CN107163582A - Silicon rubber and preparation method thereof - Google Patents
Silicon rubber and preparation method thereof Download PDFInfo
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- CN107163582A CN107163582A CN201710439873.6A CN201710439873A CN107163582A CN 107163582 A CN107163582 A CN 107163582A CN 201710439873 A CN201710439873 A CN 201710439873A CN 107163582 A CN107163582 A CN 107163582A
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- silicon rubber
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- 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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- Polymers & Plastics (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The present invention provides a kind of silicon rubber preparation method：Including：Graphene mixing is added in the first silicon rubber；Graphene mixing is added in the second silicon rubber；With by first silicon rubber and the second mixing silicon rubber, wherein first silicon rubber is different from second silicon rubber, the graphene is the graphene prepared using low-temperature reduction method.The present invention also provides silicon rubber prepared by a kind of use this method.The silicon rubber prepared by the method for the present invention has higher tensile property energy.
Description
Technical field
The present invention substantially belongs to field of polymer composite material, more particularly to a kind of high tensile property energy silicon rubber and its
Preparation method.
Background technology
Silicon rubber is as a kind of medical macromolecular materials of function admirable, either in rubber industry still in medical domain
All receive the concern of professional person.Its reason is, first, as rubber medical material, its with high content of technology, cost is low, additional
Value is high, economic benefit is very considerable；Second, using the medical characteristic of silicon rubber, many problems in medical skill can be solved, such as also may be used
Patient is set to obtain satisfactory effect.But in some medical fields, the mechanical property of silicon rubber in itself is very poor, and tensile strength is relatively low,
Use requirement can not be met, so general medical grade silicon rubber will pass through some modifications or filling filler.General is exactly silicon
The compatibility of alkane modification enhancing silicon rubber and matrix reaches the purpose of enhancing mechanical property, is also exactly to add the enhancing such as white carbon
Filler is modified.But they are while mechanical strength is strengthened, rebound performance can have a greatly reduced quality.It is medical without modification
The tensile property of silicon rubber can be very poor, does not reach use requirement, demand can not be similarly met by modified silicon rubber, because
To be suitable material modified.
Therefore there is the improvement demand of the silicon rubber for high tensile property energy in the art.
The technology contents listed in the prior art only represent the technology that inventor is grasped, and are not considered as naturally
It is novelty and creativeness that prior art and being used for evaluates the present invention.
The content of the invention
The purpose of the present invention is a kind of high tensile property energy silicon rubber, using graphene as filler, prepares graphene silicon rubber
Glue, can significantly improve tensile property energy.This graphene is low-temperature reduction graphene, greatly remains the oxygen-containing official on surface
It can roll into a ball, the interface binding power with rubber is preferable；
It is a further object of the present invention to provide a kind of tensile property energy silicon rubber.
To achieve these goals, the present invention is disclosed directly below technical scheme.
The invention provides a kind of silicon rubber, each component by weight, including：
First 20-150 parts of silicon rubber；
Second 100 parts of silicon rubber；With
0.1-1 parts of graphene in the first silicon rubber and the second silicon rubber is blended in,
Wherein described first silicon rubber is different from second silicon rubber, and the graphene is 16.5-30wt% containing dose rate.
As above-mentioned silicon rubber preferred scheme each component by weight, including：
First 100 parts of silicon rubber；
Second 100 parts of silicon rubber；With
0.6 part of graphene in the first silicon rubber and the second silicon rubber is blended in,
The graphene is 20wt% containing dose rate..
According to an aspect of the present invention, the graphene is to carry out redox preparation at 100 DEG C -300 DEG C,
It is preferred that reducing 30min-24h.
According to an aspect of the present invention, first silicon rubber includes dimethyl, methyl, vinyl organosilicon copolymerization
Thing, and/or second silicon rubber include dimethyl, methylsiloxane copolymer and peroxide.
The present invention provides a kind of silicon rubber preparation method：Including：Graphene mixing is added in the first silicon rubber, thing is obtained
Expect A；Graphene mixing is added in the second silicon rubber, material B is obtained；Kneaded with by the material A and material B, wherein described
First silicon rubber is different from second silicon rubber, and the graphene is the graphene prepared using low-temperature reduction method.
