CN109082123A - Modified electromagnetic shielding silastic material of graphene and preparation method thereof - Google Patents
Modified electromagnetic shielding silastic material of graphene and preparation method thereof Download PDFInfo
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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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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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Abstract
The present invention provides modified electromagnetic shielding silastic material of a kind of graphene and preparation method thereof, and the raw material of the material includes at least the component of following parts by weight: 100 parts of silicon rubber;5~50 parts of graphene-silicon rubber;0.2~1.0 part of crosslinking agent;10~150 parts of conductive metal material;5 ~ 50 parts of auxiliary agent.The method at least includes the following steps: by graphene and octamethylcy-clotetrasiloxane (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4), acquisition graphene-silicon rubber is mixed and reacted under anionic catalyst, then is kneaded jointly in proportion with other components.The application or material keeping its mechanical performance and the prior art to maintain an equal level, in 300-1000MHz shield effectiveness up to 80dB, density can be down to 1.80g/cm3。
Description
Technical field
The present invention relates to a kind of electromagnetic shield rubber materials, belong to electromagnetic shielding material field, and in particular to a kind of graphite
The modified electromagnetic shielding silastic material of alkene.
Background technique
In order to effectively inhibit electromagnetic interference and electromagnetic pollution, designs and prepare high-efficiency electromagnetic shielding material and have become one
Problem in the urgent need to address.For screening conductive material based on metal, but the disadvantage is that quality is big, price is high currently on the market
It is expensive, and molding not easy to be processed.With the development of materials industry, shield electromagnetic radiation conductive rubber material be continuously available exploitation and
Using, just gradually replace pure metal shielding material.Using graphene filler and its dispersion and electrical conduction mechanism in rubber is studied,
It is suitable for the small and light demand of delicate electronic device, and improves the comprehensive performance of electromagnetic shield rubber, to realize electromagnetic shielding rubber
The demand for development of glue " thin, light, wide, strong ".However graphene is difficult to reach in rubber matrix since surface is substantially without group
It is uniform to disperse and make its density larger due to needing to add metal material in the prior art.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide the modified electromagnetic shielding silicon rubbers of graphene
Glue material and preparation method thereof.Cause material close since metal packing dosage is larger in solution in the prior art electromagnetic shield rubber
Spend larger situation.The invention solves another question be: graphene is as the optimal material of electric conductivity, because of surface
There is no other groups, it is difficult to form the distribution of stable homogeneous with rubber matrix.
In order to achieve the above objects and other related objects, the present invention provides a kind of modified electromagnetic shielding silicon rubber material of graphene
Material, the material include at least the component of following parts by weight:
What the graphene-silicon rubber referred to graphene uniform is dispersed in the complex formed in silicon rubber.
Preferably, the modified electromagnetic shielding silastic material of the graphene at least further includes the component of following parts by weight:
0.1~100 part of non-metallic conducting material;Preferably 1~80 part;More preferably 10~50 parts.
Optimization, the modified electromagnetic shielding silastic material of above-mentioned graphene, includes the component of following parts by weight:
Optimization, the modified electromagnetic shielding silastic material of above-mentioned graphene, includes the component of following parts by weight:
Optimization, the modified electromagnetic shielding silastic material of above-mentioned graphene, includes the component of following parts by weight:
Further, the molecular weight that the silicon rubber is is 350,000-150;Preferably 50~1,000,000.
Further, the crosslinking agent is selected from 2,5- dimethyl -2,5- di-t-butyl hexane peroxide (DBPMH), peroxide
Change di-t-butyl (DTBP), any one or more in cumyl peroxide (DCP).
Further, the conductive metal material is selected from one of silver powder, silver-plated copper powder, silvered aluminum powder or a variety of.
Further, the non-metallic conducting material is selected from silver-plated glass beads, Ni-coated graphite, conductive black, nano-sized carbon
Any one or more in pipe.
