CN107236262A - A kind of method for preparing polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film - Google Patents
A kind of method for preparing polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film Download PDFInfo
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- CN107236262A CN107236262A CN201710463319.1A CN201710463319A CN107236262A CN 107236262 A CN107236262 A CN 107236262A CN 201710463319 A CN201710463319 A CN 201710463319A CN 107236262 A CN107236262 A CN 107236262A
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- hydroxy group
- terminal hydroxy
- carbon nanotube
- walled carbon
- ethylene glycol
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/08—Heat treatment
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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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Abstract
A kind of method for preparing polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film, comprises the following steps：1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, the terminal hydroxy group multi-walled carbon nanotube for weighing different quality is placed into 10mL N, N dimethylformamides（DMF）In solvent, ultrasonic disperse 1h；2）Weigh the polyadipate ethylene glycol of different quality and be dissolved in 10mL DMF；3）By step 1）With step 2）The solution of acquisition is mixed in proportion, and ultrasonic disperse 2h is used after mechanical agitation, Casting solution is obtained；4）Pipette casting solution film-forming on Thermostatic platform；5）By step 4）In obtained blend film eliminate thermal history, be cooled to 25 DEG C ~ 35 DEG C isothermal crystals, and make to be fully crystallized；Technique is simple, easy to operate, short preparation period, can be achieved as a kind of degradability functional high molecule material, and in capacitor, sensor, biomedical devices aspect has potential application value.
Description
Technical field
The invention belongs to prepare the technology neck of polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film
A kind of domain, and in particular to method for preparing polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film.
Background technology
With deteriorating increasingly and concern of the people to living environment for environmental problem, Biodegradable material is received extensively
Concern.Aliphatic polyester is due to its biological degradability and excellent biocompatibility, it has also become the focus of research.Polyadipate second
Diol ester is a kind of excellent aliphatic polyester, easily by the enzyme decomposition in the multiple-microorganism in nature or animal and plant body, generation
Thank, ultimately form carbon dioxide and water.But polyadipate ethylene glycol is present, and crystallinity is low, molding rate slow, heat endurance and thing
The defects such as mechanicalness is poor are managed, this greatly limits its extensive use.At present, used people more with the copolymerization such as PLA or
Improve the heat endurance and mechanical performance of polyadipate ethylene glycol with the method such as polyvinylidene blending, but with nano combined research
It is very few.Multi-walled carbon nanotube has larger draw ratio and specific surface area, and polymer composites can be assigned as Nano filling
Excellent mechanical strength, extremely low thermal coefficient of expansion and processing characteristics.Compared with traditional filler, only add a small amount of terminal hydroxy group
Multi-walled carbon nanotube can increase substantially the mechanics of material, electrically and thermally property, so as to prepare high-performance and multi-functional
The polymer matrix composite of change provides new way.
Polyadipate ethylene glycol is added after terminal hydroxy group multi-walled carbon nanotube, can quickly improve the knot of polyadipate ethylene glycol
Brilliant temperature simultaneously shortens its molding cycle, improves mechanical property.Future has widely in intelligent degradable material, electric capacity, medical industry
Potentiality.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, it is an object of the invention to provide one kind prepare polyadipate ethylene glycol/
The method of terminal hydroxy group multi-walled carbon nanotube nano compound film, improves polyadipate ethylene glycol crystallization temperature, strengthens mechanical property,
Process is simple, and obtained composite not only has excellent mechanical property but also substantially reduces molding cycle.
