with molar ratio 0.52:It is compound that 1 polymerization prepares high-molecular anti-bacteria
Film.
Embodiment five：
A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material, includes the following steps,
Step 1：Stearic acid obtains nano-graphene after reacting 2h at a temperature of 280 DEG C；
Step 2：Nano-graphene is in mass ratio 2.3:Thiosemicarbazones under the action of 1 EDC and NHS with metal complex
With molar ratio 1:1 is obtained by the reaction the thiocarbamide functionalized nano graphene of sheet；
Step 3：Thiocarbamide functionalized nano graphene is with coating with molar ratio 1:1 polymerization directly carries out antibacterial test.
Its nano-graphene obtained of the method for the present invention design synthesizing thiourea class nano-graphene quantum possesses carboxyl, hydroxyl
The abundant functional group such as base, amino is reacted with amino-containing Thiourea antiseptic by amide using nano-ink Xi Shang functional groups
In conjunction with to which the high molecule nano material containing anti-microbial property be made, strong antibacterial, safety is more preferable, easy to use.
Claims (9)
1. a kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material, which is characterized in that include the following steps,
Step 1：Organic acid obtains nano-graphene after reacting 1-10h at a temperature of 150-300 DEG C；
Step 2：Thiocarbamide functionalized nano is obtained by the reaction with Thiourea organic amino antiseptic under the action of catalyst in nano-graphene
Graphene；
Step 3：Thiocarbamide functionalized nano graphene polymerize with high molecular material to be prepared high-molecular anti-bacteria composite membrane or directly carries out
Antibacterial test.
2. the preparation method of thiocarbamide functionalized nano Graphene antibiosis material as described in claim 1, which is characterized in that institute
It is the carboxylic acid derivates containing carboxyl functional group to state the organic acid in step 1.
3. the preparation method of thiocarbamide functionalized nano Graphene antibiosis material as described in claim 1, which is characterized in that institute
It is one kind in tartaric acid, citric acid, oxalic acid, maleic acid and stearic acid to state the organic acid in step 1.
4. the preparation method of thiocarbamide functionalized nano Graphene antibiosis material as described in claim 1, which is characterized in that institute
State the graphene that the thiocarbamide functionalized nano graphene in step 2 is sheet.
5. the preparation method of thiocarbamide functionalized nano Graphene antibiosis material as described in claim 1, which is characterized in that institute
It is thiosemicarbazides, symmetrical double random phase encryption, asymmetric double contracting diamino to state the Thiourea organic amino antiseptic in step 2
One kind in the thiosemicarbazones of thiocarbamide and metal complex.
6. the preparation method of thiocarbamide functionalized nano Graphene antibiosis material as described in claim 1, which is characterized in that institute
It is 1 to state the molar ratio of nano-graphene and Thiourea organic amino antiseptic in step 2:0.01-1:1.
7. the preparation method of thiocarbamide functionalized nano Graphene antibiosis material as described in claim 1, which is characterized in that institute
The type for stating the high molecular material in step 3 is one kind in rubber, plastics, fiber, hot melt adhesive and coating.
8. the preparation method of thiocarbamide functionalized nano Graphene antibiosis material as claimed in claim 1 or 7, feature exist
In the molar ratio that nano-graphene is mixed with high molecular material in the step 3 is 0.001:1-1:1.
9. the preparation method of thiocarbamide functionalized nano Graphene antibiosis material as described in claim 1, which is characterized in that institute
It is mass ratio 1.6-2.3 to state the catalyst in step 2：1 1- ethyls -3- (3- dimethyl aminopropyls)-carbodiimides and N-
HOSu NHS.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810498244.5A CN108503921A (en) | 2018-05-23 | 2018-05-23 | A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810498244.5A CN108503921A (en) | 2018-05-23 | 2018-05-23 | A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108503921A true CN108503921A (en) | 2018-09-07 |
Family
ID=63401313
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810498244.5A Pending CN108503921A (en) | 2018-05-23 | 2018-05-23 | A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108503921A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2669409A1 (en) * | 2012-05-29 | 2013-12-04 | King Saud University | Method for preparing highly crystalline Pb chalcogenide nanoparticles, nanoparticles prepared thereby and use thereof |
| CN104862676A (en) * | 2015-03-25 | 2015-08-26 | 上海应用技术学院 | Graphene oxide nickel-phosphorus composite plating solution, preparation method and applications thereof |
| CN106362771A (en) * | 2016-08-11 | 2017-02-01 | 广西南宁胜祺安科技开发有限公司 | Novel cadmium sulfide photocatalyst with high activity |