Further, any one or a few in filler, heat-resistant agent, release agent, constitution controller of the auxiliary agent.
Further, it is one such or several to be selected from precipitated silica, diatomite, glass powder for above-mentioned filler.
Further, above-mentioned heat-resistant agent is selected from the one or more of iron oxide, cerium oxide, zinc oxide.
Further, above-mentioned release agent is selected from one or both of stearic acid, zinc stearate.
Further, above structure controlling agent is selected from one or both of hydroxy silicon oil, diphenyl silanediol.
To solve the above-mentioned problems, another aspect provides the modified electromagnetic shielding silicon rubber materials of above-mentioned graphene
The preparation method of material, the method at least include the following steps:
By graphene and octamethylcy-clotetrasiloxane (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4), in anion
Acquisition graphene-silicon rubber is mixed and reacted under catalyst, then is kneaded jointly in proportion with other components.
Further, the anionic catalyst is to appoint in tetramethylammonium hydroxide silicon alkoxide or tetramethylammonium hydroxide
Meaning is one or two kinds of.
Specifically, the above method the following steps are included:
(1) octamethylcy-clotetrasiloxane of vacuum drying (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4) are put into
Protective atmosphere and under reaction kettle in, be added anionic catalyst, be added graphene, mix, obtain graphene-silicon rubber, it is close
Envelope;
(2) each component is added in mixer in proportion and is blended, obtain rubber compound;
(3) by the mill blending, vulcanization on a mill of rubber compound and vulcanizing agent.
Preferably, the step (1) specifically: be warming up to 60-80 DEG C after catalyst is added, be added after graphene in 800-
It is mixed under the speed of 2000rpm, keeps 20~40min, then heated to 100 DEG C ± 10 DEG C and kept for 1~3 hour, finally risen again
Then temperature vacuumizes (50mmHg) to 150 DEG C of ± 10 DEG C of 20~40min of holding, be warming up to 180 DEG C ± 10 DEG C, keep 20~
40min。
Further, the quality of the octamethylcy-clotetrasiloxane (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4)
Than for 600:1~700:1.
Further, the mass ratio of the graphene and octamethylcy-clotetrasiloxane is 1:10~1:5.
Further, the mass ratio of the anionic catalyst and octamethylcy-clotetrasiloxane is 1:10000.
Further, the anionic catalyst is tetramethylammonium hydroxide silicon alkoxide, appointing in tetramethylammonium hydroxide
Meaning is one or more of.
Further, the protection gas is nitrogen or other inert gases.
Preferably, the mixer mixing time is 20~60 minutes in the step (2).
Further, it vacuumizes when mixing in the step (2), and cools down simultaneously.
Further, curing temperature is 160 DEG C~170 DEG C in the step (3), and the time is 5~10 minutes.
As described above, modified electromagnetic shielding silastic material of graphene of the invention and preparation method thereof, has with following
Beneficial effect:
Its mechanical performance and the prior art is being kept to maintain an equal level, in 300-1000MHz shield effectiveness up to 80dB, density can
Down to 1.80g/cm3。
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.It should be clear that the process equipment or device that are not indicated specifically in the following example
It is all made of conventional equipment or device in the art.In addition, it should also be understood that, one or more method and step mentioned in the present invention is simultaneously
Do not repel and may be used also before and after the combination step there may also be other methods step or between these explicitly mentioned steps
To be inserted into other methods step, unless otherwise indicated;It should also be understood that one or more equipment/device mentioned in the present invention it
Between combination connection relationship do not repel before and after the unit equipment/device there may also be other equipment/device or at this
It can also be inserted into other equipment/device between the two equipment/devices specifically mentioned a bit, unless otherwise indicated.Moreover, unless another
It is described, the number of various method steps is only the convenient tool of identification various method steps, rather than is the row of limitation various method steps
Column order limits the scope of the invention, and relativeness is altered or modified, without essence change technology contents
In the case of, when being also considered as the enforceable scope of the present invention.
