CN104448837B - A kind of high temperature resistant electromagnetic shielding heat-shrink tube and preparation method thereof - Google Patents
A kind of high temperature resistant electromagnetic shielding heat-shrink tube and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of high temperature resistant electromagnetic shielding heat-shrink tube, and it is made up of the raw material of following proportion by weight：Silicon rubber 100, thermoplastic resin 10~50, reinforcing agent 5~30, vulcanizing agent 1.5~6, silicone oil 2~20, denatured conductive powder 175~543.Cable, connector for needing electromagnetic protection under hot environment.Meanwhile, the present invention also provides the specific steps that a kind of above-mentioned material processes heat-shrink tube：Cold mixed, heat is mixed, be blended, extrude vulcanization, expansion sizing.The heat-shrink tube prepared using the present invention has good stability, high-fire resistance, cold resistance and excellent electromagnetic protection performance, 200 DEG C of high temperature above can be for a long time tolerated, can apply to have the electric power of high request, electronics industry place to heat-resisting, cold-resistant, anti-electromagnetic interference.
Description
Technical field：
The invention belongs to field of functional materials, it is related to material contracting with heat technology, and in particular to a kind of high temperature resistant electromagnetic shielding heat
The technology of preparing of the draw.
Background technology:
Material contracting with heat is also known as polymer shape memory material.Being heated to the uniform temperature material with thermal source will shrink rapidly
Diminish, its radial shrinkage ratio is finally tightly coated on object outside, and can show and be wrapped by thing up to 50%~80%
The original form of body.Material contracting with heat can play sealing, anti-corrosion, protection against the tide and the effect of continuing etc., in electrician, electric power, communication, stone
The industry extensive uses such as oil, building, household electrical appliances and military project.
The material contracting with heat overwhelming majority in the market be all with PE, PVC, PET, EVA etc. as base-material, through mixing, shaping,
Crosslinking with radiation, heating expansion, cooling and shaping and be made.Chinese patent CN101824181A discloses a kind of magnetically-conductive plastic heat and receives
The preparation method of Heat-Shrinkable Tubings, the mainly method preparation by adding magnetic in EVA, EEA, LDPE, LLDPE or its mixture is led
Magnetic heat-shrinkable T bush, magnetic conduction heat-shrinkable T bush prepared by the method is functional, can carry out effective magnetic screen to electromagnetic element.But
It is that the heat-resisting quantities such as its matrix resin EVA, LDPE are poor, this type shrinkable tube cannot be applied in temperature requirement occasion high.China
Patent CN103772855A describes a kind of composite for preparing electromagnetic shielding conductive heat-shrink tube, with PVC as matrix resin, leads to
Cross addition plating metal graphite powder and prepare shielding heat-shrink tube, although capability of electromagnetic shielding is excellent, but same resistance to elevated temperatures compared with
Difference.
Chinese patent CN101993589A discloses a kind of silicon rubber shrinkable tube, and the basic composition of the heat-shrink tube is silicon rubber
And thermoplastic resin, pyrocondensation mechanism is significantly different with said polyolefins heat-shrink tube, and its pyrocondensation function depends on the resilience of silicon rubber
Interaction between power and the support force of thermoplastic resin, therefore so this heat-shrink tube is not required to crosslinking with radiation, processing technology
It is relatively easy.Because material of main part employs silicon rubber, therefore resistance to elevated temperatures improves, but its thermoplastic for using
Property resin in containing the resin such as EVA, LDPE, so this heat-shrink tube can't for a long time tolerate more than 200 DEG C.In addition, the pyrocondensation
Pipe does not have electro-magnetic screen function, using being restricted.
Not only high temperature resistant was simultaneously but also the heat-shrink tube with electro-magnetic screen function is there is not yet all open reports.
The content of the invention：
The purpose of the present invention is intended to overcome the deficiencies in the prior art, for cable, company that electromagnetic protection is needed under hot environment
Device is connect, the first purpose is to provide a kind of with good stability, high-fire resistance, cold resistance and excellent electromagnetic protection performance
High temperature resistant electromagnetic shielding heat-shrink tube；The second purpose is to provide a kind of high temperature resistant to realize the first purpose and is electromagnetically shielded heat-shrink tube
Preparation method.
