CN105949536A - {0><}0{>Preparation method of high-strength natural rubber (NR)/carbon nano tube (CNT) conductive composite film - Google Patents
{0><}0{>Preparation method of high-strength natural rubber (NR)/carbon nano tube (CNT) conductive composite film Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
- C08L7/02—Latex
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- 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
- C08J2307/00—Characterised by the use of natural rubber
- C08J2307/02—Latex
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- 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
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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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
- C08K2201/00—Specific properties of additives
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
{0><}0{>The invention provides a preparation method of a high-strength natural rubber (NR)/carbon nano tube (CNT) conductive composite film. <0}{0><}0{>The method comprises the following steps of: uniformly dispersing the CNT with nano cellulose (CNF) serving as a dispersant, so as to form a stable CNF/CNT suspension; <0}{0><}0{>And then adding the suspension into the NR in a certain proportion, further adding a certain weight percentage of vulcanization dispersoid, and preparing NR/CNT composite films different in thickness by virtue of a latex blending method. <0}{0><}0{>The preparation method has the advantages that nano cellulose is taken as a green dispersant and is capable of uniformly dispersing the CNT into the NR under a physical action, so that the high-strength and good-conductibility NR/CNT composite film is prepared.
Description
Technical field
The present invention relates to a kind of natural rubber/carbon nanotube conducting laminated film with high intensity and preparation method thereof, its technological core is using biomass nano cellulose as dispersant, CNT is dispersed in natural rubber, thus prepare the natural rubber/carbon nano-tube coextruded film of high intensity, good conductivity, belong to Wood Science and Technology field.
Background technology
Natural rubber (NR) is a kind of natural polymer with polyisoprene as main component, and wherein the moon 91% ~ 94% is rubber hydrocarbon, and remaining is the nonrubber compositions such as protein, fatty acid, ashes, saccharide.As a kind of green Renewable resource, along with expanding economy and people use the enhancing that green resource realize, the Chinese degree of dependence to NR the most constantly promotes, and demand increases day by day.But, owing to the free volume of natural rubber is relatively big, intermolecular force is more weak, thus its intensity and modulus are the lowest, so just having higher use value after reinforcement, bad mechanical property (especially tearing toughness is the highest) is the highly desirable problems having been resolved of one, NR goods.
CNT (CNTs) is by the seamless nanoscale tubular shell Rotating fields of single or multiple lift graphite flake curling, having the biggest draw ratio, the intensity of superelevation and modulus, good toughness, density is low, conduction, heat conductivity are good, therefore it becomes the important filler that rubber reinforcement is modified.Owing to CNTs has good mechanical property, rubber adds CNTs and is conducive to improving the mechanical property of rubber, and improve the advantages such as heat stability.
Owing to the filler of micro-meter scale is little to the enhancing of mechanical properties of polymer, and the filler of nanoscale is little due to its particle diameter, specific surface area is big, because its skin effect (such as small-size effect, quantum effect, unsaturated valency electrical effect and electron tunneling effect etc.) is greatly improved and active force between polymer macromolecule, macromolecular material can be played obvious reinforced effects by nanoparticle when consumption is little.Therefore, the dispersion how making nanoparticle be really achieved nanoscale in substrate then becomes the key issue that nanometer strengthens, and is also the high molecule nano composite material difficult problem that fails for a long time to be solved very well.Similarly, when using CNT to strengthen natural rubber, CNT is in the dispersed emphasis becoming research of natural rubber substrate and difficult point.At present, in order to improve CNT dispersibility in natural rubber, numerous studies are mainly concentrated the strong acid chemical to CNT to process and add the methods such as surfactant.
Fang Qinghong etc. utilize sulphuric acid at high temperature CNT to be carried out surface process with the mixed acid of nitric acid, the chemical bond point making its surface produce after destroying with a small amount of hydrogen atom, free radical and oxygen-containing functional group and strong acid, improves the interface binding power of CNT and natural rubber to a certain extent；
Jiang waits the surfactant utilizing silane coupler as CNT quietly, preferably improves the interface cohesion between CNT and rubber.But, after strong acid treatment, the cost of product is significantly increased, and, after strong acid destroys, CNT self-strength substantially reduces, and electrical conductivity is also remarkably decreased, and similarly, after adding surfactant, the electrical conductivity of CNT also significantly decreases.