Embodiment 1
Raw material is matched by following parts by weight:
First weigh vacuum drying octamethylcy-clotetrasiloxane (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4) (matter
Amount is than 600:1) it is put into the reaction kettle of nitrogen atmosphere, 1% concentration tetramethylammonium hydroxide silicon alkoxide is added (is with D4 mass ratio
1:100), 60 DEG C are warming up to, graphene (being 1:10 with D4 mass ratio) is added, mixing speed 1500rpm keeps 30min, then
It is warming up to 100 DEG C to be kept for 1 hour, is finally warming up to 150 DEG C of holding 20min again.Then (50mmHg) is vacuumized, is warming up to 180
DEG C, keep 20min.
Silicon rubber, graphene masterbatch and other raw materials (in addition to DBPMH) are put into mixer are blended according to the proportion
40min, when mixing, vacuumize, and cool down simultaneously, obtain electromagnetic shielding silicon rubber gross rubber;By rubber compound and DBPMH according to matching
It is blended than mill on a mill, is sulfided into product with mould shape on vulcanizing press, conditions of vulcanization: 170 DEG C × 5min.
The detection of product:
With reference to GJB 6190-2008 " electromagnetic shielding material shield effectiveness measurement method ", GB/T 533-2008 " vulcanization rubber
The measurement of glue or thermoplastic elastomer density " and GB/T 528-2009 " vulcanized rubber or thermoplastic elastomer tensile stress-strain performance
Measurement " to product carry out performance detection, as a result are as follows:
1 embodiment of table, 1 performance test results
Project | Unit | As a result |
Tensile strength | MPa | 2.8 |
Elongation at break | % | 180 |
Density (23 DEG C) | g/cm3 | 4.1 |
Shield effectiveness (300-1000MHz) | dB | 92 |
Embodiment 2
Raw material is matched by following parts by weight:
First weigh vacuum drying octamethylcy-clotetrasiloxane (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4) (matter
Amount is than 700:1) it is put into the reaction kettle of nitrogen atmosphere, 1% concentration tetramethylammonium hydroxide of addition (it is 1 with D4 mass ratio:
100) 70 DEG C, are warming up to, graphene (being 1:5 with D4 mass ratio) is added, mixing speed 2000rpm keeps 20min, then rises
Temperature to 110 DEG C keep 2 hours, be finally warming up to 160 DEG C of holding 40min again.Then (50mmHg) is vacuumized, is warming up to 170 DEG C,
Keep 30min.
Silicon rubber, graphene masterbatch and other raw materials (in addition to DBPMH and DTBP) are put into mixer altogether according to the proportion
Mixed 40min, when mixing, vacuumize, and cool down simultaneously, obtain electromagnetic shielding silicon rubber gross rubber;By rubber compound and DTBP, DBPMH
Mill is blended on a mill according to the proportion, is sulfided into product with mould shape on vulcanizing press, conditions of vulcanization: 165 DEG C
×8min。
The detection of product:
With reference to GJB 6190-2008 " electromagnetic shielding material shield effectiveness measurement method ", GB/T 533-2008 " vulcanization rubber
The measurement of glue or thermoplastic elastomer density " and GB/T 528-2009 " vulcanized rubber or thermoplastic elastomer tensile stress-strain performance
Measurement " to product carry out performance detection, as a result are as follows:
2 embodiment of table, 2 performance test results
Project | Unit | As a result |
Tensile strength | MPa | 4.8 |
Elongation at break | % | 300 |
Density (23 DEG C) | g/cm3 | 3.2 |
Shield effectiveness (300-1000MHz) | dB | 89 |
Embodiment 3
Raw material is matched by following parts by weight:
First weigh vacuum drying octamethylcy-clotetrasiloxane (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4) (matter
Amount is than 660:1) it is put into the reaction kettle of nitrogen atmosphere, 1% concentration tetramethylammonium hydroxide of addition (it is 1 with D4 mass ratio:
100) 80 DEG C, are warming up to, graphene (being 1.2:10 with D4 mass ratio) is added, mixing speed 2000rpm keeps 40min, then
It is warming up to 90 DEG C to be kept for 4 hours, is finally warming up to 150 DEG C of holding 30min again.Then (50mmHg) is vacuumized, is warming up to 190
DEG C, keep 20min.
