CN107163582B - Silicone rubber and preparation method thereof - Google Patents
Silicone rubber and preparation method thereof Download PDFInfo
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- CN107163582B CN107163582B CN201710439873.6A CN201710439873A CN107163582B CN 107163582 B CN107163582 B CN 107163582B CN 201710439873 A CN201710439873 A CN 201710439873A CN 107163582 B CN107163582 B CN 107163582B
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- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention provides a preparation method of silicon rubber, which comprises the following steps: the method comprises the following steps: adding graphene into the first silicon rubber for mixing; adding graphene into the second silicon rubber for mixing; and mixing the first silicon rubber and the second silicon rubber, wherein the first silicon rubber is different from the second silicon rubber, and the graphene is prepared by adopting a low-temperature reduction method. The invention also provides the silicon rubber prepared by the method. The silicone rubber prepared by the method of the invention has higher tensile resilience.
Description
Technical Field
The invention belongs to the field of polymer composite materials, and particularly relates to high-tensile resilience silicon rubber and a preparation method thereof.
Background
Silicone rubber is a medical polymer material with excellent performance, and is concerned by professionals in the rubber industry and the medical field. The reasons are that firstly, the rubber medical material has high technical content, low cost, high added value and considerable economic benefit; secondly, the medical characteristics of the silicon rubber are utilized, so that the problems in medical science can be solved, and if the patients can obtain satisfactory curative effect. However, in some medical fields, the mechanical properties of the silicone rubber are poor, the tensile strength is low, and the use requirements cannot be met, so that the common medical silicone rubber is modified or filled with fillers. Generally, the compatibility of silane modified reinforced silicone rubber and a matrix achieves the purpose of enhancing mechanical properties, and reinforcing fillers such as white carbon black are added for modification. But their resilience is greatly compromised while they increase mechanical strength. The medical silicon rubber has poor tensile resilience without modification, cannot meet the use requirement, and cannot meet the requirement due to the absence of a proper modified material.
There is therefore a need in the art for improved silicone rubbers with high stretch resilience properties.
The technical contents listed in the prior art merely represent the techniques mastered by the inventor and are not of course considered as the prior art for evaluating the novelty and inventive step of the present invention.
Disclosure of Invention
The invention aims to provide high-tensile resilience silicon rubber, which is prepared by taking graphene as a filler, and can remarkably improve the tensile resilience. The graphene is low-temperature reduced graphene, so that oxygen-containing functional groups on the surface are greatly reserved, and the interface bonding force with rubber is good;
another object of the present invention is to provide a stretch resilient silicone rubber.
In order to achieve the above object, the present invention discloses the following technical solutions.
The invention provides silicon rubber which comprises the following components in parts by weight:
20-150 parts of first silicon rubber;
100 parts of second silicon rubber; and
0.1-1 part of graphene mixed in the first silicon rubber and the second silicon rubber,
wherein the first silicone rubber is different from the second silicone rubber, and the graphene content is 16.5-30 wt%.
The preferable scheme of the silicone rubber comprises the following components in parts by weight:
100 parts of first silicon rubber;
100 parts of second silicon rubber; and
0.6 part of graphene mixed in the first silicon rubber and the second silicon rubber,
the content of the graphene is 20 wt%. .
According to one aspect of the invention, the graphene is prepared by oxidation reduction at 100-300 ℃, preferably for 30min-24 h.
According to one aspect of the invention, the first silicone rubber comprises a dimethyl, methyl, vinyl silicone copolymer, and/or the second silicone rubber comprises a dimethyl, methyl silicone copolymer and a peroxide.
The invention provides a preparation method of silicon rubber, which comprises the following steps: the method comprises the following steps: adding graphene into the first silicon rubber, and mixing to obtain a material A; adding graphene into the second silicon rubber, and mixing to obtain a material B; and mixing the material A and the material B, wherein the first silicon rubber is different from the second silicon rubber, and the graphene is prepared by adopting a low-temperature reduction method.
According to one aspect of the invention, the graphene is prepared by oxidation reduction at 100-300 ℃, preferably for 30min-24 h.
