CN105801892A - Method for preparing LLDPE (Linear Low-Density Polyethylene) conductive film - Google Patents

Method for preparing LLDPE (Linear Low-Density Polyethylene) conductive film Download PDF

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CN105801892A
CN105801892A CN201510679331.7A CN201510679331A CN105801892A CN 105801892 A CN105801892 A CN 105801892A CN 201510679331 A CN201510679331 A CN 201510679331A CN 105801892 A CN105801892 A CN 105801892A
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lldpe
film
conductive film
hot pressing
thin film
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CN105801892B (en
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石素宇
王延伟
辛长征
许文仲
郑国强
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Foshan Shunde haijinna new material industry Co.,Ltd.
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Henan Institute of Engineering
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Abstract

The invention discloses a method for preparing an LLDPE (Linear Low-Density Polyethylene) conductive film. The method comprises the steps: carrying out hot pressing on LLDPE granules in a suction press, so as to obtain an LLDPE film; swelling the LLDPE film in a xylene solvent for 8 to 15 minutes; dispersing MWCNTs in the xylene solvent, and carrying out ultrasonic oscillation so as to prepare solutions A; putting the swelled LLDPE film into the solutions A, carrying out ultrasonic oscillation, then, taking out the swelled LLDPE film, and carrying out washing and natural airing; and carrying out hot pressing on the LLDPE film for 10 to 15 minutes in the suction press again at the temperature of 140 to 150 DEG C and the pressure of 1MPa to 2MPa, thereby obtaining the LLDPE conductive film. According to the method, the surface of the swelled film is uniformly modified with carbon nanotubes by using an ultrasonic dispersion method, and a layer of conductive network structure is formed on the surface of the film, so that the agglomeration of the carbon nanotubes is effectively avoided, and the percolation threshold of a conductive material is remarkably reduced; and the process is simple, and the prepared conductive film simultaneously has relatively high mechanical properties and a relatively low percolation threshold.

