CN108997750A - A kind of preparation method of graphene oxide self-healing polymers - Google Patents
A kind of preparation method of graphene oxide self-healing polymers Download PDFInfo
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- CN108997750A CN108997750A CN201811142249.0A CN201811142249A CN108997750A CN 108997750 A CN108997750 A CN 108997750A CN 201811142249 A CN201811142249 A CN 201811142249A CN 108997750 A CN108997750 A CN 108997750A
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/34—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids using polymerised unsaturated fatty acids
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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/21—Urea; Derivatives thereof, e.g. biuret
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- 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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
- C08J2377/08—Polyamides derived from polyamines and polycarboxylic acids from polyamines and polymerised unsaturated fatty acids
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Abstract
A kind of preparation method of graphene oxide self-healing polymers, belongs to self-healing polymers technical field of material.The present invention prepares graphene oxide using graphene using improved Hummers method first, passes through examination of infrared spectrum, it was demonstrated that graphene surface active group dramatically increases.Then, cross-linked polymeric is carried out by using dimeric dibasic acid and diethylenetriamine, prepare dendritic oligomer, finally, respectively by graphene oxide obtained and dendritic oligomer obtained, urea is mixed, cross-linking polymerization 4h at a temperature of 135~160 DEG C, graphene oxide self-healing polymers are prepared, the beneficial effect of the present invention compared with the existing technology is: original self-healing polymers poor mechanical property of urea and the production of dendritic oligomer cross-linked polymeric, it is difficult to practical application, the present invention improves the mechanical property of material using the laminated structure enhancing characteristic of graphene oxide, enhance the practicability of material.
Description
Technical field
The invention belongs to self-healing polymers technical field of material, and in particular to a kind of graphene oxide selfreparing is poly-
Close the preparation method of object.
Background technique
In recent years, with the development and application of polymer material, the damage problem of material becomes the one of Material Field development
Hang-up.And the selfreparing of material can solve the problem just, self-healing polymers material refers to there is self-regeneration
New material, Inspiration Sources are damaged rear self-regeneration in organism, in the material, self-repair function major embodiment material
The various forms of damages of appearance itself can be diagnosed and repaired in time.The safety system of material can be improved in self-healing polymers material
Number, the service life for extending material, reduce maintenance cost etc., thus be used in aerospace, military project, construction material etc. it is many
Field has huge market potential and application prospect.Self-repair technology can be mainly divided into Intrinsical and foreign aid's type two major classes.
Foreign aid's type self-repair technology needs to fill the extraneous reparation substance such as renovation agent.Intrinsical self-repair technology is not required to add extraneous reparation
Agent.Currently, Intrinsical self-repair technology application is further extensive, Intrinsical self-repair technology principle includes two kinds: reversible covalent bonds
Selfreparing and reversible non-covalent key selfreparing.Reversible covalent bonds selfreparing be some special chemical keys are introduced in system, such as
Acylhydrazone key, cystine linkage, N-O key, Dieal-Alder reversible reaction etc. are realized.Reversible non-covalent key self-repair function includes system
In hydrogen bond interaction, mercapto water effect, electrostatic interaction, ionic interaction, molecule diffusion etc. realize.In recent years
, based on the self-healing polymers of hydrogen bond because of advantages such as its material matrix range of choice is big, repairing performance stabilizations, from 2008
It is rapidly developed after Leibler report, but the mechanical property of original self-healing polymers matrix is poor, application range is limited.
Graphene oxide is single atomic layer, can expand to some tens of pm on lateral dimension at any time.Therefore, it ties
Structure spans the typical size of general chemistry and material science.Graphene oxide can be considered a kind of soft material of non-traditional kenel
Material, the characteristic with polymer, colloid, film and amphiphatic molecule can be used as obturator addition in self-healing polymers matrix
In, improve self-healing polymers matrix mechanical property, keeps self-healing polymers material application range more extensive.