Silicon rubber, graphene masterbatch and other raw materials (in addition to DBPMH and DCP) are put into mixer are blended according to the proportion
50min, when mixing, vacuumize, and cool down simultaneously, obtain electromagnetic shielding silicon rubber gross rubber;Rubber compound and DCP, DBPMH are pressed
According to proportion, mill is blended on a mill, is sulfided into product with mould shape on vulcanizing press, conditions of vulcanization: 160 DEG C ×
10min。
The detection of product:
With reference to GJB 6190-2008 " electromagnetic shielding material shield effectiveness measurement method ", GB/T 533-2008 " vulcanization rubber
The measurement of glue or thermoplastic elastomer density " and GB/T 528-2009 " vulcanized rubber or thermoplastic elastomer tensile stress-strain performance
Measurement " to product carry out performance detection, as a result are as follows:
3 embodiment of table, 3 performance test results
Project | Unit | As a result |
Tensile strength | MPa | 3.7 |
Elongation at break | % | 350 |
Density (23 DEG C) | g/cm3 | 3.0 |
Shield effectiveness (300-1000MHz) | dB | 90 |
Embodiment 4
Raw material is matched by following parts by weight:
First weigh vacuum drying octamethylcy-clotetrasiloxane (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4) (matter
Amount is than 660:1) it is put into the reaction kettle of nitrogen atmosphere, 1% concentration tetramethylammonium hydroxide of addition (it is 1 with D4 mass ratio:
100) 70 DEG C, are warming up to, graphene (being 1.2:10 with D4 mass ratio) is added, mixing speed 800rpm keeps 30min, then
It is warming up to 100 DEG C to be kept for 3 hours, is finally warming up to 150 DEG C of holding 30min again.Then (50mmHg) is vacuumized, is warming up to 180
DEG C, keep 30min.
Silicon rubber, graphene masterbatch and other raw materials (in addition to DBPMH) are put into mixer are blended according to the proportion
60min, when mixing, vacuumize, and cool down simultaneously, obtain electromagnetic shielding silicon rubber gross rubber;By rubber compound and DBPMH according to matching
It is blended than mill on a mill, is sulfided into product with mould shape on vulcanizing press, conditions of vulcanization: 170 DEG C × 5min.
The detection of product:
With reference to GJB 6190-2008 " electromagnetic shielding material shield effectiveness measurement method ", GB/T 533-2008 " vulcanization rubber
The measurement of glue or thermoplastic elastomer density " and GB/T 528-2009 " vulcanized rubber or thermoplastic elastomer tensile stress-strain performance
Measurement " to product carry out performance detection, as a result are as follows:
4 embodiment of table, 4 performance test results
Project | Unit | As a result |
Tensile strength | MPa | 1.6 |
Elongation at break | % | 380 |
Density (23 DEG C) | g/cm3 | 2.3 |
Shield effectiveness (300-1000MHz) | dB | 90 |
Embodiment 5
Raw material is matched by following parts by weight:
First weigh vacuum drying octamethylcy-clotetrasiloxane (D4) and t etram-ethyltetravinylcyclotetrasiloxane (V4) (matter
Amount is than 660:1) it is put into the reaction kettle of nitrogen atmosphere, 1% concentration tetramethylammonium hydroxide of addition (it is 1 with D4 mass ratio:
100) 70 DEG C, are warming up to, graphene (being 1:10 with D4 mass ratio) is added, mixing speed 1200rpm keeps 30min, then rises
Temperature to 100 DEG C keep 3 hours, be finally warming up to 150 DEG C of holding 30min again.Then (50mmHg) is vacuumized, is warming up to 180 DEG C,
Keep 30min.