Description

A kind of preparation method of LLDPE conductive film
Technical field
The invention belongs to field of high polymer material processing, be specifically related to a kind of simple preparation method with higher force performance and relatively low excess effusion value LLDPE conductive film.
Background technology
CNT has high-modulus, high intensity, low-density, good conduction and heat conductivility, has become as and prepares a kind of filler that polymer composites is highly desirable.In conductive material field, CNT is used to prepare the conducing composite material that excess effusion value is relatively low because of its good electric conductivity and high specific surface area.But, conducting polymer composite material preparation usually adopts blended method, not only complex operation, and CNT is easy to reunite when blended, seriously restricts preparation and the application of high-performance conductive composite.
Summary of the invention
For problems of the prior art, the present invention provides a kind of LLDPE(linear low density polyethylene with higher force performance and relatively low excess effusion value) preparation method of conductive film, this preparation technology is simple, equipment requirements is low, and prepared LLDPE conductive film has higher mechanical property and relatively low excess effusion value.
For solving above-mentioned technical problem, the present invention by the following technical solutions: the preparation method of a kind of LLDPE conductive film, step is as follows:
(1) hot pressing: LLDPE pellet is put into hot pressing in vacuum press and obtains LLDPE thin film;
(2) swelling: to be placed in xylene solvent by LLDPE thin film swelling 8 ~ 15min;Meanwhile, by MWCNTs(multi-walled carbon nano-tubes) it is scattered in xylene solvent ultrasonic vibration and prepares the solution A of variable concentrations;
(3) ultrasonic vibration: be placed in the solution A of variable concentrations by the LLDPE thin film after swelling ultrasonic vibration 20 ~ 30min;
(4) washing: the LLDPE thin film in step (3) is taken out, with absolute ethanol washing, naturally dries;
(5) secondary hot pressing: the LLDPE thin film after drying is put in vacuum press again 140 ~ 150 DEG C, 1 ~ 2MPa when hot pressing 10 ~ 15min, obtain the LLDPE conductive film with higher force performance and low excess effusion value.
Hot pressing in described step (1) be the pellet of LLDPE is put in vacuum press 150 ~ 170 DEG C, 4.5 ~ 5.5MPa when hot pressing 8 ~ 15min, obtain the LLDPE thin film that thickness is 0.2mm.
Being placed in xylene solvent by LLDPE thin film in described step (2) swelling, wherein the temperature of xylene solvent is 60 ~ 75oC。
The concentration of described solution A respectively 1,0.5,0.25,0.1,0.05 and 0.025mg/ml.
In described step (2), the time of MWCNTs sonic oscillation in xylene solvent is 10 ~ 20min.
Beneficial effects of the present invention: the preparation method of (1) LLDPE conductive film provided by the invention, CNT is uniformly modified at LLDPE film surface by the main employing scattered method of ultrasound wave, compared with the method that tradition is blended, not only technique is simple, equipment requirements is low, and avoids CNT agglomeration in Blending Processes.(2) by excellent for electric conductivity carbon nano tube modified on film surface in this invention, preparing LLDPE conductive film by forming one layer of conductive network structure on film surface, conductive film has relatively low excess effusion value.(3) preparation of the conducting polymer film of bibliographical information is often with the reduction of mechanical property, especially elongation at break.And adopt LLDPE conductive film prepared by the present invention to have good mechanical property.Main cause has two aspects: on the one hand, the scattered method of ultrasound wave is conducive to CNT in the uniform modification of polymeric film surface, utilize ultrasound wave scattered method that CNT is modified at swelling film surface equably, form one layer of conductive network structure on film surface, effectively prevent the reunion of CNT.On the other hand, the CNT on film surface is depressed into intrinsic silicon by the method for hot pressing, is internally formed a network structure induced polymer matrix crystallization at polymeric film, promote the interface cohesion effect of CNT and polymeric matrix, so that the mechanical property of conductive composite film is improved.Compared with prior art, not only technique is simple, and can obtain a kind of conductive film with higher force performance and relatively low excess effusion value.
Figure of description
Fig. 1 is the electric performance test curve of the LLDPE conductive film that embodiment 1 prepares.
Fig. 2 is the Mechanics Performance Testing curve of the LLDPE conductive film that embodiment 1 prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.
Embodiment 1
The preparation method of the LLDPE conductive film of the present embodiment, step is as follows:
The pellet of LLDPE is put in vacuum press in 150 DEG C and hot pressing 10min when 5MPa, obtains the LLDPE thin film that thickness is 0.2mm;It is placed in the xylene solvent of 60 DEG C by above-mentioned LLDPE film swelling 10min;Meanwhile, weigh the MWCNTs of certain mass and be scattered in the xylene solvent of 40ml ultrasonic vibration 10min, configuration MWCNTs concentration respectively 1,0.5,0.25,0.1,0.05 and the solution of 0.025mg/ml;It is respectively placed in the xylene solution of above-mentioned CNT by the LLDPE thin film after swelling ultrasonic wave concussion 20min;Take out LLDPE thin film, with absolute ethanol washing, naturally dry after again at 150 DEG C of temperature and 2MPa pressure hot pressing 10min can obtain having the LLDPE conductive film of higher force performance and relatively low excess effusion value.
The electric performance test of the LLDPE conductive film that the present embodiment prepares is as shown in Figure 1, as seen from Figure 1, increase with the concentration of MWCNTs, the resistivity of LLDPE film significantly reduces, when the concentration of MWCNTs is only 0.1mg/ml, the resistivity of LLDPE conducting film reduces up to 8 orders of magnitude compared with pure LLDPE film.When the concentration of MWCNTs increases to 0.25mg/ml, the resistivity of LLDPE conducting film tends towards stability, and now LLDPE film electric conductivity is better.Analyzing based on TG, the excess effusion value of LLDPE conducting film is only 0.1%.Compared with the result of report in document, in the present invention, the excess effusion value of LLDPE conducting film significantly reduces.
The Mechanics Performance Testing curve of the LLDPE conductive film that the present embodiment prepares is as shown in Figure 2.As shown in Figure 2, the hot strength of LLDPE conductive film obtains bigger raising compared with pure LLDPE thin film, and wherein, when the concentration of MWCNTs is only 0.1mg/ml, hot strength improves 22%.Meanwhile, the elongation at break of LLDPE conductive film slightly improves.Compared with the mechanical property result of the conductive film of report in document, it is an advantage of the current invention that elongation at break does not reduce, hot strength obtains bigger raising simultaneously.