| CN106883849A (en) * | 2017-03-29 | 2017-06-23 | 温州医科大学 | Graphene quantum dot that a kind of nitrogenous sulphur mixes and preparation method thereof and the application on lysine luciferase assay reagent is prepared |
| CN106938842A (en) * | 2016-01-04 | 2017-07-11 | 天津工业大学 | It is a kind of to be pyrolyzed the method that citric acid prepares graphene quantum dot |
| CN107227151A (en) * | 2016-03-24 | 2017-10-03 | 天津工业大学 | A kind of method for preparing nitrogen-doped graphene quantum dot |
| CN107312188A (en) * | 2017-08-02 | 2017-11-03 | 四川大学 | A kind of porous silicone rubber film of graphene-containing and its production and use |
-
2018
- 2018-05-23 CN CN201810498244.5A patent/CN108503921A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2669409A1 (en) * | 2012-05-29 | 2013-12-04 | King Saud University | Method for preparing highly crystalline Pb chalcogenide nanoparticles, nanoparticles prepared thereby and use thereof |
| CN104862676A (en) * | 2015-03-25 | 2015-08-26 | 上海应用技术学院 | Graphene oxide nickel-phosphorus composite plating solution, preparation method and applications thereof |
| CN106938842A (en) * | 2016-01-04 | 2017-07-11 | 天津工业大学 | It is a kind of to be pyrolyzed the method that citric acid prepares graphene quantum dot |
| CN107227151A (en) * | 2016-03-24 | 2017-10-03 | 天津工业大学 | A kind of method for preparing nitrogen-doped graphene quantum dot |
| CN106362771A (en) * | 2016-08-11 | 2017-02-01 | 广西南宁胜祺安科技开发有限公司 | Novel cadmium sulfide photocatalyst with high activity |
| CN106883849A (en) * | 2017-03-29 | 2017-06-23 | 温州医科大学 | Graphene quantum dot that a kind of nitrogenous sulphur mixes and preparation method thereof and the application on lysine luciferase assay reagent is prepared |
| CN107312188A (en) * | 2017-08-02 | 2017-11-03 | 四川大学 | A kind of porous silicone rubber film of graphene-containing and its production and use |
Non-Patent Citations (3)
| Title |
|---|
| QIANFEN ZHUANG, ET AL.: "Solid-phase synthesis of graphene quantum dots from the food additive citric acid under microwave irradiation and their use in live-cell imaging", 《LUMINESCENCE》 * |
| 李碧桐: "柠檬酸热解法制备石墨烯量子点及其光学性能研究", 《云南大学硕士研究生学会论文》 * |
| 马庆运: "热解柠檬酸制备石墨烯量子点及其光学性质研究", 《化工新型材料》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Sun et al. | Nanocomposite hydrogel-based strain and pressure sensors: a review | |
| CN101654243B (en) | Preparation method of functional nano-graphene | |
| Han et al. | Graphene oxide grafted carbon fiber reinforced siliconborocarbonitride ceramics with enhanced thermal stability | |
| CN105776181B (en) | A kind of preparation method of flake nano porous carbon and carbon nano tube compound material | |
| Yu et al. | One-pot green fabrication and antibacterial activity of thermally stable corn-like CNC/Ag nanocomposites | |
| CN102431997B (en) | Graphene oxide with antibacterial and anticoagulant functions and preparation method thereof | |
| Cheng et al. | Hydrothermal growing of cluster-like ZnO nanoparticles without crystal seeding on PET films via dopamine anchor | |
| Li et al. | Fabrication of regenerated cellulose membranes with high tensile strength and antibacterial property via surface amination | |
| Liu et al. | A conductive polyacrylamide hydrogel enabled by dispersion-enhanced MXene@ chitosan assembly for highly stretchable and sensitive wearable skin | |
| CN104277415A (en) | Long-acting antibacterial amino molding compound | |
| CN111607839A (en) | Method for preparing modified white graphene polyester composite fiber and fiber prepared by method | |
| CN109608607B (en) | High-performance polyurethane elastomer material and preparation method thereof | |
| CN106336574A (en) | BOPP film | |
| Hao et al. | Metal ion-coordinated carboxymethylated chitosan grafted carbon nanotubes with enhanced antibacterial properties | |
| Yang et al. | Performance comparison of immobilized enzyme on the titanate nanotube surfaces modified by poly (dopamine) and poly (norepinephrine) | |
| Ramesh et al. | Cellulose–polyvinyl alcohol–nano-TiO2 hybrid nanocomposite: thermal, optical, and antimicrobial properties against pathogenic bacteria | |
| CN108503921A (en) | A kind of preparation method of thiocarbamide functionalized nano Graphene antibiosis material | |
| CN112175239B (en) | Long-acting and controllable composite anti-aging agent and preparation method and application thereof | |
| CN110746654A (en) | Halloysite-containing flame-retardant antibacterial compound and preparation method thereof | |
| CN114644771A (en) | Polyvinyl chloride medicine package sheet with anti-fouling and antibacterial functions and preparation method thereof | |
| CN108719317A (en) | A kind of preparation method of positive charge nano-graphene anti-biotic material | |
| CN101239725A (en) | Nano-stage calcium borate and use thereof | |
| CN110862681A (en) | Ternary composite gas-sensitive material and preparation method thereof | |
| CN111137877B (en) | Benzoxazine-based carbon nanomaterial and preparation method and application thereof | |
| Yang et al. | Enhanced antibacterial effect of polypyrazole-graphene oxide composite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180907 |