According to one aspect of the invention, in the step of adding graphene into the first silicone rubber and mixing, the mass ratio of the first silicone rubber to the graphene is 100:0.05-0.5, preferably 100:0.3, and in the step of adding graphene into the second silicone rubber and mixing, the mass ratio of the second silicone rubber to the graphene is 100:0.05-0.5, preferably 100: 0.3.
According to one aspect of the invention, in the step of mixing by adding graphene into the first silicone rubber, mixing is carried out in an internal mixer or an open mill for 10min to 30min, preferably 20min, and in the step of mixing by adding graphene into the second silicone rubber, mixing is carried out in an internal mixer or an open mill for 10min to 30min, preferably 20 min.
The invention also provides a preparation method of the silicon rubber, which comprises the following steps: the method comprises the following steps: mixing the first silicon rubber and the second silicon rubber; and adding graphene into the first silicon rubber and the second silicon rubber for mixing, wherein the first silicon rubber is different from the second silicon rubber, and the graphene is prepared by adopting a low-temperature reduction method.
The invention also provides a silicone rubber prepared according to the above method.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of a method for preparing the silicone rubber of the present invention; and
figure 2 is tensile test data.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
According to one embodiment of the present invention, a method 100 of preparing a silicone rubber is provided. The silicone rubber prepared by the method has high tensile resilience. According to the method 100 for preparing the silicone rubber, graphene is used as a filler, and the tensile resilience performance of the prepared graphene silicone rubber can be obviously improved. The graphene is low-temperature reduced graphene, oxygen-containing functional groups on the surface are greatly reserved, and the interface bonding force with rubber is good. Researches show that the oxygen-containing functional group with the surface of the graphene sheet layer obtained by reduction at the reduction temperature of 100-300 ℃ for 30min-24h is combined with the functional group in the rubber by chemical bonds, so that the acting force for generating the chemical bonds is strongest, and the combination of the graphene and the rubber is improved.
The graphene used in the method 100 of the present invention is graphite oxide, which is reduced by heating at a low temperature to remove a part of oxygen-containing functional groups, so as to realize the graphene required by the present invention (the oxygen content is optimally 20%). And graphite oxide is reduced at low temperature (100-300 ℃), and the reduction time is 30min-24 h.
As shown in fig. 1, a method 100 for preparing a silicone rubber of the present invention includes: 101, adding graphene into first silicon rubber for mixing; 103, adding graphene into the second silicon rubber for mixing; 105, mixing the first silicon rubber and the second silicon rubber. The steps 101-105 are described below by way of specific examples. Wherein the first silicone rubber is different in composition from the second silicone rubber.
In step 101, the temperature is raised, for example using an internal mixer or an open mill, to 70 to 100 ℃, preferably 90 ℃. Weighing the component A of silicon rubber: and (3) mixing the materials with the graphene accounting for 100:0.05-0.5 mass ratio, preferably 100:0.3, in an internal mixer or an open mill for 10-30 min, preferably 20min for later use. The main component of the A-component silicone rubber is composed of dimethyl, methyl and vinyl silicone copolymers. The A-component silicone rubber can also be added with some auxiliary agents, such as silane coupling agents, dispersing agents and the like.
In step 103, weighing the silicone rubber component B: and (3) mixing the materials with the graphene accounting for 100:0.05-0.5 mass ratio, preferably 100:0.3, in an internal mixer or an open mill for 10-30 min, preferably 20min for later use. The main components of the component B silicone rubber are dimethyl silicone copolymer, methyl silicone copolymer and peroxide.
At step 105, A, B components are weighed out in a mass ratio of 0.2-1.5:1, preferably 1:1, and are mixed for 10min at 100 ℃ by using an internal mixer or an open mill to fully cure the silicone rubber. And preparing a rubber ring with a certain shape by using the cured silicon rubber, thereby carrying out a tensile resilience performance test.