To achieve these goals, the technical solution adopted by the present invention is：One kind prepares polyadipate ethylene glycol/terminal hydroxy group
The method of multi-walled carbon nanotube nano compound film, comprises the following steps：
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh the 0.001g~0.003g many wall carbon of terminal hydroxy group
Nanotube is placed into 10ml N,N-dimethylformamides（DMF）In solvent, ultrasonic disperse 1h obtains terminal hydroxy group multi-wall carbon nano-tube
Pipe solution；
2）Weigh 0.3g~0.5g polyadipate ethylene glycol and be dissolved in 10mL DMF, obtain polyadipate ethylene glycol molten
Liquid；
3）By step 1）With step 2）Solution mix in proportion, ultrasonic disperse 2h is continuing with after mechanical agitation 30min, finally
So that terminal hydroxy group multi-walled carbon nanotube is well mixed with polyadipate ethylene glycol, polyadipate ethylene glycol/many walls of terminal hydroxy group are obtained
CNT Casting solution；
4）By step 3）The Casting solution of acquisition film-forming on 20 DEG C ~ 40 DEG C of Thermostatic platform, is made blend film；
5）By step 4）In three kinds of blend films of obtained different quality ratio melt 8min on 80 DEG C of Thermostatic platform and eliminates
Thermal history, is then cooled to 25 DEG C ~ 35 DEG C isothermal crystal 2h ~ 4h, and make to be fully crystallized with 60 DEG C/min speed；
Blend film after crystallization is used into wide-angle X ray diffractor, differential scanning calorimeter, petrographic microscope and scanning electron
The means such as microscope characterize the crystal morphology feature of polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film with
Crystallization temperature.
The beneficial effects of the invention are as follows：
The present invention prepares a kind of polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film using solution cast,
Cultivated at the temperature of the present invention and under different ratio, a kind of aliphatic Biodegradable film of high added value of preparation.This hair
It is bright employ crystalline organic polymer Material cladding inorganic nano-filler prepare it is environmentally friendly thin with excellent high additional properties
The material that membrane material replaces high pollution, is not easily decomposed, is expected to obtain in fields such as conductive material, functional coatings, degraded multipotencys
It is widely applied.The present invention shortens shaping week by improving polyadipate ethylene glycol crystallization temperature, change crystalline size size
Phase, improve the added value of composite.
Brief description of the drawings
Fig. 1 is petrographic microscope shape appearance figure of the present invention, wherein Fig. 1（a）For the petrographic microscope shape appearance figure of embodiment 1；Fig. 1
（b）For the petrographic microscope shape appearance figure of embodiment 2；Fig. 1（c）For the petrographic microscope shape appearance figure of embodiment 3.
Fig. 2 is that differential scanning calorimeter cools figure, in wherein Fig. 2 PEA, PEA-0.2 and PEA-0.4 be respectively embodiment 1,
The differential scanning calorimeter cooling figure of embodiment 2 and embodiment 3.
Embodiment
The present invention is described in further detail with reference to specific embodiment.
Embodiment 1（Embodiment 1 is comparative example, is answering of being prepared in the case of without terminal hydroxy group multi-walled carbon nanotube
Close film）：
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh 0.000g terminal hydroxy group multi-walled carbon nanotube simultaneously
Insert N,N-dimethylformamide 10mL（DMF）In solvent, ultrasonic disperse 1h；
2）Weigh 0.5g polyadipate ethylene glycol and be dissolved in 10mL DMF；
3）By step 1）With step 2）Two solution obtained press 0.5:Continue to make after 0.000 ratio mixing, mechanical agitation 30min
Use ultrasonic disperse 2h, finally terminal hydroxy group multi-walled carbon nanotube be well mixed with polyadipate ethylene glycol, obtain it is pure it is poly- oneself two
Sour ethylene glycol Casting solution；
4）Pipette casting solution and be solidified into blend film on 40 DEG C of Thermostatic platforms；
5）By step 4）In obtained blend film melt 8min elimination thermal histories on 80 DEG C of Thermostatic platform, then with 60 DEG C/
Min speed is cooled to 32 DEG C of isothermal crystal 4h, and makes to be fully crystallized；
6）Blend film after crystallization is used into wide-angle X ray diffractor, differential scanning calorimeter, petrographic microscope and scanning
The crystallization temperature that the means such as electron microscope characterize polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film is
14.98 DEG C, spherulite size is 200 μm.
Embodiment 2：
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh 0.001g terminal hydroxy group multi-walled carbon nanotube simultaneously
Insert N,N-dimethylformamide 10ml（DMF）In solvent, ultrasonic disperse 1h；
2）Weigh 0.5g polyadipate ethylene glycol and be dissolved in 10mL DMF；
3）By step 1）With step 2）Two solution obtained press 0.5:Continue to make after 0.001 ratio mixing, mechanical agitation 30min
Ultrasonic disperse 2h is used, finally terminal hydroxy group multi-walled carbon nanotube is well mixed with polyadipate ethylene glycol, obtaining proportioning is
The Casting solution of 0.2% polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube；
4）Pipette casting solution and be solidified into blend film on 20 DEG C of Thermostatic platforms；
5）By step 4）In obtained blend film melt 8min elimination thermal histories on 80 DEG C of Thermostatic platform, then with 60
DEG C/min speed is cooled to 25 DEG C of isothermal crystal 3h, and makes to be fully crystallized.