Embodiment 2
The preparation method of the LLDPE conductive film of the present embodiment, step is as follows:
It is put in vacuum press by the pellet of LLDPE at 170 DEG C of temperature and 5MPa pressure hot pressing 10min, obtains the LLDPE thin film that thickness is 0.2mm;LLDPE film is placed in the xylene solvent of 60 DEG C swelling 10min;Meanwhile, weigh the MWCNTs of certain mass and be scattered in the xylene solvent of 40ml ultrasonic vibration 10min, configuration MWCNTs concentration respectively 1,0.5,0.25,0.1,0.05 and the solution of 0.025mg/ml;It is respectively placed in the xylene solution of above-mentioned CNT by the LLDPE thin film after swelling ultrasonic wave concussion 20min;Take out LLDPE thin film, with absolute ethanol washing, naturally dry after again in 150 DEG C and 2MPa when hot pressing 10min can obtain the LLDPE conductive film with higher force performance and low excess effusion value.
Embodiment 3
The preparation method of the LLDPE conductive film of the present embodiment, step is as follows:
It is put in vacuum press by the pellet of LLDPE at 150 DEG C of temperature and 5MPa pressure hot pressing 10min, obtains the LLDPE thin film that thickness is 0.2mm;LLDPE film is placed in the xylene solvent of 70 DEG C swelling 10min;Meanwhile, weigh the MWCNTs of certain mass and be scattered in the xylene solvent of 40ml ultrasonic vibration 10min, configuration MWCNTs concentration respectively 1,0.5,0.25,0.1,0.05 and the solution of 0.025mg/ml;It is respectively placed in the xylene solution of above-mentioned CNT by the LLDPE thin film after swelling ultrasonic wave concussion 20min;Take out LLDPE thin film, with absolute ethanol washing, naturally dry after again in 150 DEG C and 2MPa when hot pressing 10min can obtain the LLDPE conductive film with higher force performance and low excess effusion value.
Embodiment 4
The preparation method of the LLDPE conductive film of the present embodiment, step is as follows:
The pellet of LLDPE is put in vacuum press in 150 DEG C and hot pressing 10min when 5MPa, obtains the LLDPE thin film that thickness is 0.2mm;LLDPE film is placed in the xylene solvent of 60 DEG C swelling 15min;Meanwhile, weigh the MWCNTs of certain mass and be scattered in the xylene solvent of 40ml ultrasonic vibration 10min, configuration MWCNTs concentration respectively 1,0.5,0.25,0.1,0.05 and the solution of 0.025mg/ml;It is respectively placed in the xylene solution of above-mentioned CNT by the LLDPE thin film after swelling ultrasonic wave concussion 20min;Take out LLDPE thin film, with absolute ethanol washing, naturally dry after again in 150 DEG C and 2MPa when hot pressing 10min can obtain the LLDPE conductive film with higher force performance and low excess effusion value.
Embodiment 5
The preparation method of the LLDPE conductive film of the present embodiment, step is as follows:
The pellet of LLDPE is put in vacuum press in 150 DEG C and hot pressing 10min when 5MPa, obtains the LLDPE thin film that thickness is 0.2mm;It is placed in the xylene solvent of 60 DEG C by LLDPE thin film swelling 10min;Meanwhile, weigh the MWCNTs of certain mass and be scattered in the xylene solvent of 40ml ultrasonic vibration 10min, configuration MWCNTs concentration respectively 1,0.5,0.25,0.1,0.05 and the solution of 0.025mg/ml;It is respectively placed in the xylene solution of above-mentioned CNT by the LLDPE thin film after swelling ultrasonic wave concussion 30min;Take out LLDPE thin film, with absolute ethanol washing, naturally dry after again in 150 DEG C and 1MPa when hot pressing 10min can obtain the LLDPE conductive film with higher force performance and low excess effusion value.
Embodiment 6
The preparation method of the LLDPE conductive film of the present embodiment, step is as follows:
(1) hot pressing: the pellet of LLDPE is put in vacuum press at 150 DEG C, hot pressing 8min under the pressure of 5.5MPa, obtains the LLDPE thin film that thickness is 0.2mm;
(2) swelling: LLDPE thin film is placed in xylene solvent (65oC) swelling 8min in;Meanwhile, it is scattered in xylene solvent by MWCNTs ultrasonic vibration 20min obtained solution A, concentration respectively 1,0.5,0.25,0.1,0.05 and 0.025mg/ml;
(3) ultrasonic vibration: be placed in the solution A of above-mentioned variable concentrations by the LLDPE thin film after swelling ultrasonic vibration 20min;
(4) washing: the LLDPE thin film in step (3) is taken out, with absolute ethanol washing, naturally dries;
(5) secondary hot pressing: the LLDPE thin film after drying is put in vacuum press again 140 DEG C, 2MPa when hot pressing 10min, obtain the LLDPE conductive film with higher force performance and low excess effusion value.
Embodiment 7
The preparation method of the LLDPE conductive film of the present embodiment, step is as follows:
(1) hot pressing: the pellet of LLDPE is put in vacuum press at 170 DEG C, hot pressing 15min under the pressure of 4.5MPa, obtains the LLDPE thin film that thickness is 0.2mm;
(2) swelling: LLDPE thin film is placed in xylene solvent (70oC) swelling 15min in;Meanwhile, it is scattered in xylene solvent by MWCNTs ultrasonic vibration 10min obtained solution A, concentration respectively 1,0.5,0.25,0.1,0.05 and 0.025mg/ml;
(3) ultrasonic vibration: be placed in the solution A of above-mentioned variable concentrations by the LLDPE thin film after swelling ultrasonic vibration 30min;
(4) washing: the LLDPE thin film in step (3) is taken out, with absolute ethanol washing, naturally dries;
(5) secondary hot pressing: the LLDPE thin film after drying is put in vacuum press again 150 DEG C, 1MPa when hot pressing 15min, obtain the LLDPE conductive film with higher force performance and low excess effusion value.
Embodiment 8
The preparation method of the LLDPE conductive film of the present embodiment, step is as follows:
(1) hot pressing: the pellet of LLDPE is put in vacuum press 160 DEG C, 5MPa when hot pressing 10min, obtain the LLDPE thin film that thickness is 0.2mm;
(2) swelling: LLDPE thin film is placed in xylene solvent (75oC) swelling 12min in;Meanwhile, it is scattered in xylene solvent by MWCNTs ultrasonic vibration 15min obtained solution A, concentration respectively 1,0.5,0.25,0.1,0.05 and 0.025mg/ml;
(3) ultrasonic vibration: be placed in the solution A of above-mentioned variable concentrations by the LLDPE thin film after swelling ultrasonic vibration 25min;
(4) washing: the LLDPE thin film in step (3) is taken out, with absolute ethanol washing, naturally dries;
(5) secondary hot pressing: the LLDPE thin film after drying is put in vacuum press again 145 DEG C, 1.5MPa when hot pressing 12min, obtain the LLDPE conductive film with higher force performance and low excess effusion value.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; described in above-described embodiment and description is that principles of the invention is described; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within the claimed scope of the invention.Claimed scope is defined by appending claims and equivalent thereof.

