CN105801892B - A kind of preparation method of LLDPE conductive films - Google Patents
A kind of preparation method of LLDPE conductive films Download PDFInfo
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- CN105801892B CN105801892B CN201510679331.7A CN201510679331A CN105801892B CN 105801892 B CN105801892 B CN 105801892B CN 201510679331 A CN201510679331 A CN 201510679331A CN 105801892 B CN105801892 B CN 105801892B
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Abstract
The invention discloses a kind of preparation method of LLDPE conductive films, and LLDPE pellets are put into hot pressing in vacuum press and obtain LLDPE films；LLDPE films are placed in 8 ~ 15min of swelling in xylene solvent；MWCNTs is scattered in ultrasonic vibration obtained solution A in xylene solvent；LLDPE films after swelling are placed in solution A after ultrasonic vibration and are taken out, washing, naturally dry；10 ~ 15min of hot pressing under conditions of 140 ~ 150 DEG C, 1 ~ 2MPa is put in vacuum press again, obtains LLDPE conductive films.Carbon nanotubes is equably modified to the film surface in swelling using the method that ultrasonic wave disperses, one layer of conductive network structure is formed in film surface, it not only effectively prevent the reunion of carbon nanotubes, it has been significantly reduced the excess effusion value of conductive material, technique is simple, and obtained conductive film has higher force performance and compared with low excess effusion value at the same time.
Description
Technical field
The invention belongs to field of high polymer material processing, and in particular to one kind has higher force performance and compared with low excess effusion value
The simple preparation method of LLDPE conductive films.
Background technology
Carbon nanotubes has high-modulus, high intensity, low-density, good conduction and heat conductivility, and it is poly- to have become preparation
A kind of highly desirable filler of compound composite material.In conductive material field, carbon nanotubes is because of its good electric conductivity and high
Specific surface area be used to prepare the relatively low conducing composite material of excess effusion value.Usually adopted however, prepared by conducting polymer composite material
It is not only cumbersome with the method for blending, and carbon nanotubes is easy to reunite in blending, and the serious high-performance that restricts is led
The preparation and application of composite.
The content of the invention
For problems of the prior art, the present invention provides a kind of with higher force performance and compared with low excess effusion value
LLDPE（Linear low density polyethylene）The preparation method of conductive film, the preparation process is simple, and equipment requirement is low, prepared
LLDPE conductive films have higher mechanical property and relatively low excess effusion value.
In order to solve the above technical problems, the present invention uses following technical scheme：A kind of preparation side of LLDPE conductive films
Method, step are as follows：
（1）Hot pressing：LLDPE pellets are put into hot pressing in vacuum press and obtain LLDPE films；
（2）Swelling：LLDPE films are placed in 8 ~ 15 min of swelling in xylene solvent；Meanwhile by MWCNTs（Multi wall carbon
Nanotube）It is scattered in the solution A that various concentrations are made in ultrasonic vibration in xylene solvent；
（3）Ultrasonic vibration：LLDPE films after swelling are placed in ultrasonic vibration 20 ~ 30 in the solution A of various concentrations
min；
（4）Washing：By step（3）In LLDPE films take out, washed with absolute ethyl alcohol, naturally dry；
（5）Secondary hot pressing：LLDPE films after drying are put in vacuum press in 140 ~ 150 DEG C, 1 ~ 2 MPa again
Under conditions of 10 ~ 15 min of hot pressing, obtain the LLDPE conductive films with higher force performance and low excess effusion value.
The step（1）In hot pressing be by the pellet of LLDPE be put in vacuum press 150 ~ 170 DEG C, 4.5 ~ 5.5
8 ~ 15 min of hot pressing under conditions of MPa, obtains the LLDPE films that thickness is 0.2 mm.
The step（2）Middle LLDPE films are placed in xylene solvent is swollen, and wherein the temperature of xylene solvent is 60
~75 oC。
The concentration of the solution A is respectively 1,0.5,0.25,0.1,0.05 and 0.025 mg/ml.
The step（2）The time of sonic oscillations of the middle MWCNTs in xylene solvent is 10 ~ 20 min.
