CN115010964A - Preparation method of conductive silicone rubber composite material - Google Patents

Preparation method of conductive silicone rubber composite material Download PDF

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Publication number
CN115010964A
CN115010964A CN202210795691.3A CN202210795691A CN115010964A CN 115010964 A CN115010964 A CN 115010964A CN 202210795691 A CN202210795691 A CN 202210795691A CN 115010964 A CN115010964 A CN 115010964A
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silicone rubber
mixture
composite material
rubber composite
conductive silicone
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梅顺齐
王建
刘腾
丁俊武
白元钎
陈振
郑权
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Wuhan Textile University
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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
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
    • C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
    • C08J3/215—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase at least one additive being also premixed with a liquid phase
    • 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
    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes
    • 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
    • C08K2201/001—Conductive additives
    • 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
    • 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
    • C08K3/041—Carbon nanotubes
    • 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
    • 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
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/06—Elements
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

A preparation method of a conductive silicone rubber composite material comprises the steps of firstly uniformly mixing a conductive filler and n-heptane to obtain a mixture A, wherein the conductive filler is a mixture of graphene, carbon nano tubes and a carbon fiber material, then uniformly mixing liquid silicone rubber and n-heptane to obtain a mixture B, then uniformly mixing the mixture A and the mixture B according to a required proportion, wherein the mass ratio of the mixture A to the mixture B is 1:1-1.5, then sequentially carrying out vacuum pumping treatment, pouring and standing until the n-heptane is completely volatilized, and curing to obtain the conductive silicone rubber composite material, wherein the content of the graphene, the content of the carbon nano tubes and the content of the carbon fibers in the conductive silicone rubber composite material are 4.5-5.5wt%, 1-1.25wt% and 6-7.5 wt%. The conductive silicone rubber composite material prepared by the method has high conductivity and high tensile strength.