An object of the present invention can be achieved by the following technical measures：
High temperature resistant electromagnetic shielding heat-shrink tube is made up of the raw material of following proportion by weight：
An object of the present invention can also be achieved by the following technical measures：
Described silicon rubber is the one kind in methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, fluorosioloxane rubber
Or two kinds with it is any proportioning mix；Described silicon rubber medium vinyl content is 0.03~0.2% weight.
Described thermoplastic resin is methyl silicon resin, vinyl polysiloxane, phenyl polysiloxane, penylene silicones, poly- inclined
One or two in PVF are mixed with any proportioning.
Described reinforcing agent is the fume colloidal silica or precipitated silica processed using HMDS.
Described vulcanizing agent is the one kind or 2 in 2,4- dichlorobenzoperoxides (DCBP), benzoyl peroxide (BP),
4- dichlorobenzoperoxides, benzoyl peroxide match the mixing for mixing with Triallyl isocyanurate (TAIC) with any
Thing.
Described silicone oil is one kind or methyl-silicone oil and vinyl silicone oil in methyl-silicone oil, vinyl silicone oil arbitrarily to match somebody with somebody
Than the mixture for mixing.
Described denatured conductive powder refers to by the treatment of conductive powder body vinyl silicane coupling agent, to improve resin to powder
The affinity of body, so as to increase the addition of powder；Described conductive powder body be silver powder, nickel powder, silver-plated copper powder, silvered aluminum powder,
One or more of silver-plated glass beads, silver-plated nickel powder, Ni-coated graphite with it is any proportioning mixing powder, its shape include but not
It is limited to sheet, spherical and dendroid, average grain diameter is not more than 50 μm.
The described specific processing method of denatured conductive powder is：
In 100~150 mass parts industrial alcohol, the vinyl silicane coupling agent of 0.35~10.9 mass parts is added, then
The conductive powder body for adding 175~543 mass parts average grain diameters to be not more than 50 μm, pours into pallet after stirring 30min and dries.
The second object of the present invention can be achieved by the following technical measures：
The method that high temperature resistant is electromagnetically shielded heat-shrink tube is prepared with the raw material of the above-mentioned first purpose, the preparation method is by following step
Suddenly carry out：
A. it is cold mixed：Take silicon rubber, reinforcing agent and silicone oil to be well mixed in vacuum kneader, then vacuumize 0.5~2h,
Obtain elastomeric compound；
B. heat is mixed：By a steps it is cold it is mixed after elastomeric compound be heated to 150~175 DEG C, add thermoplastic resin, be well mixed,
In two-roll mill slice after taking-up, room temperature is cooled to, obtains sheet elastomeric compound；
C. it is blended：Sheet elastomeric compound of the b step heat after mixed is inserted in two-roll mill, crosslinking agent mixing is subsequently adding equal
It is even, add the blending of denatured conductive powder, slice after mixing is uniform；
D. extrusion vulcanization：Sheet elastomeric compound after step c is blended first is extruded through Teh Extrusion Press for Extruding Silicone Rubber Products, then again through hot empty
The vulcanization sizing of gas drying tunnel, obtains elastic rubber tube；
E. expansion sizing：The elastic rubber tube of Step d is heated to more than the fusing point of thermoplastic resin, it is expanded using external force
, then quenching sizing, obtains product.
The present invention is for cable, the connector that electromagnetic protection is needed under hot environment, there is provided a kind of high temperature resistant electromagnetic shielding heat
The draw, electromagnetic shielding heat-shrink tube of the invention is anti-with good stability, high-fire resistance, cold resistance and excellent electromagnetism
Shield performance, can for a long time tolerate 200 DEG C of high temperature above, can apply to the electricity for having high request to heat-resisting, cold-resistant, anti-electromagnetic interference
Power, electronics industry place.
Specific embodiment：
Technical scheme proposed by the present invention is further described with reference to embodiment, but not as to technical scheme
Limitation.