Blend film after crystallization is used into wide-angle X ray diffractor, differential scanning calorimeter, petrographic microscope and scanning
The crystallization temperature that the means such as electron microscope characterize polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film is
24.43℃；
Embodiment 3
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh 0.002g terminal hydroxy group multi-walled carbon nanotube simultaneously
Insert N,N-dimethylformamide 10mL（DMF）In solvent, ultrasonic disperse 1h；
2）Weigh 0.5g polyadipate ethylene glycol and be dissolved in 10mL DMF；
3）By step 1）With step 2）Two solution obtained press 0.5:Continue to make after 0.002 ratio mixing, mechanical agitation 30min
Ultrasonic disperse 2h is used, finally terminal hydroxy group multi-walled carbon nanotube is well mixed with polyadipate ethylene glycol, obtaining proportioning is
0.4% polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube Casting solution；
4）Pipette casting solution and be solidified into blend film on 30 DEG C of Thermostatic platforms；
5）By step 4）In obtained blend film melt 8min elimination thermal histories on 80 DEG C of Thermostatic platform, then with 60 DEG C/
Min speed is cooled to 30 DEG C of isothermal crystal 2h, and makes to be fully crystallized.
Blend film after crystallization is used into wide-angle X ray diffractor, differential scanning calorimeter, petrographic microscope and scanning
The crystallization temperature that the means such as electron microscope characterize polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film is
27.06 DEG C, generate the broken grain less than 20 μm；
Embodiment 4
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh 0.003g terminal hydroxy group multi-walled carbon nanotube simultaneously
Insert N,N-dimethylformamide 10mL（DMF）In solvent, ultrasonic disperse 1h；
2）Weigh 0.4g polyadipate ethylene glycol and be dissolved in 10mL DMF；
3）By step 1）With step 2）Two solution obtained press 0.5:Continue to make after 0.002 ratio mixing, mechanical agitation 30min
Ultrasonic disperse 2h is used, finally terminal hydroxy group multi-walled carbon nanotube is well mixed with polyadipate ethylene glycol, obtaining proportioning is
0.4% polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube Casting solution；
4）Pipette casting solution and be solidified into blend film on 40 DEG C of Thermostatic platforms；
5）By step 4）In obtained blend film melt 8min elimination thermal histories on 80 DEG C of Thermostatic platform, then with 60 DEG C/
Min speed is cooled to 30 DEG C of isothermal crystal 3h, and makes to be fully crystallized.
Referring to Fig. 2 and in conjunction with the embodiments it can be seen from 1,2,3, CNT is added, compared with pure, the crystallization temperature of blend film is improved
It is a lot, improve 10 DEG C.
Claims (5)
1. a kind of method for preparing polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube nano compound film, it is characterised in that
Comprise the following steps：
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh the 0.001g~0.003g many wall carbon of terminal hydroxy group
Nanotube is placed into 10mL N,N-dimethylformamides（DMF）In solvent, ultrasonic disperse 1h obtains terminal hydroxy group multi-wall carbon nano-tube
Pipe solution；
2）Weigh 0.3g~0.6g polyadipate ethylene glycol and be dissolved in 10mL DMF, obtain polyadipate ethylene glycol molten
Liquid；
3）By step 1）With step 2）Solution mix in proportion, ultrasonic disperse 2h is continuing with after mechanical agitation 30min, finally
So that terminal hydroxy group multi-walled carbon nanotube is well mixed with polyadipate ethylene glycol, polyadipate ethylene glycol/many walls of terminal hydroxy group are obtained
The Casting solution of CNT；
4）By step 3）The Casting solution of acquisition film-forming on 20 DEG C ~ 40 DEG C of Thermostatic platform, is made blend film；
5）By step 4）In the blend film of obtained different quality ratio melt 8min eliminations heat on 80 DEG C of Thermostatic platform and goes through
History, is then cooled to 25 DEG C ~ 35 DEG C isothermal crystal 2h ~ 4h, and make to be fully crystallized with 60 DEG C/min speed.
