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 PDF

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CN109082123A
CN109082123A CN201810686542.7A CN201810686542A CN109082123A CN 109082123 A CN109082123 A CN 109082123A CN 201810686542 A CN201810686542 A CN 201810686542A CN 109082123 A CN109082123 A CN 109082123A
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graphene
electromagnetic shielding
silicon rubber
modified electromagnetic
silastic material
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CN109082123B (en
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陆燕红
洪宁宁
鲁进敏
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Shanghai Electric Cable Research Institute
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0806Silver
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0812Aluminium
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/221Oxides; Hydroxides of metals of rare earth metal
    • C08K2003/2213Oxides; Hydroxides of metals of rare earth metal of cerium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2272Ferric oxide (Fe2O3)
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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

Modified electromagnetic shielding silastic material of graphene and preparation method thereof
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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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
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