Embodiment 1:
A. conductive powder body is modified：In 100 mass parts industrial alcohol, the vinyl triethoxyl of 0.35 mass parts is added
Silane (A-151), adds the ball shape silver powder that 175 mass parts average grain diameters are 30 μm, is poured into pallet after stirring 30min and dried
It is standby；
B. it is cold mixed：Methyl vinyl silicone rubber that 100 mass parts contents of ethylene are 0.03%, 30 mass parts are used six
Fume colloidal silica, the 2 mass parts methyl-silicone oils of methyl disilazane treatment are well mixed on banbury, then vacuumize
2h；
C. heat is mixed：By b step it is cold it is mixed after elastomeric compound be heated to 175 DEG C, add the mixing of 50 mass parts methyl silicon resins equal
It is even, in two-roll mill slice after taking-up, it is cooled to room temperature standby；
D. it is blended：Sheet elastomeric compound is first added the 2,4- dichloro benzoyl peroxide first of 1.5 mass parts in two-roll mill
Acyl (DCBP) mixing is uniform, then adds the denatured conductive powder blending of 175 mass parts of a steps, slice after mixing is uniform；
E. extrusion vulcanization：Sheet elastomeric compound after Step d is blended is extruded after being cut into small bar on Teh Extrusion Press for Extruding Silicone Rubber Products, then
Vulcanize through hot-air drying tunnel and shape, be made elastic rubber tube；
F. expansion sizing：The elastic rubber tube of step e is heated to more than 175 DEG C, then expands it, then be quenched sizing.
The heat-shrink tube smooth in appearance, radial shrinkage ratio 55%, the Ω cm of specific insulation 0.097, shield effectiveness after contraction
45~55dB (30MHz~1.5GHz).
Embodiment 2：
A. conductive powder body is modified：In 150 mass parts industrial alcohol, the vinyl triethoxyl of 10.8 mass parts is added
Silane (A-151), adds the ball shape silver powder that 543 mass parts average grain diameters are 50 μm, is poured into pallet after stirring 30min and dried
It is standby；
B. it is cold mixed：Methyl vinyl silicone rubber that 100 mass parts contents of ethylene are 0.2%, 5 mass parts are used into pregnancy
Fume colloidal silica, the 20 mass parts methyl-silicone oils of base disilazane treatment are well mixed on banbury, then vacuumize 2h；
C. heat is mixed：By b step it is cold it is mixed after elastomeric compound be heated to 150 DEG C, add the mixing of 10 mass parts methyl silicon resins equal
It is even, in two-roll mill slice after taking-up, it is cooled to room temperature standby；
D. it is blended：Sheet elastomeric compound is first added the 2,4- dichlorobenzoperoxides of 6 mass parts in two-roll mill
(DCBP) knead uniformly, then add the denatured conductive powder blending of 543 mass parts of a steps, slice after mixing is uniform；
E. extrusion vulcanization：Sheet elastomeric compound after Step d is blended is extruded after being cut into small bar on Teh Extrusion Press for Extruding Silicone Rubber Products, then
Vulcanize through hot-air drying tunnel and shape, be made elastic rubber tube；
F. expansion sizing：The elastic rubber tube of step e is heated to more than 175 DEG C, then expands it, then be quenched sizing.
The heat-shrink tube smooth in appearance, radial shrinkage ratio 50%, the Ω cmcm of specific insulation 0.0012 after contraction, shielding
80~90dB of efficiency (30MHz~1.5GHz).
Embodiment 3：
A. conductive powder body is modified：In 120 mass parts industrial alcohol, the vinyl triethoxyl of 4.5 mass parts is added
Silane (A-151), adds the ball shape silver powder that 360 mass parts average grain diameters are 5 μm, is poured into pallet after stirring 30min and dried
It is standby.
B. it is cold mixed：Methyl vinyl silicone rubber that 100 mass parts contents of ethylene are 0.1%, 15 mass parts are used six
Fume colloidal silica, the 10 mass parts methyl-silicone oils of methyl disilazane treatment are well mixed on banbury, then vacuumize
2h；
C. heat is mixed：By b step it is cold it is mixed after elastomeric compound be heated to 160 DEG C, add the mixing of 30 mass parts methyl silicon resins equal
It is even, in two-roll mill slice after taking-up, it is cooled to room temperature standby；
D. it is blended：Sheet elastomeric compound is first added the 2,4- dichloro benzoyl peroxide first of 4.2 mass parts in two-roll mill
Acyl (DCBP) mixing is uniform, then adds the denatured conductive powder blending of 360 mass parts of a steps, slice after mixing is uniform；
E. extrusion vulcanization：Sheet elastomeric compound after Step d is blended is extruded after being cut into small bar on Teh Extrusion Press for Extruding Silicone Rubber Products, then
Vulcanize through hot-air drying tunnel and shape, be made elastic rubber tube；
F. expansion sizing：The elastic rubber tube of step e is heated to more than 175 DEG C, then expands it, then be quenched sizing.
The heat-shrink tube smooth in appearance, radial shrinkage ratio 53%, the Ω cm of specific insulation 0.0075, shield effectiveness after contraction
65~75dB (30MHz~1.5GHz).