2. the method for polyadipate ethylene glycol according to claim 1/terminal hydroxy group multi-walled carbon nanotube nano compound film,
Characterized in that, described step 3）Solution press 0.5:0.001 or 0.5:0.002 ratio mixing.
3. the method for polyadipate ethylene glycol according to claim 1/terminal hydroxy group multi-walled carbon nanotube nano compound film,
It is characterised in that it includes there is following steps：
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh 0.001g terminal hydroxy group multi-walled carbon nanotube simultaneously
Insert N,N-dimethylformamide 10ml（DMF）In solvent, ultrasonic disperse 1h；
2）Weigh 0.5g polyadipate ethylene glycol and be dissolved in 10mL DMF；
3）By step 1）With step 2）Two solution obtained press 0.5:Continue to make after 0.001 ratio mixing, mechanical agitation 30min
Ultrasonic disperse 2h is used, finally terminal hydroxy group multi-walled carbon nanotube is well mixed with polyadipate ethylene glycol, obtaining proportioning is
The Casting solution of 0.2% polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube；
4）Pipette casting solution and be solidified into blend film on 20 DEG C of Thermostatic platforms；
5）By step 4）In obtained blend film melt 8min elimination thermal histories on 80 DEG C of Thermostatic platform, then with 60
DEG C/min speed is cooled to 25 DEG C of isothermal crystal 3h, and makes to be fully crystallized.
4. the method for polyadipate ethylene glycol according to claim 1/terminal hydroxy group multi-walled carbon nanotube nano compound film,
It is characterised in that it includes there is following steps：
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh 0.002g terminal hydroxy group multi-walled carbon nanotube simultaneously
Insert N,N-dimethylformamide 10mL（DMF）In solvent, ultrasonic disperse 1h；
2）Weigh 0.5g polyadipate ethylene glycol and be dissolved in 10mL DMF；
3）By step 1）With step 2）Two solution obtained press 0.5:Continue to make after 0.002 ratio mixing, mechanical agitation 30min
Ultrasonic disperse 2h is used, finally terminal hydroxy group multi-walled carbon nanotube is well mixed with polyadipate ethylene glycol, obtaining proportioning is
0.4% polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube Casting solution；
4）Pipette casting solution and be solidified into blend film on 30 DEG C of Thermostatic platforms；
5）By step 4）In obtained blend film melt 8min elimination thermal histories on 80 DEG C of Thermostatic platform, then with 60 DEG C/
Min speed is cooled to 30 DEG C of isothermal crystal 2h, and makes to be fully crystallized.
5. the method for polyadipate ethylene glycol according to claim 1/terminal hydroxy group multi-walled carbon nanotube nano compound film,
It is characterised in that it includes there is following steps：
1）Taken out after terminal hydroxy group multi-walled carbon nanotube is dried in vacuo 3 days, weigh 0.003g terminal hydroxy group multi-walled carbon nanotube simultaneously
Insert N,N-dimethylformamide 10mL（DMF）In solvent, ultrasonic disperse 1h；
2）Weigh 0.4g polyadipate ethylene glycol and be dissolved in 10mL DMF；
3）By step 1）With step 2）Two solution obtained press 0.5:Continue to make after 0.002 ratio mixing, mechanical agitation 30min
Ultrasonic disperse 2h is used, finally terminal hydroxy group multi-walled carbon nanotube is well mixed with polyadipate ethylene glycol, obtaining proportioning is
0.4% polyadipate ethylene glycol/terminal hydroxy group multi-walled carbon nanotube Casting solution；
4）Pipette casting solution and be solidified into blend film on 40 DEG C of Thermostatic platforms；
5）By step 4）In obtained blend film melt 8min elimination thermal histories on 80 DEG C of Thermostatic platform, then with 60 DEG C/
Min speed is cooled to 30 DEG C of isothermal crystal 3h, and makes to be fully crystallized.
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Cited By (2)
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| CN110699949A (en) * | 2019-11-01 | 2020-01-17 | 电子科技大学 | Flexible self-adhesive cloth with pressure/friction force sensing function, flexible mechanical sensor and preparation method of flexible mechanical sensor |
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