Summary of the invention
It is poor based on hydrogen bond self-healing polymers mechanical property that the purpose of the present invention is to solve existing, and then causes
It is difficult to the problem of practical application, provides a kind of preparation method of graphene oxide self-healing polymers.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of graphene oxide self-healing polymers, specific step is as follows for the method:
Step 1: the preparation of graphene oxide: 1.00g~1.50g graphite, 10mL phosphoric acid and 90mL sulfuric acid is taken to be added to
In 500mL there-necked flask, 6g potassium permanganate was divided into 12 times in 1 minute and is uniformly added into there-necked flask, in 4 DEG C of stirred in water bath
1h；50 DEG C are warming up to, insulated and stirred is for 24 hours；Products therefrom is poured into 0 DEG C of ice water of 250mL, 30% peroxide is added dropwise while stirring
Changing hydrogen solution to solution colour becomes golden yellow；
The use of the pH value that product is centrifuged to supernatant by the dilute hydrochloric acid solution of volume fraction 5% and distilled water is successively 7, uses
Water washing precipitating is distilled, then pours into the thick precipitating washed in 100mL beaker, the ultrasound when ultrasonic power is 150W
120 minutes, then sufficiently dry 48h is placed in 70 DEG C of vacuum ovens to get graphene oxide is arrived；
Step 2: the preparation of dendritic oligomer: 30~40g dimeric dibasic acid and 12.3g~16.4g diethylenetriamine are placed on
In 100mL there-necked flask, using magnetic agitation, reaction is condensed back for 24 hours at 160 DEG C, is continually fed into nitrogen during the reaction
Protection, generates dendritic oligomer；
Step 3: the preparation of graphene oxide self-healing polymers: the dendritic oligomer 35g for taking step 2 to prepare, respectively
At 7 parts, then to graphene oxide, 7 parts of dendritic oligomer and 7 parts of graphene oxides made from a step 1 of addition in every part
It corresponds and is added, 7 parts of graphene oxides are 0.05,0.15g, 0.25g, 0.35g, 0.45g, 0.55g, 0.65g respectively；And handle
Every part is all uniformly mixed, then to being separately added into urea 1.18g in every part, cross-linking polymerization 4h at a temperature of 135~160 DEG C,
The graphene oxide self-healing polymers that content is followed successively by 1%, 3%, 5%, 7%, 9%, 11%, 13% are prepared.
The beneficial effect of the present invention compared with the existing technology is: the selfreparing that urea and dendritic oligomer cross-linked polymeric obtain
Mechanical properties of polymer is poor, it is difficult to which practical application, the present invention are improved certainly using the laminated structure enhancing characteristic of graphene oxide
The mechanical property of rehabilitation polymer material enhances the practicability of material.
Detailed description of the invention
Fig. 1 is the ir data figure of graphene oxide produced by the present invention.
Specific embodiment
Further description of the technical solution of the present invention with reference to the accompanying drawings and examples, and however, it is not limited to this,
All to be modified to technical solution of the present invention or equivalent replacement, range without departing from the spirit of the technical scheme of the invention should all
Cover within the protection scope of the present invention.
The present invention prepares graphene oxide using graphene using improved Hummers method first, and to oxidation obtained
Graphene carries out examination of infrared spectrum, obtains Fig. 1, and as can be seen from the figure graphene oxide is 3445.6,1622.83,
1115.55cm-1Place occur peak be respectively belonging to-OH ,-COOH in C==O key, C-O-C vibration absorption peak, and
In 874cm-1There is apparent epoxy group feature in place.1384.63cm-1Place is the flexural vibrations peak of O-H.These functional groups
In the presence of illustrating that crystalline flake graphite has been oxidized completely, and the presence of the especially hydroxyl of the polar group on graphene oxide, make it
It is easy to form hydrogen bond with hydrone, here it is graphite oxides and graphene oxide to have the reason of excellent hydrophilic.Meanwhile it is logical
It crosses Mechanics Performance Testing and obtains 1~table of table 8, graphene oxide can be used as the mechanical property that obturator improves original self-repair material
Can, in order to advanced optimize, graphene oxide is added by different proportion, passes through remediation efficiency test and mechanical property
Test synthesis considers, it is determined that the optimal adding proportion of graphene oxide, the best repair of graphene oxide self-healing polymers
Condition.