In the process, the AB two components are respectively mixed with the graphene, and then the two components are mixed, wherein a secondary dispersion process of the graphene exists in the process. Thereby improving the dispersion of the graphene in the matrix and finally improving the mechanical property of the composite material. The component B contains a curing agent component, and the method disclosed by the invention avoids the problem that graphene is difficult to disperse due to advanced curing.
In the invention, under the condition of not adding any other modifier or auxiliary agent, only the graphene with low filling amount is added, so that the tensile resilience of the silicone rubber is greatly improved. Figure 2 shows tensile force test data. Fig. 2 shows that the addition of graphene increases the rebound resilience of silicone rubber from 1000% to 1200%, and increases the tensile strength by 200%.
The method 100 of the present invention is described below by way of specific examples.
Example one
Heating the internal mixer to 90 ℃, weighing 1000g of the component A silicone rubber and 3g of graphene, adding the components A into the internal mixer with constant temperature for mixing, and taking out the components A for later use after 20 min. Then 1000g of the B component silicone rubber and 3g of graphene are weighed and added into an internal mixer with constant temperature for mixing, and the mixture is taken out after 20 min. And (3) heating the internal mixer to 100 ℃, adding the component A silicone rubber and the component B silicone rubber into the internal mixer with constant temperature for mixing, taking out after 10min, preparing a rubber ring through a forming process, and testing the tensile resilience performance. The well mixed A, B two-component silicone rubber is medical silicone rubber with high tensile resilience.
Example two
Heating the mixture to 90 ℃ by using an open mill, weighing 1000g of the component A silicone rubber and 3g of graphene, adding the components A into a constant-temperature internal mixer for mixing, and taking out the components A for later use after 20 min. Then 1000g of the B component silicone rubber and 3g of graphene are weighed and added into an internal mixer with constant temperature for mixing, and the mixture is taken out after 20 min. And (3) heating the internal mixer to 100 ℃, adding the component A silicone rubber and the component B silicone rubber into the internal mixer with constant temperature for mixing, taking out after 10min, preparing a rubber ring through a forming process, and testing the tensile resilience performance. The well mixed A, B two-component silicone rubber is medical silicone rubber with high tensile resilience.
Example three
Heating the internal mixer to 90 ℃, weighing 1000g of the component A silicone rubber and 5g of graphene, adding the components A into the internal mixer with constant temperature for mixing, and taking out the components A for later use after 20 min. Then 1000g of the component silicon rubber and 5g of graphene are weighed and added into an internal mixer with constant temperature for mixing, and the mixture is taken out after 20 min. And (3) heating the internal mixer to 100 ℃, adding the component A silicone rubber and the component B silicone rubber into the internal mixer with constant temperature for mixing, taking out after 10min, preparing a rubber ring through a forming process, and testing the tensile resilience performance. The well mixed A, B two-component silicone rubber is medical silicone rubber with high tensile resilience.
Example four
Heating the internal mixer to 90 ℃, weighing 1000g of the component A silicone rubber and 0.5g of graphene, adding the components A into the internal mixer with constant temperature for mixing, and taking out the components A for later use after 20 min. Then 1000g of the B component silicone rubber and 0.5g of graphene are weighed and added into a constant-temperature internal mixer for mixing, and the mixture is taken out after 20 min. And (3) heating the internal mixer to 100 ℃, adding the component A silicone rubber and the component B silicone rubber into the internal mixer with constant temperature for mixing, taking out after 10min, preparing a rubber ring through a forming process, and testing the tensile resilience performance. The well mixed A, B two-component silicone rubber is medical silicone rubber with high tensile resilience.
Example five
Heating the internal mixer to 90 ℃, weighing 1000g of the component A silicone rubber and 5g of graphene, adding the components A into the internal mixer with constant temperature for mixing, and taking out the components A for later use after 30 min. Then 1000g of the component silicon rubber and 5g of graphene are weighed and added into an internal mixer with constant temperature for mixing, and the mixture is taken out after 30 min. And (3) heating the internal mixer to 100 ℃, adding the component A silicone rubber and the component B silicone rubber into the internal mixer with constant temperature for mixing, taking out after 10min, preparing a rubber ring through a forming process, and testing the tensile resilience performance. The well mixed A, B two-component silicone rubber is medical silicone rubber with high tensile resilience.