According to an aspect of the present invention, the graphene is to carry out redox preparation at 100 DEG C -300 DEG C,
It is preferred that reducing 30min-24h.
According to an aspect of the present invention, it is described graphene to be added in the first silicon rubber the step of knead, described the
The mass ratio of one silicon rubber and graphene is 100:0.05-0.5, preferably 100:0.3, it is described to add stone in the second silicon rubber
In the step of black alkene is kneaded, the mass ratio of second silicon rubber and graphene is 100:0.05-0.5, preferably 100:0.3.
According to an aspect of the present invention, it is described to be added in the first silicon rubber in the step of graphene is kneaded, in banburying
10min-30min, preferably 20min are kneaded in machine or mill, it is described that the step of graphene is kneaded is added in the second silicon rubber
In, 10min-30min, preferably 20min are kneaded in banbury or mill.
The present invention also provides a kind of silicon rubber preparation method：Including：By the first silicon rubber and the second mixing silicon rubber；With to
Graphene mixing is added in one silicon rubber and the second silicon rubber, wherein first silicon rubber is different from second silicon rubber,
The graphene is the graphene prepared using low-temperature reduction method.
The present invention also provides a kind of silicon rubber prepared according to above-mentioned method.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, the reality with the present invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the preparation method flow chart of the silicon rubber of the present invention；With
Fig. 2 is extension test data.
Embodiment
Hereinafter, some exemplary embodiments are simply just described.As one skilled in the art will recognize that
Like that, without departing from the spirit or scope of the present invention, described implementation can be changed by various different modes
Example.Therefore, accompanying drawing and description are considered essentially illustrative rather than restrictive.
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that preferred reality described herein
Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
There is provided a kind of method 100 for preparing silicon rubber according to one embodiment of present invention.The silicon prepared by this method
Rubber has high tensile property energy.The method 100 for preparing silicon rubber of the present invention prepares graphene silicon using graphene as filler
Rubber, can significantly improve tensile property energy.This graphene is low-temperature reduction graphene, greatly remains the oxygen-containing of surface
Functional group, the interface binding power with rubber is preferable.It has been investigated that, 30min-24h institutes are reduced under 100-300 DEG C of reduction temperature
Obtained oxygen-containing functional group with graphene film layer surface with and rubber in functional group carry out the combination of chemical bond, generationization
The active force for learning key is most strong, so as to improve the combination of graphene and rubber.
Graphene used in the method 100 of the present invention is that graphite oxide carries out heating reduction at low temperature, removes part
Oxygen-containing functional group, realizes the graphene (oxygen content most preferably 20%) required for the present invention.And be low by graphite oxide
Temperature is lower to be reduced (100 DEG C -300 DEG C), and the recovery time is 30min-24h.
As shown in figure 1, the preparation method 100 of the silicon rubber of the present invention includes：101, add graphite in the first silicon rubber
Alkene is kneaded；103, graphene mixing is added in the second silicon rubber；105, by the first silicon rubber and the second mixing silicon rubber.Below
Step 101-105 is described by specific example.Wherein the first silicon rubber is different from the second silicone rubber component.
In step 101, such as, using banbury or mill, it is warming up to 70-100 DEG C, preferably 90 DEG C.Weigh component A silicon
Rubber：Graphene=100:The material of 0.05-0.5 mass ratioes, preferably 100:0.3, then carried out in banbury or mill
Mixing, mixing time is 10min-30min, and preferably 20min is standby.The main component of component A silicon rubber be, for example, dimethyl,
Methyl, vinyl organosilicon copolymer composition.Some auxiliary agents, such as silane coupler can also be added in component A silicon rubber, are disperseed
Agent etc.
In step 103, B component silicon rubber is weighed：Graphene=100:The material of 0.05-0.5 mass ratioes, preferably 100:
0.3, then kneaded in banbury or mill, mixing time is 10min-30min, preferably 20min, standby.B component
Silicon rubber main component is that dimethyl, methylsiloxane copolymer and peroxide are constituted.
In step 105, by A, B component according to 0.2-1.5:1 mass ratio carries out weighing, preferably 1:1, using banbury or
Mill carries out refining 10min at 100 DEG C, silicon rubber is fully solidified.Prepared necessarily using the silicon rubber after solidification
The rubber ring of shape, so that carrying out tensile property can test.