Biomass cellulose nanofibers has high radial direction ratio, the advantages such as high mechanical properties, low-thermal-expansion rate and low-density, can mention in the same breath with CNT, simultaneously, biomass nano cellulose is also a kind of physical dispersion agent, can improve nanoparticle dispersibility in substrate.Owing between nano-cellulose and nanoparticle being a kind of physical dispersion effect, so the performance of nanoparticle self will not be produced impact.
Summary of the invention
What the present invention proposed is a kind of natural rubber/carbon nanotube conducting laminated film with high intensity and preparation method thereof, its purpose is intended to the drawbacks described above overcome existing for prior art, with nano-cellulose as dispersant, by physical action, CNT is dispersed in natural rubber substrate, form stable nano-cellulose/carbon nano tube suspension, the most by a certain percentage this suspension is added in natural rubber, add the vulcanized disperse body of certain mass mark, use high temperature to prolong sulfur method and be prepared as high intensity, natural rubber/the carbon nano-tube coextruded film of good conductivity.
The technical solution of the present invention: the preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity, comprises the steps:
(1) weigh 1g nano-cellulose to be dissolved in 1L distilled water, be put on magnetic stirring apparatus stirring 4～6h, ultrasonic 20～35min, continue magnetic agitation 0.5h, more ultrasonic 8～12min, obtain the nanofiber cellulose solution that concentration is 1g/L；
(2) with biomass as raw material, TEMPO oxidizing process is used to prepare nano-cellulose；
(3) preparation CNT and the mass ratio of nano-cellulose；Weigh 0.8g CNT and add step 2) in concentration be 1g/L the nanofiber cellulose solution of 1L in, the mass ratio of CNT and nano-cellulose is 0.8:1；
(4) carbon nanotube/nano cellulose solution is put on magnetic stirring apparatus: then
1) 8～12h are stirred under room temperature, ultrasonic 30～45min；
2) magnetic agitation 2～4h at normal temperatures, more ultrasonic 15～25min are continued；
3) for centrifugal 6～8min under rotating speed is 8000～1000r/min；
4) finely dispersed carbon nanotube/nano cellulose suspension is obtained；
(5) according to Lang Bo-Beer law and utilize UV-vis-NIR calculate in step (4) centrifugal after the actual concentration of CNT in carbon nanotube/nano cellulose suspension；
(6) after weighing the 10g natural rubber that solid content is 60%:
1) it is placed in beaker；
2) being respectively 2% by CNT and natural rubber mass ratio, 5%, 8%, 10%, 12% measures the carbon nano tube suspension obtained by step (5) mixes with the Heveatex (NR) of 10g；
(7) by the CNT of different quality ratio/natural rubber mixed liquor in step (6):
1) magnetic agitation 3～4h under temperature 70 C；
2) add in vulcanized disperse body in the ratio of natural rubber dry glue/vulcanized disperse body solid content 50:1；
3) stirring 2～3h, set aside for use are continued；
(8) formula of the every 100g of vulcanized disperse body in step (7): sulfur 25g, ZnO12.5g, ZDC12.5g, 10% casein 20g, 20%KOH10g, distilled water 20g, solid content is 45%；
(9) mixed liquor obtained by step (7) filtered, stand 3～5h, pour casting film-forming in the glass plate of horizontal positioned into, natural coagulation is dried, 1～2h is boiled in 65～80 DEG C of water-baths, hang up and drain, then place and vacuum drying oven is dried at 60～80 DEG C 4～8h, i.e. obtain the CNT/Heveatex conductive composite film of high intensity.
Advantages of the present invention: CNT, with nano-cellulose as dispersant, can be dispersed in natural rubber by the present invention, thus prepare intensity height, the natural rubber/carbon nano-tube coextruded film of good conductivity.
Detailed description of the invention
nullEmbodiment 1: take the 10g natural rubber that solid content is 60% and be placed in beaker，It is that 2% Heveatex (NR) weighing CNT 0.12g with 10g mixes by CNT and natural rubber mass ratio，Then magnetic agitation 4h at 70 DEG C，Press natural rubber dry glue/vulcanized disperse body (formula of every 100g: sulfur 25g again、ZnO12.5g、ZDC12.5g、10% casein 20g、20%KOH10g、Distilled water 20g，Solid content is 45%) ratio of solid content 50:1 adds vulcanized disperse body and continues stirring 2h，It is filtrated to get the mixed liquor after filtration again by vacuum，Stand 5h，Pour casting film-forming in the glass plate of horizontal positioned into，Natural coagulation is dried，1h is boiled in 80 DEG C of water-baths，Hang up and drain，Then place and vacuum drying oven is dried at 80 DEG C 6h，Obtain the CNT/Heveatex conductive composite film of high intensity.