Example six
Heating the internal mixer to 90 ℃, weighing 1000g of the component A silicone rubber and 5g of graphene, adding the components A into the internal mixer with constant temperature for mixing, and taking out the components A for later use after 10 min. Then 1000g of the component silicon rubber and 5g of graphene are weighed and added into an internal mixer with constant temperature for mixing, and the mixture is taken out after 10 min. And (3) heating the internal mixer to 100 ℃, adding the component A silicone rubber and the component B silicone rubber into the internal mixer with constant temperature for mixing, taking out after 10min, preparing a rubber ring through a forming process, and testing the tensile resilience performance. The well mixed A, B two-component silicone rubber is medical silicone rubber with high tensile resilience.
Figure 2 shows tensile force test data. Fig. 2 shows that the addition of graphene increases the rebound resilience of silicone rubber from 1000% to 1200%, and increases the tensile strength by 200%.
According to another embodiment of the present invention, there is also provided a silicone rubber prepared by the above method 100.
According to another embodiment of the present invention, a silicone rubber is provided. The silicone rubber comprises: a first component silicone rubber, a second component silicone rubber, and graphene. Wherein the first component silicone rubber is different from the second component silicone rubber. The main component of the first component silicone rubber is composed of dimethyl, methyl and vinyl silicone copolymer. The second component silicone rubber mainly comprises dimethyl, methyl organic silicon copolymer and peroxide. The graphene is prepared by an oxidation-reduction method, and is reduced by graphite oxide at low temperature (100-300 ℃), wherein the reduction time is 30min-24 h.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The silicone rubber comprises the following components in parts by weight:
20-150 parts of first silicon rubber;
100 parts of second silicon rubber; and
0.1-1 part of graphene mixed in the first silicon rubber and the second silicon rubber,
wherein the first silicone rubber comprises a dimethyl, methyl, vinyl silicone copolymer, and the second silicone rubber comprises a dimethyl, methyl silicone copolymer and a peroxide; the oxygen content of the graphene is 20%; the graphene is prepared by oxidation reduction at 100-300 ℃ and is reduced for 30min-24 h;
the silicone rubber is prepared by the following method:
adding graphene into the first silicon rubber, and mixing to obtain a material A;
adding graphene into the second silicon rubber, and mixing to obtain a material B; and
and mixing the material A and the material B.
2. The silicone rubber according to claim 1, wherein each component comprises, in parts by weight:
100 parts of first silicon rubber;
100 parts of second silicon rubber; and
0.6 part of graphene mixed in the first silicon rubber and the second silicon rubber,
wherein the graphene has an oxygen content of 20%.
3. The silicone rubber according to claim 1 or 2, wherein in the step of adding graphene into the first silicone rubber and mixing, the mass ratio of the first silicone rubber to the graphene is 100: 0.05-0.5; and/or in the step of adding graphene into the second silicone rubber and mixing, the mass ratio of the second silicone rubber to the graphene is 100: 0.05-0.5.
4. The silicone rubber according to claim 3, wherein in the step of adding graphene to the first silicone rubber and mixing, the mass ratio of the first silicone rubber to the graphene is 100:0.3, and/or in the step of adding graphene to the second silicone rubber and mixing, the mass ratio of the second silicone rubber to the graphene is 100: 0.3.
5. The silicone rubber according to claim 4, wherein in the step of mixing the first silicone rubber with the added graphene, the first silicone rubber is mixed in an internal mixer or an open mill for 10min to 30min, and in the step of mixing the second silicone rubber with the added graphene, the second silicone rubber is mixed in the internal mixer or the open mill for 10min to 30 min.
6. The silicone rubber according to claim 5, wherein in the step of mixing the first silicone rubber with the added graphene, the mixture is mixed in an internal mixer or an open mill for 20min, and in the step of mixing the second silicone rubber with the added graphene, the mixture is mixed in the internal mixer or the open mill for 20 min.
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