Embodiment 4：
The difference is that replace methyl vinyl silicone rubber with methyl phenyl vinyl silicone rubber, others were same as embodiment 1-
3。
Embodiment 5：
The difference is that replace methyl vinyl silicone rubber with fluorosioloxane rubber, others were same as embodiment 1-3.
Embodiment 6：
The difference is that using two kinds in methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, fluorosioloxane rubber to appoint
Meaning proportioning mixing replaces methyl vinyl silicone rubber, others were same as embodiment 1-3.
Embodiment 7：
The difference is that replace methyl silicon resin with vinyl polysiloxane, others were same as embodiment 1-6.
Embodiment 8：
The difference is that replace methyl silicon resin with phenyl polysiloxane, others were same as embodiment 1-7.
Embodiment 9：
The difference is that replace methyl silicon resin with penylene silicones, others were same as embodiment 1-7.
Embodiment 10：
The difference is that replace methyl silicon resin with Kynoar, others were same as embodiment 1-7.
Embodiment 11：
The difference is that with methyl silicon resin, vinyl polysiloxane, phenyl polysiloxane, penylene silicones, Kynoar
Two kinds with it is any proportioning mixing replace methyl silicon resin, others were same as embodiment 1-7.
Embodiment 12：
The difference is that being replaced with the precipitated silica that HMDS is processed with HMDS treatment
Fume colloidal silica, others were same as embodiment 1-11.
Embodiment 13：
The difference is that replace 2,4- dichlorobenzoperoxides with benzoyl peroxide, others were same as embodiment 1-12.
Embodiment 14：
The difference is that with 2,4- dichlorobenzoperoxides, benzoyl peroxide and Triallyl isocyanurate with any
The mixture of proportioning replaces 2,4- dichlorobenzoperoxides, others were same as embodiment 1-12.
Embodiment 15：
The difference is that replace methyl-silicone oil with vinyl silicone oil, others were same as embodiment 1-14.
Embodiment 16：
The difference is that methyl-silicone oil is replaced with any mixture for mixing that matches with methyl-silicone oil with vinyl silicone oil, other
Respectively with embodiment 1-14.
Embodiment 17：
Unlike replace silver powder with nickel powder, the shape of nickel powder includes but is not limited to sheet, spherical, others were same as implementation
Example 1-16.
Embodiment 18：
The difference is that replacing silver powder with silver-plated copper powder, the shape of silver-plated copper powder includes but is not limited to sheet, spherical and tree
It is dendritic, others were same as embodiment 1-16.
Embodiment 19：
The difference is that replacing the shape of silver powder, silvered aluminum powder to include but is not limited to sheet, spherical, other points with silvered aluminum powder
Not with embodiment 1-16.
Embodiment 20：
The difference is that replacing silver powder with silver-plated glass beads, the shape of silver-plated glass beads is including but not limited to spherical, its
He is respectively with embodiment 1-16.
Embodiment 21：
The difference is that replacing the shape of silver powder, silver-plated nickel powder to include but is not limited to sheet, spherical, other points with silver-plated nickel powder
Not with embodiment 1-16.
Embodiment 22：
The difference is that replace the shape of silver powder, Ni-coated graphite to include but is not limited to sheet with Ni-coated graphite, others were same as
Embodiment 1-16.