Claims (5)

1. the preparation method of a LLDPE conductive film, it is characterised in that step is as follows:
(1) hot pressing: LLDPE pellet is put into hot pressing in vacuum press and obtains LLDPE thin film;
(2) swelling: to be placed in xylene solvent by LLDPE thin film swelling 8 ~ 15min;Meanwhile, it is scattered in xylene solvent by MWCNTs ultrasonic vibration and prepares the solution A of variable concentrations;
(3) ultrasonic vibration: be respectively placed in the solution A of variable concentrations by the LLDPE thin film after swelling ultrasonic vibration 20 ~ 30min;
(4) washing: the LLDPE thin film in step (3) is taken out, with absolute ethanol washing, naturally dries;
(5) secondary hot pressing: the LLDPE thin film after drying is put in vacuum press again 140 ~ 150 DEG C, 1 ~ 2MPa when hot pressing 10 ~ 15min, obtain the LLDPE conductive film with higher force performance and low excess effusion value.
2. the preparation method of LLDPE conductive film according to claim 1, it is characterized in that: the hot pressing in described step (1) be the pellet of LLDPE is put in vacuum press 150 ~ 170 DEG C, 4.5 ~ 5.5MPa when hot pressing 8 ~ 15min, obtain the LLDPE thin film that thickness is 0.2mm.
3. the preparation method of LLDPE conductive film according to claim 1, it is characterised in that: being placed in xylene solvent by LLDPE thin film in described step (2) swelling, wherein the temperature of xylene solvent is 60 ~ 75oC。
4. the preparation method of LLDPE conductive film according to claim 1, it is characterised in that: the concentration of described solution A respectively 1,0.5,0.25,0.1,0.05 and 0.025mg/ml.
5. the preparation method with better mechanical property and low excess effusion value LLDPE conductive film according to claim 1, it is characterised in that: in described step (2), the time of MWCNTs sonic oscillation in xylene solvent is 10 ~ 20min.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106479047A (en) * 2016-09-30 2017-03-08 河南工程学院 A kind of preparation method of low excess effusion value strong mechanical performance polypropylene conductive thin film
CN109535463A (en) * 2018-10-31 2019-03-29 河南工程学院 A kind of preparation method of TPU conductive film

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106479047A (en) * 2016-09-30 2017-03-08 河南工程学院 A kind of preparation method of low excess effusion value strong mechanical performance polypropylene conductive thin film
CN106479047B (en) * 2016-09-30 2018-08-28 河南工程学院 A kind of preparation method of low excess effusion value strong mechanical performance polypropylene conductive film
CN109535463A (en) * 2018-10-31 2019-03-29 河南工程学院 A kind of preparation method of TPU conductive film

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