Specific embodiment 1: present embodiment record be a kind of graphene oxide self-healing polymers preparation side
Method, specific step is as follows for the method:
Step 1: the preparation of graphene oxide: 1.00g~1.50g graphite, 10mL phosphoric acid and 90mL sulfuric acid is taken to be added to
In 500mL there-necked flask, 6g potassium permanganate was divided into 12 times in 1 minute and is uniformly added into there-necked flask, in 4 DEG C of stirred in water bath
1h；
Chemical equation are as follows: KMnO4+H2SO4(dense) → K2SO4+Mn2O7+H2O；
50 DEG C are warming up to, insulated and stirred is for 24 hours；Chemical equation are as follows:
KMnO4+H2SO4+C→MnSO4+CO2+SO2+H2O；
Products therefrom is poured into 0 DEG C of ice water of 250mL, 30% hydrogenperoxide steam generator is added dropwise while stirring to solution colour
Become golden yellow；Chemical equation are as follows:
KMnO4+H2SO4+H2O2→MnSO4+K2SO4+H2O+O4；
It is successively 7 with the pH value that product is centrifuged to supernatant by the dilute hydrochloric acid solution of volume fraction 5% and distilled water, with steaming
Distilled water washing precipitating, then pours into the thick precipitating washed in 100mL beaker, the ultrasound when ultrasonic power is 150W
120 minutes, then sufficiently dry 48h is placed in 70 DEG C of vacuum ovens；
Step 2: the preparation of dendritic oligomer: 30~40g dimeric dibasic acid and 12.3g~16.4g diethylenetriamine are placed on
In 100mL there-necked flask, using magnetic agitation, reaction is condensed back for 24 hours at 160 DEG C, is continually fed into nitrogen during the reaction
Protection, generates dendritic oligomer；
Step 3: the preparation of graphene oxide self-healing polymers: the dendritic oligomer 35g for taking step 2 to prepare, respectively
At 7 parts, then to graphene oxide, 7 parts of dendritic oligomer and 7 parts of graphene oxides made from a step 1 of addition in every part
It corresponds and is added, 7 parts of graphene oxides are 0.05,0.15g, 0.25g, 0.35g, 0.45g, 0.55g, 0.65g respectively；And handle
Every part is all uniformly mixed, then to being separately added into urea 1.18g in every part, cross-linking polymerization 4h at a temperature of 135~160 DEG C,
The graphene oxide self-healing polymers that content is followed successively by 1%, 3%, 5%, 7%, 9%, 11%, 13% are prepared.Benefit
With 4V310-10 air press, the graphene oxide self-healing polymers that will be obtained under the conditions of pressure 0.2MPa, 90 DEG C of temperature
The standard sample of 30*7*1 (unit: mm) is made up of die pressing, that is, completes the preparation of graphene oxide self-healing polymers.It is logical
Cross and change the ratio of graphene oxide additive amount control graphene oxide and prepare material, by carry out remediation efficiency test and
Mechanics Performance Testing, integrated condition, it is determined that the optimal adding proportion of graphene oxide is that 3%, graphene oxide selfreparing is poly-
The best repair condition for closing object is 60 DEG C of reparation 1h.
Comparative example 1:
A kind of preparation method of graphene oxide self-healing polymers, specific step is as follows for the method:
Step 1: the preparation of graphene oxide: 1.00g~1.50g graphite, 10mL phosphoric acid and 90mL sulfuric acid is taken to be added to
In 500mL there-necked flask, 6g potassium permanganate was divided into 12 times in 1 minute and is uniformly added into there-necked flask, in 4 DEG C of stirred in water bath
1h；
Chemical equation are as follows: KMnO4+H2SO4(dense) → K2SO4+Mn2O7+H2O；
50 DEG C are warming up to, insulated and stirred is for 24 hours；Chemical equation are as follows:
KMnO4+H2SO4+C→MnSO4+CO2+SO2+H2O；
Products therefrom is poured into 0 DEG C of ice water of 250mL, 30% hydrogenperoxide steam generator is added dropwise while stirring to solution colour
Become golden yellow；Chemical equation are as follows:
KMnO4+H2SO4+H2O2→MnSO4+K2SO4+H2O+O4；
It is successively 7 with the pH value that product is centrifuged to supernatant by the dilute hydrochloric acid solution of volume fraction 5% and distilled water, with steaming
Distilled water washing precipitating, then pours into the thick precipitating washed in 100mL beaker, the ultrasound when ultrasonic power is 150W
120 minutes, then sufficiently dry 48h is placed in 70 DEG C of vacuum ovens；
Step 2: the preparation of dendritic oligomer: 30~40g dimeric dibasic acid and 12.3g~16.4g diethylenetriamine are placed on
In 100mL there-necked flask, using magnetic agitation, reaction is condensed back for 24 hours at 160 DEG C, is continually fed into nitrogen during the reaction
Protection, generates dendritic oligomer；
Step 3: the preparation of original self-healing polymers: urea is added in the dendritic oligomer 10g for taking step 2 to prepare
2.36g, cross-linking polymerization 4h at a temperature of 135~160 DEG C, obtains original self-healing polymers.