Above-mentioned technique, the components of AB two are first each kneaded with graphene, are then kneaded two components, in the technique
It there is the twice dispersing process of graphene.So as to improve, graphene is scattered in matrix, the power of final raising composite
Learn performance.Contain curing agent component in B component, cause graphene to be difficult to scattered ask inventive process avoids premature cure
Topic.
In the present invention, in the case of without any other modifying agent or auxiliary agent, the graphene of low loading is only added,
The tensile property of silicon rubber is set to greatly promote.Fig. 2 shows tensile strength testing data.Following knot can be drawn by Fig. 2
By by adding graphene, the drawing recovery of silicon rubber brings up to 1200% by original 1000%, and tensile strength is improved
200%.
The method 100 of the present invention is described below by specific example.
Example one
Banbury is heated to 90 DEG C, weighs 1000g component A silicon rubber, 3g graphene, adds into constant close of temperature
Kneaded in mill, take out standby after 20min.Then 1000gB component silicone rubbers, 3g graphenes are weighed, is added permanent into temperature
Kneaded, taken out after 20min in fixed banbury.Banbury temperature is warming up to 100 DEG C, then by component A silicon rubber and B
Component silicone rubber is added to be kneaded into the constant banbury of temperature, is taken out, is then prepared by moulding process after 10min
Rubber ring, tests tensile property energy.A, the B two-component silicon rubber mixed is high tensile property energy medical grade silicon rubber.
Example two
Mill is heated to 90 DEG C, weighs 1000g component A silicon rubber, 3g graphene, adds into constant close of temperature
Kneaded in mill, take out standby after 20min.Then 1000gB component silicone rubbers, 3g graphenes are weighed, is added permanent into temperature
Kneaded, taken out after 20min in fixed banbury.Banbury temperature is warming up to 100 DEG C, then by component A silicon rubber and B
Component silicone rubber is added to be kneaded into the constant banbury of temperature, is taken out, is then prepared by moulding process after 10min
Rubber ring, tests tensile property energy.A, the B two-component silicon rubber mixed is high tensile property energy medical grade silicon rubber.
Example three
Banbury is heated to 90 DEG C, weighs 1000g component A silicon rubber, 5g graphene, adds into constant close of temperature
Kneaded in mill, take out standby after 20min.Then 1000gB component silicone rubbers, 5g graphenes are weighed, is added permanent into temperature
Kneaded, taken out after 20min in fixed banbury.Banbury temperature is warming up to 100 DEG C, then by component A silicon rubber and B
Component silicone rubber is added to be kneaded into the constant banbury of temperature, is taken out, is then prepared by moulding process after 10min
Rubber ring, tests tensile property energy.A, the B two-component silicon rubber mixed is high tensile property energy medical grade silicon rubber.
Example four
Banbury is heated to 90 DEG C, weighs 1000g component A silicon rubber, 0.5g graphene, adds constant into temperature
Kneaded in banbury, take out standby after 20min.Then 1000gB component silicone rubbers, 0.5g graphenes are weighed, is added into temperature
Kneaded, taken out after 20min in the constant banbury of degree.Banbury temperature is warming up to 100 DEG C, then by component A silicon rubber
Glue is added with B component silicon rubber and kneaded into the constant banbury of temperature, is taken out after 10min, is then passed through moulding process
Rubber ring is prepared, tensile property energy is tested.A, the B two-component silicon rubber mixed is that high tensile property can medical silicon
Rubber.
Example five
Banbury is heated to 90 DEG C, weighs 1000g component A silicon rubber, 5g graphene, adds into constant close of temperature
Kneaded in mill, take out standby after 30min.Then 1000gB component silicone rubbers, 5g graphenes are weighed, is added permanent into temperature
Kneaded, taken out after 30min in fixed banbury.Banbury temperature is warming up to 100 DEG C, then by component A silicon rubber and B
Component silicone rubber is added to be kneaded into the constant banbury of temperature, is taken out, is then prepared by moulding process after 10min
Rubber ring, tests tensile property energy.A, the B two-component silicon rubber mixed is high tensile property energy medical grade silicon rubber.