Beneficial effects of the present invention：（1）The preparation method of LLDPE conductive films provided by the invention, it is main using ultrasound
The method that wavelength-division dissipates uniformly modifies carbon nanotubes on LLDPE film surface, compared with the method for tradition blending, not only technique letter
Single, equipment requirement is low, and avoids the agglomeration of carbon nanotubes in the blending process.（2）It is in the invention that electric conductivity is excellent
It is different carbon nano tube modified in film surface, LLDPE conductive films are prepared by forming one layer of conductive network structure in film surface, are led
Conductive film has relatively low excess effusion value.（3）The preparation of the conducting polymer film of document report often with the reduction of mechanical property,
Especially elongation at break.And there is preferable mechanical property using LLDPE conductive films prepared by the present invention.Main cause has
Two aspects：On the one hand, the method that ultrasonic wave disperses is conducive to uniform modification of the carbon nanotubes in polymeric film surface, using super
Carbon nanotubes is equably modified the film surface in swelling by the method that sound wave disperses, and one layer of conductive network knot is formed in film surface
Structure, effectively prevent the reunion of carbon nanotubes.On the other hand, the carbon nanotubes of film surface is depressed into matrix by the method for hot pressing
Portion, a network structure is internally formed in polymer film, and induced polymer matrix crystallizes, and promotes carbon nanotubes and polymer matrix
The interface cohesion effect of body, so that the mechanical property of conductive composite film is improved.Compared with prior art, not only technique
Simply, and it can obtain a kind of while there is higher force performance and the conductive film compared with low excess effusion value.
Figure of description
Fig. 1 is the electric performance test curve for the LLDPE conductive films that embodiment 1 is prepared.
Fig. 2 is the Mechanics Performance Testing curve for the LLDPE conductive films that embodiment 1 is prepared.
Embodiment
With reference to specific embodiment, the present invention is further explained.
Embodiment 1
The preparation method of the LLDPE conductive films of the present embodiment, step are as follows：
The pellet of LLDPE is put in vacuum press 10 min of hot pressing under the conditions of 150 DEG C and 5 MPa, obtaining thickness is
The LLDPE films of 0.2 mm；Above-mentioned LLDPE film is placed in 60 DEG C of xylene solvent and is swollen 10 min；Meanwhile weigh one
The MWCNTs for determining quality is scattered in 10 min of ultrasonic vibration in the xylene solvent of 40 ml, and configuration MWCNTs concentration is respectively
The solution of 1,0.5,0.25,0.1,0.05 and 0.025 mg/ml；LLDPE films after swelling are respectively placed in above-mentioned carbon nanometer
20 min of ultrasonic oscillation in the xylene solution of pipe；Take out LLDPE films, washed with absolute ethyl alcohol, after naturally dry again
10 min of hot pressing can obtain having higher force performance and compared with low excess effusion value at 150 DEG C of temperature and 2 MPa pressure
LLDPE conductive films.
The electric performance tests of the LLDPE conductive films that the present embodiment is prepared as shown in Figure 1, as seen from Figure 1, with
The concentration increase of MWCNTs, the resistivity of LLDPE film significantly reduces, when the concentration of MWCNTs is only 0.1 mg/ml, LLDPE
The resistivity of conducting film reduces up to 8 orders of magnitude compared with pure LLDPE film.When the concentration of MWCNTs increases to 0.25 mg/
During ml, the resistivity of LLDPE conducting films tends towards stability, and LLDPE film electric conductivity is preferable at this time.Analyzed based on TG, LLDPE is conductive
The excess effusion value of film is only 0.1 %.Compared with result reported in the literature, the excess effusion value of LLDPE conducting films significantly drops in the present invention
It is low.
The Mechanics Performance Testing curve for the LLDPE conductive films that the present embodiment is prepared is as shown in Figure 2.As shown in Figure 2,
The tensile strength of LLDPE conductive films obtains larger raising compared with pure LLDPE films, wherein, the concentration of MWCNTs is only 0.1
During mg/ml, tensile strength improves 22%.Meanwhile the elongation at break of LLDPE conductive films slightly improves.With being reported in document
The mechanical property result of conductive film compare, the advantage of the invention is that elongation at break does not reduce, while tensile strength
Obtain larger raising.
Embodiment 2
The preparation method of the LLDPE conductive films of the present embodiment, step are as follows：
The pellet of LLDPE is put in vacuum press 10 min of hot pressing at 170 DEG C of temperature and 5 MPa pressure, obtains thickness
Spend the LLDPE films for 0.2 mm；LLDPE film is placed in 60 DEG C of xylene solvent and is swollen 10 min；Meanwhile weigh one
The MWCNTs for determining quality is scattered in 10 min of ultrasonic vibration in the xylene solvent of 40 ml, and configuration MWCNTs concentration is respectively
The solution of 1,0.5,0.25,0.1,0.05 and 0.025 mg/ml；LLDPE films after swelling are respectively placed in above-mentioned carbon nanometer
20 min of ultrasonic oscillation in the xylene solution of pipe；Take out LLDPE films, washed with absolute ethyl alcohol, after naturally dry again
10 min of hot pressing can obtain having the LLDPE of higher force performance and low excess effusion value conductions under the conditions of 150 DEG C and 2 MPa
Film.