Embodiment 2: weigh nano-cellulose prepared by 1g TEMPO oxidizing process and be dissolved in 1L distilled water, is put on magnetic stirring apparatus stirring 4h, ultrasonic 30 min, continues magnetic agitation 0.5 h, more ultrasonic 10 min, obtains the nanofiber cellulose solution that concentration is 1g/L.It is the ratio of 0.8:1 in CNT and nano-cellulose mass ratio, weigh in the nanofiber cellulose solution of the 1L that 0.8g CNT adds 1g/L, then on magnetic stirring apparatus, stir 8 h, after ultrasonic 30 min, continue magnetic agitation 4 h at normal temperatures, the most ultrasonic 20 min, then for centrifugal 8 min under rotating speed is 8000 r/min, finally obtain finely dispersed carbon nanotube/nano cellulose suspension, according to Lang Bo-Beer law and utilize UV-vis-NIR calculate centrifugal after in carbon nanotube/nano cellulose suspension the actual concentration of CNT be 0.6 g/L.nullWeigh the 10g natural rubber that solid content is 60% to be placed in beaker，Then it is 2% to measure 120 ml carbon nano tube suspension and mix then magnetic agitation 4h at 70 DEG C with the Heveatex (NR) of 10g by CNT and natural rubber mass ratio，Press natural rubber dry glue/vulcanized disperse body (formula of every 100g: sulfur 25g again、ZnO12.5g、ZDC12.5g、10% casein 20g、20%KOH10g、Distilled water 20g，Solid content is 45%) ratio of solid content 50:1 adds vulcanized disperse body and continues stirring 2h，It is filtrated to get the mixed liquor after filtration again by vacuum，Stand 5h，Pour casting film-forming in the glass plate of horizontal positioned into，Natural coagulation is dried，1h is boiled in 80 DEG C of water-baths，Hang up and drain，Then place and vacuum drying oven is dried at 80 DEG C 6h，Obtain the CNT/Heveatex conductive composite film of high intensity.
Embodiment 3: weigh nano-cellulose prepared by 1g TEMPO oxidizing process and be dissolved in 1L distilled water, is put on magnetic stirring apparatus stirring 4h, ultrasonic 30 min, continues magnetic agitation 0.5 h, more ultrasonic 10 min, obtains the nanofiber cellulose solution that concentration is 1g/L.It is the ratio of 0.8:1 in CNT and nano-cellulose mass ratio, weigh in the nanofiber cellulose solution of the 1L that 0.8g CNT adds 1g/L, then on magnetic stirring apparatus, stir 8 h, after ultrasonic 30 min, continue magnetic agitation 4 h at normal temperatures, the most ultrasonic 20 min, then for centrifugal 8 min under rotating speed is 8000 r/min, finally obtain finely dispersed carbon nanotube/nano cellulose suspension, according to Lang Bo-Beer law and utilize UV-vis-NIR calculate centrifugal after in carbon nanotube/nano cellulose suspension the actual concentration of CNT be 0.6 g/L.nullWeigh the 10g natural rubber that solid content is 60% to be placed in beaker，Then it is 5% to measure 500 ml carbon nano tube suspension and mix then magnetic agitation 4h at 70 DEG C with the Heveatex (NR) of 10g by CNT and natural rubber mass ratio，Press natural rubber dry glue/vulcanized disperse body (formula of every 100g: sulfur 25g again、ZnO12.5g、ZDC12.5g、10% casein 20g、20%KOH10g、Distilled water 20g，Solid content is 45%) ratio of solid content 50:1 adds vulcanized disperse body and continues stirring 2h，It is filtrated to get the mixed liquor after filtration again by vacuum，Stand 5h，Pour casting film-forming in the glass plate of horizontal positioned into，Natural coagulation is dried，1h is boiled in 80 DEG C of water-baths，Hang up and drain，Then place and vacuum drying oven is dried at 80 DEG C 6h，Obtain the CNT/Heveatex conductive composite film of high intensity.