Description

Preparation method of conductive silicone rubber composite material
Technical Field
The invention belongs to the technical field of rubber materials, and particularly relates to a preparation method of a conductive silicone rubber composite material, which is suitable for simultaneously improving the conductivity and the tensile strength of the silicone rubber composite material.
Background
As a novel functional material, the conductive polymer material has wide application prospect in electromagnetic shielding and antistatic materials, and the market demand is in an explosive growth trend. The silicon rubber has good high temperature resistance and low temperature resistance, excellent processing performance and mechanical property and unique chemical stability, and is usually used in severer environment. However, the common silicon rubber has poor conductivity, and the conductivity can be obviously improved by adding the conductive filler. Commonly used conductive fillers are divided into two categories: most of the conductive silicone rubbers sold in the market at present are prepared by acetylene black, but the preparation process is complex, and the mechanical properties of the conductive silicone rubber are poor.
Chinese patent: the invention of granted publication No. CN103665875A, application date 2015.11.18 discloses a method for preparing conductive silicone rubber, the method mixes acetylene black, aluminium oxide, hydroxyl silicone oil and water accounting for 1% of the weight of acetylene black, then adds the mixture into a granulator to prepare acetylene black and aluminium oxide particles, and then mixes the acetylene black and aluminium oxide particles with liquid silicone rubber, the prepared silicone rubber has the advantages of high thermal conductivity, heat resistance and low compressibility, the tensile strength is more than 9.6MPa, the tearing strength is more than 36N/mm, the volume resistivity is less than 45 omega.cm, Chinese patent: the invention of publication number CN107141809A and application date 20170518 discloses a low-resistance conductive silicone rubber, which comprises the following components in parts by weight: the low-resistance conductive silicone rubber reduces the surface resistance of the silicone rubber to about 10 omega and solves the phenomenon of easy roller adhesion, but the two silicone rubbers can not give consideration to high conductivity and high tensile strength and can not meet the actual use requirements.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of a conductive silicone rubber composite material, which can simultaneously improve the conductive performance and the tensile strength of the silicone rubber composite material.
In order to achieve the above purpose, the invention provides the following technical scheme:
a preparation method of a conductive silicone rubber composite material sequentially comprises the following steps:
s1, uniformly mixing a conductive filler and n-heptane to obtain a mixture A, wherein the conductive filler is a mixture of graphene, carbon nanotubes and a carbon fiber material;
s2, uniformly mixing the liquid silicone rubber and n-heptane to obtain a mixture B;
s3, uniformly mixing the mixture A and the mixture B according to a required proportion, then sequentially carrying out vacuum pumping treatment, pouring and standing until n-heptane is completely volatilized, and curing to obtain the conductive silicone rubber composite material, wherein the mass ratio of the mixture A to the mixture B is 1:1-1.5, the content of graphene in the conductive silicone rubber composite material is 4.5-5.5wt%, the content of carbon nanotubes is 1-1.25wt%, and the content of carbon fibers is 6-7.5 wt%.
In step S2, the volume ratio of the liquid silicone rubber to the n-heptane is 1: 2-2.5.
In step S3, the curing specifically includes: curing for 30-45min in a constant-temperature drying box at the temperature of 120-130 ℃.
The carbon fiber material is carbon black.
In step S3, the mass ratio of the mixture A to the mixture B is 1: 1.2-1.3.
In step S3, the content of graphene in the conductive silicone rubber composite material is 4.8-5.1wt%, the content of carbon nanotubes is 1.1-1.18wt%, and the content of carbon fibers is 6.5-7.2 wt%.
The volume ratio of the liquid silicone rubber to the n-heptane is 1: 2.1-2.3.
The curing specifically comprises the following steps: curing for 35-40min in a constant-temperature drying oven at 125-128 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a method for preparing conductive silicon rubber composite material, which uses liquid silicon rubber as a matrix, volatile n-heptane as a solvent, carbon fiber, carbon nano tube and graphene as conductive fillers, and utilizes a solution blending method to disperse the conductive fillers and the liquid silicon rubber in the n-heptane respectively, and then uniformly mix the conductive fillers and the liquid silicon rubber to volatilize the n-heptane, thereby finally preparing the conductive silicon rubber composite material. Can meet the actual use requirement. Therefore, the invention has high conductivity and high tensile strength.
Drawings
FIG. 1 is an XRD analysis chart of a test example in the present invention.
FIG. 2 is an XRD analysis chart of comparative examples 1 to 4 in the present invention.
FIG. 3 is a cross-sectional electron micrograph of a test example of the present invention.
Detailed Description
The present invention will be further described with reference to the following embodiments.
A preparation method of a conductive silicone rubber composite material sequentially comprises the following steps:
s1, uniformly mixing a conductive filler and n-heptane to obtain a mixture A, wherein the conductive filler is a mixture of graphene, carbon nanotubes and a carbon fiber material;
s2, uniformly mixing the liquid silicone rubber and n-heptane to obtain a mixture B;
s3, uniformly mixing the mixture A and the mixture B according to a required proportion, then sequentially carrying out vacuum pumping treatment, pouring and standing until n-heptane is completely volatilized, and curing to obtain the conductive silicone rubber composite material, wherein the mass ratio of the mixture A to the mixture B is 1:1-1.5, the content of graphene in the conductive silicone rubber composite material is 4.5-5.5wt%, the content of carbon nanotubes is 1-1.25wt%, and the content of carbon fibers is 6-7.5 wt%.
In step S2, the volume ratio of the liquid silicone rubber to the n-heptane is 1: 2-2.5.
In step S3, the curing specifically includes: curing for 30-45min in a constant-temperature drying box at the temperature of 120-130 ℃.
The carbon fiber material is carbon black.