Embodiment 3
The preparation method of the LLDPE conductive films of the present embodiment, step are as follows：
The pellet of LLDPE is put in vacuum press 10 min of hot pressing at 150 DEG C of temperature and 5 MPa pressure, obtains thickness
Spend the LLDPE films for 0.2 mm；LLDPE film is placed in 70 DEG C of xylene solvent and is swollen 10 min；Meanwhile weigh one
The MWCNTs for determining quality is scattered in 10 min of ultrasonic vibration in the xylene solvent of 40 ml, and configuration MWCNTs concentration is respectively
The solution of 1,0.5,0.25,0.1,0.05 and 0.025 mg/ml；LLDPE films after swelling are respectively placed in above-mentioned carbon nanometer
20 min of ultrasonic oscillation in the xylene solution of pipe；Take out LLDPE films, washed with absolute ethyl alcohol, after naturally dry again
10 min of hot pressing can obtain having the LLDPE of higher force performance and low excess effusion value conductions under the conditions of 150 DEG C and 2 MPa
Film.
Embodiment 4
The preparation method of the LLDPE conductive films of the present embodiment, step are as follows：
The pellet of LLDPE is put in vacuum press 10 min of hot pressing under the conditions of 150 DEG C and 5 MPa, obtaining thickness is
The LLDPE films of 0.2 mm；LLDPE film is placed in 60 DEG C of xylene solvent and is swollen 15 min；Meanwhile weigh certain matter
The MWCNTs of amount is scattered in 10 min of ultrasonic vibration in the xylene solvent of 40 ml, and configuration MWCNTs concentration is respectively 1,
The solution of 0.5,0.25,0.1,0.05 and 0.025 mg/ml；LLDPE films after swelling are respectively placed in above-mentioned carbon nanotubes
Xylene solution in 20 min of ultrasonic oscillation；Take out LLDPE films, washed with absolute ethyl alcohol, after naturally dry again in
10 min of hot pressing is the LLDPE conductive thins that can obtain having higher force performance and low excess effusion value under the conditions of 150 DEG C and 2 MPa
Film.
Embodiment 5
The preparation method of the LLDPE conductive films of the present embodiment, step are as follows：
The pellet of LLDPE is put in vacuum press 10 min of hot pressing under the conditions of 150 DEG C and 5 MPa, obtaining thickness is
The LLDPE films of 0.2 mm；LLDPE films are placed in 60 DEG C of xylene solvent and are swollen 10 min；Meanwhile weigh certain
The MWCNTs of quality is scattered in 10 min of ultrasonic vibration in the xylene solvent of 40 ml, and configuration MWCNTs concentration is respectively 1,
The solution of 0.5,0.25,0.1,0.05 and 0.025 mg/ml；LLDPE films after swelling are respectively placed in above-mentioned carbon nanotubes
Xylene solution in 30 min of ultrasonic oscillation；Take out LLDPE films, washed with absolute ethyl alcohol, after naturally dry again in
10 min of hot pressing is the LLDPE conductive thins that can obtain having higher force performance and low excess effusion value under the conditions of 150 DEG C and 1 MPa
Film.
Embodiment 6
The preparation method of the LLDPE conductive films of the present embodiment, step are as follows：
（1）Hot pressing：The pellet of LLDPE is put in vacuum press 8 min of hot pressing under 150 DEG C, the pressure of 5.5 MPa,
Obtain the LLDPE films that thickness is 0.2 mm；
（2）Swelling：LLDPE films are placed in xylene solvent（65oC）8 min of middle swelling；Meanwhile MWCNTs is disperseed
The 20 min obtained solution A of ultrasonic vibration in xylene solvent, concentration is respectively 1,0.5,0.25,0.1,0.05 and 0.025
mg/ml；
（3）Ultrasonic vibration：LLDPE films after swelling are placed in ultrasonic vibration 20 in the solution A of above-mentioned various concentrations
min；
（4）Washing：By step（3）In LLDPE films take out, washed with absolute ethyl alcohol, naturally dry；
（5）Secondary hot pressing：LLDPE films after drying are put in vacuum press in 140 DEG C, the condition of 2 MPa again
Lower 10 min of hot pressing, obtains the LLDPE conductive films with higher force performance and low excess effusion value.