Embodiment 4: weigh nano-cellulose prepared by 1g TEMPO oxidizing process and be dissolved in 1L distilled water, is put on magnetic stirring apparatus stirring 4h, ultrasonic 30 min, continues magnetic agitation 0.5 h, more ultrasonic 10 min, obtains the nanofiber cellulose solution that concentration is 1g/L.It is the ratio of 0.8:1 in CNT and nano-cellulose mass ratio, weigh in the nanofiber cellulose solution of the 1L that 0.8g CNT adds 1g/L, then on magnetic stirring apparatus, stir 8 h, after ultrasonic 30 min, continue magnetic agitation 4 h at normal temperatures, the most ultrasonic 20 min, then for centrifugal 8 min under rotating speed is 8000 r/min, finally obtain finely dispersed carbon nanotube/nano cellulose suspension, according to Lang Bo-Beer law and utilize UV-vis-NIR calculate centrifugal after in carbon nanotube/nano cellulose suspension the actual concentration of CNT be 0.6 g/L.nullWeigh the 10g natural rubber that solid content is 60% to be placed in beaker，Then it is 8% to measure 800 ml carbon nano tube suspension and mix then magnetic agitation 4h at 70 DEG C with the Heveatex (NR) of 10g by CNT and natural rubber mass ratio，Press natural rubber dry glue/vulcanized disperse body (formula of every 100g: sulfur 25g again、ZnO12.5g、ZDC12.5g、10% casein 20g、20%KOH10g、Distilled water 20g，Solid content is 45%) ratio of solid content 50:1 adds vulcanized disperse body and continues stirring 2h，It is filtrated to get the mixed liquor after filtration again by vacuum，Stand 5h，Pour casting film-forming in the glass plate of horizontal positioned into，Natural coagulation is dried，1h is boiled in 80 DEG C of water-baths，Hang up and drain，Then place and vacuum drying oven is dried at 80 DEG C 6h，Obtain the CNT/Heveatex conductive composite film of high intensity.
Performance comparision:
Claims (10)
1. there is a preparation method for the natural rubber/carbon nanotube conducting laminated film of high intensity, it is characterized in that the method comprises the steps:
(1) the nanofiber cellulose solution that concentration is 1g/L is prepared；
(2) nano-cellulose is prepared；
(3) preparation CNT and the mass ratio of nano-cellulose；
(4) finely dispersed carbon nanotube/nano cellulose suspension is prepared；
(5) actual concentration of CNT is calculated；
(6) carbon nano tube suspension mixes with the Heveatex (NR) of 10g；
(7) CNT of different quality ratio/natural rubber mixing；
(8) formulating vulcanization dispersion；
(9) CNT/Heveatex conductive composite film of high intensity is obtained.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, it is characterized in that described step (1) prepares the nanofiber cellulose solution that concentration is 1g/L: weigh 1g nano-cellulose and be dissolved in 1L distilled water, it is put on magnetic stirring apparatus stirring 4～6h, ultrasonic 20～35min, continue magnetic agitation 0.5h, the most ultrasonic 8～12min, obtain the nanofiber cellulose solution that concentration is 1g/L.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, it is characterized in that described step (2) prepares nano-cellulose: with biomass as raw material, use TEMPO oxidizing process to prepare nano-cellulose.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, is characterized in that the mass ratio of described step (3) preparation CNT and nano-cellulose；Weigh 0.8g CNT and add step 2) in concentration be 1g/L the nanofiber cellulose solution of 1L in, the mass ratio of CNT and nano-cellulose is 0.8:1.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, is characterized in that described step (4) prepares finely dispersed carbon nanotube/nano cellulose suspension: be put on magnetic stirring apparatus by carbon nanotube/nano cellulose solution: then
1) 8～12h are stirred at normal temperatures, ultrasonic 30～45min；
2) magnetic agitation 2～4h at normal temperatures, more ultrasonic 15～25min are continued；
3) for centrifugal 6～8min under rotating speed is 8000～1000r/min；
4) finely dispersed carbon nanotube/nano cellulose suspension is obtained.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, is characterized in that described step (5) calculates the actual concentration of CNT: according to Lang Bo-Beer law and utilize UV-vis-NIR calculate in step (4) centrifugal after the actual concentration of CNT in carbon nanotube/nano cellulose suspension.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, it is characterized in that described step (6) carbon nano tube suspension mixes with the Heveatex (NR) of 10g: weigh the 10g natural rubber that solid content is 60%, then
1) it is placed in beaker；
2) being respectively 2% by CNT and natural rubber mass ratio, 5%, 8%, 10%, 12% measures the carbon nano tube suspension obtained by step (5) mixes with the Heveatex (NR) of 10g.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, is characterized in that the CNT/natural rubber mixing of described step (7) different quality ratio: by the CNT of different quality ratio/natural rubber mixed liquor in step (6):
1) magnetic agitation 3～4h under temperature 70 C；
2) add in vulcanized disperse body in the ratio of natural rubber dry glue/vulcanized disperse body solid content 50:1；
3) continue stirring 2～3h, obtain the CNT/natural rubber mixed liquor of different quality ratio, set aside for use.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, is characterized in that described step (8) formulating vulcanization dispersion:
By the vulcanized disperse body in step (7), the formula of every 100g: sulfur 25g, ZnO12.5g, ZDC12.5g, 10% casein 20g, 20%KOH10g, distilled water 20g, solid content is 45%.