In step S3, the mass ratio of the mixture A to the mixture B is 1: 1.2-1.3.
In step S3, the content of graphene in the conductive silicone rubber composite material is 4.8-5.1wt%, the content of carbon nanotubes is 1.1-1.18wt%, and the content of carbon fibers is 6.5-7.2 wt%.
The volume ratio of the liquid silicone rubber to the n-heptane is 1: 2.1-2.3.
The curing specifically comprises the following steps: curing for 35-40min in a constant-temperature drying oven at 125-128 ℃.
Example 1:
a preparation method of a conductive silicone rubber composite material specifically comprises the following steps:
s1, mixing conductive filler and n-heptane, then mechanically stirring for 30min, and then ultrasonically dispersing for 60min to obtain a mixture A, wherein the conductive filler is a mixture of graphene, carbon nanotubes and a carbon fiber material, and the carbon fiber material is carbon black;
s2, mixing the silicon rubber and n-heptane, then mechanically stirring for 30min, and then ultrasonically dispersing for 60min to obtain a mixture B, wherein the volume ratio of the silicon rubber to the n-heptane is 1: 2;
s3, uniformly mixing the mixture A and the mixture B according to a required proportion, then sequentially carrying out vacuum pumping treatment, pouring and standing until n-heptane is completely volatilized, and curing in a constant-temperature drying oven at 128 ℃ for 40min to obtain the conductive silicone rubber composite material, wherein the mass ratio of the mixture A to the mixture B is 1:1.2, the content of graphene in the conductive silicone rubber composite material is 4.8wt%, the content of carbon nanotubes in the conductive silicone rubber composite material is 1.1wt%, and the content of carbon fibers in the conductive silicone rubber composite material is 6.5 wt%.
Example 2:
the difference from example 1 is that:
in step S2, the volume ratio of the silicon rubber to the n-heptane is 1: 2.1;
in step S3, the curing temperature is 120 ℃ and the curing time is 30min, the mass ratio of the mixture a to the mixture B is 1:1.5, and the conductive silicone rubber composite material contains 4.5wt% of graphene, 1wt% of carbon nanotubes, and 6wt% of carbon fibers.
Example 3:
the difference from example 1 is that:
in step S2, the volume ratio of the silicon rubber to the n-heptane is 1: 2.5;
in step S3, the curing temperature is 130 ℃ and the curing time is 45min, the mass ratio of the mixture a to the mixture B is 1:1, and the conductive silicone rubber composite material contains 5.5wt% of graphene, 1.25wt% of carbon nanotubes, and 7.5wt% of carbon fibers.
And (3) performance testing:
with the conductive silicone rubber composite material obtained in example 1 as a test example, the silicone rubber composite material obtained without the conductive filler as comparative example 1, the silicone rubber composite material obtained with only Carbon Nanotubes (CNTs) as the conductive filler as comparative example 2, the silicone rubber composite material obtained with only carbon fiber material (CF) as the conductive filler as comparative example 3, and the silicone rubber composite material obtained with only graphene (G) as the conductive filler as comparative example 4 (the remaining preparation conditions of comparative examples 1 to 4 are the same as in example 1), the following tests were respectively performed:
first, dispersibility test
1. XRD analyses were performed on the test examples, which had an XRD analysis pattern shown in FIG. 1, and comparative examples 1 to 4, respectively, the XRD patterns of the comparative examples 1 to 4 are shown in fig. 2, and as can be seen from fig. 1 and 2, the presence of broad peaks at both 10 ° and 22.5 ° 2 θ in the comparative example 1, demonstrates that the pure LSR polymer behaves as a non-crystalline structure, while broad peaks were present at 10 ° and 22.5 ° in the test example at 2 θ, and the characteristic peak at 24 ° in the test example disappeared except for the above-mentioned two characteristic peaks identical to those in comparative example 1, the characteristic peak at the position of 28.2 degrees of 2 theta is obviously reduced, which proves that the conductive filler has stronger interface acting force due to the interaction of various substances in the conductive filler, so that the conductive filler is more uniformly dispersed and has smaller agglomeration phenomenon when the liquid silicon rubber solution is solidified, and meanwhile, the influence of the addition of the conductive filler on the crystallization of the liquid silicon rubber matrix is smaller;
2. the cross-sectional electron microscope image of the test example is shown in fig. 3, no significant agglomeration of graphene, carbon nanotubes or carbon fibers is observed in fig. 3, it can be seen that graphene, carbon nanotubes and carbon fibers are fully dispersed in liquid silicone rubber, and meanwhile, the liquid silicone rubber is used as a substrate to wrap the graphene, carbon nanotubes and carbon fibers, and the liquid silicone rubber has good binding property with the graphene, carbon nanotubes and carbon fibers.
Second, mechanical property test
1. The tensile strength and the elastic modulus of the strip samples of the test examples and the comparative examples 2 to 4 cut into the specification of 4cm by 5cm are detected, and the detection results are shown in table 1:
TABLE 1 tensile Strength and elastic modulus test results
Figure 393242DEST_PATH_IMAGE001
。
As can be seen from Table 1, the tensile strength and the modulus of elasticity of the test examples are superior to those of comparative examples 2 to 4, and the tensile strength is high.
Conductivity test
1. The test examples and comparative examples 2 to 4 were cut into wafer-shaped samples having a radius of 1 cm, and the volume resistivity was measured by a four-probe method, and the measurement results are shown in table 2:
TABLE 2 volume resistivity test results
Figure 517186DEST_PATH_IMAGE002
。
As can be seen from Table 2, the volume resistivity of the test example is superior to that of the comparative examples 2 to 4, and the conductive performance is good.
2. The test sample is cut into strip-shaped samples with the specification of 4cm by 5cm, the resistance values of the test sample under different stretching rates are detected, and the detection results are shown in table 3:
TABLE 3 results of resistance measurements at different elongations
Figure 443554DEST_PATH_IMAGE003
。
As can be seen from Table 3, the effective tensile rate of the test example is as high as 520%, and the resistance fluctuation range is small, so that the test example has good resistance and pressure-sensitive characteristics.