Embodiment 7
The preparation method of the LLDPE conductive films of the present embodiment, step are as follows：
（1）Hot pressing：The pellet of LLDPE is put in vacuum press the hot pressing 15 under 170 DEG C, the pressure of 4.5 MPa
Min, obtains the LLDPE films that thickness is 0.2 mm；
（2）Swelling：LLDPE films are placed in xylene solvent（70oC）Middle swelling 15min；Meanwhile MWCNTs is disperseed
The 10 min obtained solution A of ultrasonic vibration in xylene solvent, concentration is respectively 1,0.5,0.25,0.1,0.05 and 0.025
mg/ml；
（3）Ultrasonic vibration：LLDPE films after swelling are placed in ultrasonic vibration 30 in the solution A of above-mentioned various concentrations
min；
（4）Washing：By step（3）In LLDPE films take out, washed with absolute ethyl alcohol, naturally dry；
（5）Secondary hot pressing：LLDPE films after drying are put in vacuum press in 150 DEG C, the condition of 1 MPa again
Lower 15 min of hot pressing, obtains the LLDPE conductive films with higher force performance and low excess effusion value.
Embodiment 8
The preparation method of the LLDPE conductive films of the present embodiment, step are as follows：
（1）Hot pressing：The pellet of LLDPE is put in vacuum press 10 min of hot pressing under conditions of 160 DEG C, 5 MPa,
Obtain the LLDPE films that thickness is 0.2 mm；
（2）Swelling：LLDPE films are placed in xylene solvent（75oC）12 min of middle swelling；Meanwhile by MWCNTs points
The 15 min obtained solution A of ultrasonic vibration in xylene solvent are dissipated, concentration is respectively 1,0.5,0.25,0.1,0.05 and 0.025
mg/ml；
（3）Ultrasonic vibration：LLDPE films after swelling are placed in ultrasonic vibration 25 in the solution A of above-mentioned various concentrations
min；
（4）Washing：By step（3）In LLDPE films take out, washed with absolute ethyl alcohol, naturally dry；
（5）Secondary hot pressing：LLDPE films after drying are put in vacuum press in 145 DEG C, the bar of 1.5 MPa again
12 min of hot pressing under part, obtains the LLDPE conductive films with higher force performance and low excess effusion value.
The basic principle and main feature and advantages of the present invention of the present invention has been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (5)
1. a kind of preparation method of LLDPE conductive films, it is characterised in that step is as follows：
（1）Hot pressing：LLDPE pellets are put into hot pressing in vacuum press and obtain LLDPE films；
（2）Swelling：LLDPE films are placed in 8 ~ 15 min of swelling in xylene solvent；Meanwhile MWCNTs is scattered in diformazan
The solution A of various concentrations is made in ultrasonic vibration in benzene solvent；
（3）Ultrasonic vibration：LLDPE films after swelling are respectively placed in ultrasonic vibration 20 ~ 30 in the solution A of various concentrations
min；
（4）Washing：By step（3）In LLDPE films take out, washed with absolute ethyl alcohol, naturally dry；
（5）Secondary hot pressing：LLDPE films after drying are put in vacuum press in 140 ~ 150 DEG C, the bar of 1 ~ 2 MPa again
10 ~ 15 min of hot pressing under part, obtains the LLDPE conductive films with higher force performance and low excess effusion value.
2. the preparation method of LLDPE conductive films according to claim 1, it is characterised in that：The step（1）In heat
Pressure is that the pellet of LLDPE is put in vacuum press 8 ~ 15 min of hot pressing under conditions of 150 ~ 170 DEG C, 4.5 ~ 5.5 MPa,
Obtain the LLDPE films that thickness is 0.2 mm.
3. the preparation method of LLDPE conductive films according to claim 1, it is characterised in that：The step（2）It is middle to incite somebody to action
LLDPE films, which are placed in xylene solvent, to be swollen, and wherein the temperature of xylene solvent is 60 ~ 75oC。
4. the preparation method of LLDPE conductive films according to claim 1, it is characterised in that：The concentration of the solution A point
Wei not 1,0.5,0.25,0.1,0.05 and 0.025 mg/ml.
5. the preparation method of LLDPE conductive films according to claim 1, it is characterised in that：The step（2）In
The time of sonic oscillations of the MWCNTs in xylene solvent is 10 ~ 20 min.
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| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570609A (en) * | 2008-04-28 | 2009-11-04 | 黑龙江大学 | Method for preparing nano composite material |
| CN102785437A (en) * | 2012-07-19 | 2012-11-21 | 中国航空工业集团公司北京航空材料研究院 | Composite conductive film, its preparation method and its application |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101570609A (en) * | 2008-04-28 | 2009-11-04 | 黑龙江大学 | Method for preparing nano composite material |
| CN102785437A (en) * | 2012-07-19 | 2012-11-21 | 中国航空工业集团公司北京航空材料研究院 | Composite conductive film, its preparation method and its application |
Non-Patent Citations (1)
| Title |
|---|
| "Single Wall Carbon Nanotube/Polyethylene Nanocomposites: Nucleating and Templating Polyethylene Crystallites";Reto Haggenmueller et al.;《Macromolecules》;20061003;第39卷;第2964-2971页 * |
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