Embodiment 23：
The difference is that using silver powder, nickel powder, silver-plated copper powder, silvered aluminum powder, silver-plated glass beads, silver-plated nickel powder, Ni-coated graphite
In it is several with it is any proportioning mixing powders replace silver powder, silver powder, nickel powder, silver-plated copper powder, silvered aluminum powder, silvered glass are micro-
Pearl, silver-plated nickel powder, the shape of Ni-coated graphite include but is not limited to sheet, spherical and dendroid, others were same as embodiment 1-
16。
Claims (1)
1. a kind of high temperature resistant is electromagnetically shielded heat-shrink tube, it is characterised in that it uses the raw material of following proportion by weight：
The reinforcing agent 5~30 of 100 thermoplastic resin of silicon rubber 10~50
The denatured conductive powder 175~543 of 1.5~6 silicone oil of vulcanizing agent 2~20；
Described silicon rubber is the one kind or two in methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, fluorosioloxane rubber
Plant and mixed with any proportioning, described silicon rubber medium vinyl content is 0.03~0.2% weight；
Described thermoplastic resin is methyl silicon resin, vinyl polysiloxane, phenyl polysiloxane, penylene silicones, polyvinylidene fluoride
One or two in alkene are mixed with any proportioning；
Described reinforcing agent is the fume colloidal silica or precipitated silica processed using HMDS；
Described vulcanizing agent is one kind or 2,4- dichloro benzoyl peroxides in 2,4- dichlorobenzoperoxides, benzoyl peroxide
Formyl, benzoyl peroxide match the mixture for mixing with Triallyl isocyanurate with any；
Described silicone oil is that one kind or methyl-silicone oil and vinyl silicone oil in methyl-silicone oil, vinyl silicone oil are mixed with any proportioning
The mixture of conjunction；
Described conductive powder body is silver powder, nickel powder, silver-plated copper powder, silvered aluminum powder, silver-plated glass beads, silver-plated nickel powder, nickel plating stone
One or more of ink include but is not limited to sheet, spherical and dendroid with the powder of any proportioning mixing, its shape；
It is made as follows：
A. it is cold mixed：Take silicon rubber, reinforcing agent and silicone oil to be well mixed in vacuum kneader, then vacuumize 0.5~2h, obtain mixed
Refining glue；
B. heat is mixed：By a steps it is cold it is mixed after elastomeric compound be heated to 150~175 DEG C, add thermoplastic resin, be well mixed, take out
Afterwards in two-roll mill slice, room temperature is cooled to, obtains sheet elastomeric compound；
C. it is blended：Sheet elastomeric compound of the b step heat after mixed is inserted in two-roll mill, crosslinking agent mixing is subsequently adding uniformly,
Add the blending of denatured conductive powder, slice after mixing is uniform；
D. extrusion vulcanization：Sheet elastomeric compound after step c is blended first is extruded through Teh Extrusion Press for Extruding Silicone Rubber Products, is then dried through hot-air again
Road vulcanization sizing, obtains elastic rubber tube；
E. expansion sizing：The elastic rubber tube of Step d is heated to more than the fusing point of thermoplastic resin, it is expanded using external force,
Then quenching sizing, obtains product.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104962079A (en) * | 2015-06-02 | 2015-10-07 | 苏州市大力电器有限公司 | Excellent-mildew resistance outer rubber pipe for hydraulic oil pipe |
| CN104960101A (en) * | 2015-06-02 | 2015-10-07 | 苏州市大力电器有限公司 | Preparation method of excellent-mildew resistance outer rubber pipe for hydraulic oil pipe |
| CN106349715A (en) * | 2016-08-23 | 2017-01-25 | 杨子妹 | High-strength wear-resistant silicone rubber material for high pressure rubber pipe |
| CN107973973A (en) * | 2017-12-24 | 2018-05-01 | 广州宝之泰电子科技有限公司 | One kind electromagnetic shielding high fire-retardance ethylene-ethyl acrylate copolymer thermal contraction casing tube and preparation method thereof |
| CN110922762A (en) * | 2019-10-23 | 2020-03-27 | 平湖阿莱德实业有限公司 | High-conductivity silica gel composition based on conductive powder wet modification technology |
| CN112812564B (en) * | 2021-01-05 | 2022-06-03 | 河北兹尔新材料科技有限公司 | High-temperature-resistant silica gel sleeve and preparation method thereof |
| CN116021815B (en) * | 2022-12-27 | 2023-07-07 | 义博通信设备集团股份有限公司 | High-adaptability cold shrink tube preparation processing method |
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| CN102153869A (en) * | 2011-05-18 | 2011-08-17 | 天津大学 | Low-density high-strength conductive rubber and preparation method thereof |
| CN102942792A (en) * | 2012-12-04 | 2013-02-27 | 四川明星电缆股份有限公司 | Semiconductive silicon rubber screening material for traveling cable and preparation method thereof |
| CN103436023A (en) * | 2013-08-31 | 2013-12-11 | 青岛承天伟业机械制造有限公司 | Novel conductive rubber |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153869A (en) * | 2011-05-18 | 2011-08-17 | 天津大学 | Low-density high-strength conductive rubber and preparation method thereof |
| CN102942792A (en) * | 2012-12-04 | 2013-02-27 | 四川明星电缆股份有限公司 | Semiconductive silicon rubber screening material for traveling cable and preparation method thereof |
| CN103436023A (en) * | 2013-08-31 | 2013-12-11 | 青岛承天伟业机械制造有限公司 | Novel conductive rubber |
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