Claims (8)

1. A preparation method of a conductive silicone rubber composite material is characterized by comprising the following steps:
the preparation method comprises the following steps in sequence:
s1, uniformly mixing a conductive filler and n-heptane to obtain a mixture A, wherein the conductive filler is a mixture of graphene, carbon nanotubes and a carbon fiber material;
s2, uniformly mixing the liquid silicone rubber and n-heptane to obtain a mixture B;
s3, uniformly mixing the mixture A and the mixture B according to a required proportion, then sequentially carrying out vacuum pumping treatment, pouring and standing until n-heptane is completely volatilized, and curing to obtain the conductive silicone rubber composite material, wherein the mass ratio of the mixture A to the mixture B is 1:1-1.5, the content of graphene in the conductive silicone rubber composite material is 4.5-5.5wt%, the content of carbon nanotubes is 1-1.25wt%, and the content of carbon fibers is 6-7.5 wt%.
2. The method for preparing the conductive silicone rubber composite material according to claim 1, wherein: in step S2, the volume ratio of the liquid silicone rubber to the n-heptane is 1: 2-2.5.
3. The method for preparing a conductive silicone rubber composite material according to claim 1 or 2, wherein: in step S3, the curing specifically includes: curing for 30-45min in a constant-temperature drying box at the temperature of 120-130 ℃.
4. The method for preparing a conductive silicone rubber composite material according to claim 1 or 2, wherein: the carbon fiber material is carbon black.
5. The method for preparing the conductive silicone rubber composite material according to claim 1 or 2, wherein: in step S3, the mass ratio of the mixture A to the mixture B is 1: 1.2-1.3.
6. The method for preparing a conductive silicone rubber composite material according to claim 1 or 2, wherein: in step S3, the content of graphene in the conductive silicone rubber composite material is 4.8-5.1wt%, the content of carbon nanotubes is 1.1-1.18wt%, and the content of carbon fibers is 6.5-7.2 wt%.
7. The method for preparing the conductive silicone rubber composite material according to claim 2, wherein: the volume ratio of the liquid silicone rubber to the n-heptane is 1: 2.1-2.3.
8. The method for preparing the conductive silicone rubber composite material according to claim 3, wherein: the curing specifically comprises the following steps: curing for 35-40min in a constant-temperature drying oven at 125-128 ℃.
CN202210795691.3A 2022-07-07 2022-07-07 Preparation method of conductive silicone rubber composite material Pending CN115010964A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108165019A (en) * 2018-02-01 2018-06-15 青岛科技大学 A kind of electromagnetic shielding silicon rubber/graphene/carbon nano tube nanocomposite material and preparation method thereof
WO2021019923A1 (en) * 2019-07-30 2021-02-04 積水ポリマテック株式会社 Conductive composition, conductive film, contact member and method for producing conductive composition
CN112638993A (en) * 2018-09-28 2021-04-09 美国陶氏有机硅公司 Liquid silicone rubber composition

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108165019A (en) * 2018-02-01 2018-06-15 青岛科技大学 A kind of electromagnetic shielding silicon rubber/graphene/carbon nano tube nanocomposite material and preparation method thereof
CN112638993A (en) * 2018-09-28 2021-04-09 美国陶氏有机硅公司 Liquid silicone rubber composition
WO2021019923A1 (en) * 2019-07-30 2021-02-04 積水ポリマテック株式会社 Conductive composition, conductive film, contact member and method for producing conductive composition

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