The original self-healing polymers mechanical performance data table of table 1
2 adding proportion of table, 1% graphene oxide self-healing polymers mechanical performance data table
3 adding proportion of table, 3% graphene oxide self-healing polymers mechanical performance data table
4 adding proportion of table, 5% graphene oxide self-healing polymers mechanical performance data table
5 adding proportion of table, 7% graphene oxide self-healing polymers mechanical performance data table
6 adding proportion of table, 9% graphene oxide self-healing polymers mechanical performance data table
7 adding proportion of table, 11% graphene oxide self-healing polymers mechanical performance data table
8 adding proportion of table, 13% graphene oxide self-healing polymers mechanical performance data table
Claims (1)
1. a kind of preparation method of graphene oxide self-healing polymers, it is characterised in that: specific step is as follows for the method:
Step 1: the preparation of graphene oxide: 1.00g~1.50g graphite, 10mL phosphoric acid and 90mL sulfuric acid is taken to be added to 500mL tri-
In mouthful bottle, 6g potassium permanganate was divided into 12 times in 1 minute and is uniformly added into there-necked flask, in 4 DEG C of stirred in water bath 1h；Heating
To 50 DEG C, insulated and stirred is for 24 hours；Products therefrom is poured into 0 DEG C of ice water of 250mL, 30% hydrogenperoxide steam generator is added dropwise while stirring
Become golden yellow to solution colour；
It is successively 7 with the pH value that product is centrifuged to supernatant by the dilute hydrochloric acid solution of volume fraction 5% and distilled water, uses distilled water
Washing precipitating, then pours into the thick precipitating washed in 100mL beaker, 120 points of the ultrasound when ultrasonic power is 150W
Clock, then sufficiently dry 48h is placed in 70 DEG C of vacuum ovens；
Step 2: 30~40g dimeric dibasic acid and 12.3g~16.4g diethylenetriamine the preparation of dendritic oligomer: are placed on 100mL
It in there-necked flask, using magnetic agitation, is condensed back at 160 DEG C for 24 hours, is continually fed into nitrogen protection during the reaction, generated
Dendritic oligomer；
Step 3: the preparation of graphene oxide self-healing polymers: the dendritic oligomer 35g for taking step 2 to prepare is divided into 7
Part, then to graphene oxide, 7 parts of dendritic oligomer and 7 parts of graphene oxides one made from a step 1 of addition in every part
One corresponding addition, 7 parts of graphene oxides are 0.05,0.15g, 0.25g, 0.35g, 0.45g, 0.55g, 0.65g respectively；And every
Part is all uniformly mixed, then to being separately added into urea 1.18g in every part, cross-linking polymerization 4h at a temperature of 135~160 DEG C, i.e.,
The graphene oxide self-healing polymers that content is followed successively by 1%, 3%, 5%, 7%, 9%, 11%, 13% are prepared.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112280056A (en) * | 2020-11-06 | 2021-01-29 | 湖南科技大学 | Preparation method of repairable graphene oxide material based on hydrogen bond effect |
| CN112442253A (en) * | 2019-08-29 | 2021-03-05 | 邵武市万家美家居用品制造有限公司 | Filter net bag and preparation method thereof |
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Application publication date: 20181214 |