Silicon rubber, graphene masterbatch and other raw materials (in addition to DBPMH) are put into mixer are blended according to the proportion
60min, when mixing, vacuumize, and cool down simultaneously, obtain electromagnetic shielding silicon rubber gross rubber;By rubber compound and DBPMH according to matching
It is blended than mill on a mill, is sulfided into product with mould shape on vulcanizing press, conditions of vulcanization: 165 DEG C ×
10min。
The detection of product:
With reference to GJB 6190-2008 " electromagnetic shielding material shield effectiveness measurement method ", GB/T 533-2008 " vulcanization rubber
The measurement of glue or thermoplastic elastomer density " and GB/T 528-2009 " vulcanized rubber or thermoplastic elastomer tensile stress-strain performance
Measurement " to product carry out performance detection, as a result are as follows:
5 embodiment of table, 5 performance test results
Project | Unit | As a result |
Tensile strength | MPa | 5.0 |
Elongation at break | % | 400 |
Density (23 DEG C) | g/cm3 | 1.8 |
Shield effectiveness (300-1000MHz) | dB | 82 |
Above embodiment is can not to be interpreted as in order to illustrate embodiment disclosed by the invention to limit of the invention
System.In addition, in various modifications and invention listed herein method, composition variation, do not departing from the scope of the present invention
Be obvious for those skilled in the art under the premise of spirit.Although having combined of the invention a variety of specific
Preferred embodiment has carried out specific description to the present invention, it is to be understood that, the present invention should not be limited only to these specific embodiments.
In fact, various obviously modify as described above for those skilled in the art to obtain invention all should include
Within the scope of the invention.
Claims (11)
1. a kind of modified electromagnetic shielding silastic material of graphene, which is characterized in that the modified electromagnetic shielding silicon rubber of the graphene
The raw material of glue material includes at least following parts by weight:
What the graphene-silicon rubber referred to graphene uniform is dispersed in the complex formed in silicon rubber.
2. the modified electromagnetic shielding silastic material of graphene according to claim 1, it is characterised in that: the graphene changes
Property electromagnetic shielding silastic material at least further include following parts by weight component: it is 0.1~100 part of non-metallic conducting material, described
Any one or more of non-metallic conducting material in silver-plated glass beads, Ni-coated graphite, conductive black, carbon nanotubes.
3. the modified electromagnetic shielding silastic material of graphene according to claim 1, it is characterised in that: the silicon rubber is
Molecular weight be 350,000-150;Preferably 50~1,000,000.
4. the modified electromagnetic shielding silastic material of graphene according to claim 1, it is characterised in that: the crosslinking agent choosing
From any one in 2,5- dimethyl -2,5- di-t-butyl hexane peroxide, di-t-butyl peroxide, cumyl peroxide
Or it is a variety of.
5. the modified electromagnetic shielding silastic material of graphene according to claim 1, it is characterised in that: the metallic conduction
Material is selected from one of silver powder, silver-plated copper powder, silvered aluminum powder or a variety of.
6. the modified electromagnetic shielding silastic material of graphene according to claim 1, it is characterised in that: the auxiliary agent is selected from
Filler, heat-resistant agent, release agent, any one or a few in constitution controller.
7. the modified electromagnetic shielding silastic material of graphene according to claim 6, it is characterised in that: the graphene changes
Property electromagnetic shielding silastic material further include any one or a few in following technical characteristic:
(1) it is one such or several to be selected from precipitated silica, diatomite, glass powder for the filler;
(2) heat-resistant agent is selected from the one or more of iron oxide, cerium oxide, zinc oxide;
(3) release agent is selected from one or both of stearic acid, zinc stearate;
(4) constitution controller is selected from one or both of hydroxy silicon oil, diphenyl silanediol.