The preparation method of a kind of natural rubber/carbon nanotube conducting laminated film with high intensity the most according to claim 1, it is characterized in that described step (9) obtains the CNT/Heveatex conductive composite film of high intensity: filtered by the mixed liquor obtained by step (7), stand 3～5h, pour casting film-forming in the glass plate of horizontal positioned into, natural coagulation is dried, 1～2h is boiled in 65～80 DEG C of water-baths, hang up and drain, then place and vacuum drying oven is dried at 60～80 DEG C 4～8h, i.e. obtain the CNT/Heveatex conductive composite film of high intensity.
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Cited By (7)
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|---|---|---|---|---|
| CN107383443A (en) * | 2017-06-12 | 2017-11-24 | 西北农林科技大学 | A kind of laminated film of gutta-percha and nano-cellulose and preparation method thereof |
| CN108440802A (en) * | 2018-04-20 | 2018-08-24 | 南京林业大学 | A kind of preparation method of flexible conducting material |
| CN109251342A (en) * | 2018-07-12 | 2019-01-22 | 南京林业大学 | A kind of nano-cellulose/carbon nano-tube/poly dimethyl siloxane conductive composite film and preparation method thereof |
| CN110003503A (en) * | 2019-04-09 | 2019-07-12 | 江苏通用科技股份有限公司 | The preparation method of high-dispersibility carbon nanotube base rubber composite material |
| CN110218365A (en) * | 2019-07-11 | 2019-09-10 | 陕西延长石油(集团)有限责任公司研究院 | A kind of natural rubber carbon nano tube compound material and preparation method thereof |
| CN112961412A (en) * | 2021-01-25 | 2021-06-15 | 昆明理工大学 | Method and device for preparing ultrahigh-sensitivity natural rubber nano composite sensing material |
| CN114147214A (en) * | 2021-11-29 | 2022-03-08 | 西安理工大学 | Preparation method of carbon nano tube reinforced magnesium-based composite material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107383443A (en) * | 2017-06-12 | 2017-11-24 | 西北农林科技大学 | A kind of laminated film of gutta-percha and nano-cellulose and preparation method thereof |
| CN108440802A (en) * | 2018-04-20 | 2018-08-24 | 南京林业大学 | A kind of preparation method of flexible conducting material |
| CN109251342A (en) * | 2018-07-12 | 2019-01-22 | 南京林业大学 | A kind of nano-cellulose/carbon nano-tube/poly dimethyl siloxane conductive composite film and preparation method thereof |
| CN109251342B (en) * | 2018-07-12 | 2021-02-02 | 南京林业大学 | Nano-cellulose/carbon nano-tube/polydimethylsiloxane conductive composite membrane and preparation method thereof |
| CN110003503A (en) * | 2019-04-09 | 2019-07-12 | 江苏通用科技股份有限公司 | The preparation method of high-dispersibility carbon nanotube base rubber composite material |
| CN110218365A (en) * | 2019-07-11 | 2019-09-10 | 陕西延长石油(集团)有限责任公司研究院 | A kind of natural rubber carbon nano tube compound material and preparation method thereof |
| CN112961412A (en) * | 2021-01-25 | 2021-06-15 | 昆明理工大学 | Method and device for preparing ultrahigh-sensitivity natural rubber nano composite sensing material |
| CN114147214A (en) * | 2021-11-29 | 2022-03-08 | 西安理工大学 | Preparation method of carbon nano tube reinforced magnesium-based composite material |
| CN114147214B (en) * | 2021-11-29 | 2023-08-11 | 西安理工大学 | Preparation method of carbon nano tube reinforced magnesium-based composite material |
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Application publication date: 20160921 |