Example six
Banbury is heated to 90 DEG C, weighs 1000g component A silicon rubber, 5g graphene, adds into constant close of temperature
Kneaded in mill, take out standby after 10min.Then 1000gB component silicone rubbers, 5g graphenes are weighed, is added permanent into temperature
Kneaded, taken out after 10min in fixed banbury.Banbury temperature is warming up to 100 DEG C, then by component A silicon rubber and B
Component silicone rubber is added to be kneaded into the constant banbury of temperature, is taken out, is then prepared by moulding process after 10min
Rubber ring, tests tensile property energy.A, the B two-component silicon rubber mixed is high tensile property energy medical grade silicon rubber.
Fig. 2 shows tensile strength testing data.It can be drawn the following conclusions by Fig. 2, by adding graphene, silicon rubber
Drawing recovery bring up to 1200% by original 1000%, tensile strength improves 200%.
According to another implementation of the invention, a kind of silicon rubber prepared by the above method 100 is also provided.
There is provided a kind of silicon rubber according to another implementation of the invention.The silicon rubber includes：First component silicon rubber
Glue, the second component silicone rubber, and graphene.Wherein described first component silicone rubber is different from the second component silicone rubber.First group
The main component for dividing silicon rubber is, for example, dimethyl, methyl, vinyl organosilicon copolymer composition.Second component silicone rubber is main
Composition is that dimethyl, methylsiloxane copolymer and peroxide are constituted.Wherein described graphene is prepared by oxidation-reduction method,
And be to be reduced (100 DEG C -300 DEG C) at low temperature by graphite oxide, the recovery time is 30min-24h.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention's
Within protection domain.
Claims (10)
1. a kind of silicon rubber, each component by weight, including：
First 20-150 parts of silicon rubber；
Second 100 parts of silicon rubber；With
0.1-1 parts of graphene in the first silicon rubber and the second silicon rubber is blended in,
Wherein described first silicon rubber is different from second silicon rubber, and the graphene is 16.5-30wt% containing dose rate.
2. silicon rubber according to claim 1, it is characterised in that each component by weight, including：
First 100 parts of silicon rubber；
Second 100 parts of silicon rubber；With
0.6 part of graphene in the first silicon rubber and the second silicon rubber is blended in,
Wherein described graphene is 20wt% containing dose rate.
3. silicon rubber according to claim 1 or 2, it is characterised in that the graphene is to enter to advance at 100 DEG C -300 DEG C
Prepared by row redox.
4. silicon rubber according to claim 3, it is characterised in that reduction 30min-24h.
5. silicon rubber according to claim 1 or 2, it is characterised in that first silicon rubber include dimethyl, methyl,
Vinyl organosilicon copolymer, and/or second silicon rubber include dimethyl, methylsiloxane copolymer and peroxide.
6. the preparation method of the silicon rubber according to claim any one of 1-5, including：
Graphene mixing is added in the first silicon rubber, material A is obtained；
Graphene mixing is added in the second silicon rubber, material B is obtained；With
The material A and the material B are kneaded.
7. the preparation method of silicon rubber according to claim 6, it is characterised in that described to add stone in the first silicon rubber
In the step of black alkene is kneaded, the mass ratio of first silicon rubber and graphene is 100:0.05-0.5；And/or, it is described
Added in two silicon rubber in the step of graphene is kneaded, the mass ratio of second silicon rubber and graphene is 100:0.05-
0.5。
8. the preparation method of silicon rubber according to claim 7, it is characterised in that described to add stone in the first silicon rubber
In the step of black alkene is kneaded, the mass ratio of first silicon rubber and graphene is 100:0.3, and/or, it is described in the second silicon rubber
Added in glue in the step of graphene is kneaded, the mass ratio of second silicon rubber and graphene is 100:0.3.
9. the preparation method of silicon rubber according to claim 6, it is characterised in that described to add stone in the first silicon rubber
In the step of black alkene is kneaded, 10min-30min is kneaded in banbury or mill, it is described to add graphite in the second silicon rubber
In the step of alkene is kneaded, 10min-30min is kneaded in banbury or mill.
10. the preparation method of silicon rubber according to claim 9, it is characterised in that described to be added in the first silicon rubber
In the step of graphene is kneaded, 20min is kneaded in banbury or mill, the graphene that added in the second silicon rubber is mixed
In the step of refining, 20min is kneaded in banbury or mill.
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