8. the preparation side of the modified electromagnetic shielding silastic material of graphene as described in any one of claim 1~7 claim
Method, the method at least include the following steps:
By graphene and octamethylcy-clotetrasiloxane and t etram-ethyltetravinylcyclotetrasiloxane, mixed under anionic catalyst
And acquisition graphene-silicon rubber is reacted, then be kneaded jointly in proportion with other components.
9. preparation method according to claim 8, which is characterized in that the preparation method specifically:
(1) octamethylcy-clotetrasiloxane of vacuum drying and t etram-ethyltetravinylcyclotetrasiloxane are put into protective atmosphere under
Reaction kettle in, be added anionic catalyst, be added graphene, mix, obtain graphene-silicon rubber, sealing;
(2) each component is added in mixer in proportion and is blended, obtain rubber compound;
(3) by the mill blending, vulcanization on a mill of rubber compound and vulcanizing agent.
10. preparation method according to claim 9, it is characterised in that: the step (1) specifically: after catalyst is added
It is warming up to 60-80 DEG C, is mixed under the speed of 800-2000rpm after graphene is added, 20~40min is kept, then heats to
100 DEG C ± 10 DEG C are kept for 1~3 hour, are finally warming up to 150 DEG C of ± 10 DEG C of 20~40min of holding again, are then vacuumized, and are heated up
To 180 DEG C ± 10 DEG C, 20~40min is kept.
11. preparation method according to claim 9, it is characterised in that: the preparation method further includes following technical characteristic
In any one or a few:
1) mass ratio of the octamethylcy-clotetrasiloxane and t etram-ethyltetravinylcyclotetrasiloxane is 600:1~700:1;
2) mass ratio of the graphene and octamethylcy-clotetrasiloxane is 1:10~1:5;
3) mass ratio of the anionic catalyst and octamethylcy-clotetrasiloxane is 1:10000;
4) the mixer mixing time is 20~60 minutes in the step (2);
5) it vacuumizes when mixing in the step (2), and cools down simultaneously;
6) curing temperature is 160 DEG C~170 DEG C in the step (3), and the time is 5~10 minutes.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110819117A (en) * | 2019-12-12 | 2020-02-21 | 哈尔滨工业大学 | Preparation method of silicone resin-graphene composite material |
CN112322041A (en) * | 2020-11-11 | 2021-02-05 | 矽时代材料科技股份有限公司 | Electromagnetic shielding rubber and preparation method and application thereof |
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CN110819117A (en) * | 2019-12-12 | 2020-02-21 | 哈尔滨工业大学 | Preparation method of silicone resin-graphene composite material |
CN112322041A (en) * | 2020-11-11 | 2021-02-05 | 矽时代材料科技股份有限公司 | Electromagnetic shielding rubber and preparation method and application thereof |
CN113956838A (en) * | 2021-11-02 | 2022-01-21 | 中国科学院长春应用化学研究所 | Radiation modified electromagnetic shielding silicone rubber self-adhesive tape and preparation method thereof |
CN113999648A (en) * | 2021-12-20 | 2022-02-01 | 南通强生光电科技有限公司 | Graphene bottom sealing adhesive and preparation method thereof |
CN114231041A (en) * | 2021-12-31 | 2022-03-25 | 上海电缆研究所有限公司 | B1-grade flame-retardant ceramic low-smoke silicone rubber cable material and preparation method thereof |
CN115340768A (en) * | 2022-09-30 | 2022-11-15 | 宁波恒浩广新型电子材料有限公司 | Preparation process and application of stainless steel-based electromagnetic shielding material |
CN115340768B (en) * | 2022-09-30 | 2024-07-05 | 宁波恒浩广新型电子材料有限公司 | Preparation process and application of stainless steel-based electromagnetic shielding material |
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