CN104448837A - High-temperature-resistant electromagnetic shielding heat-shrinkable tube and preparation method thereof - Google Patents
High-temperature-resistant electromagnetic shielding heat-shrinkable tube and preparation method thereof Download PDFInfo
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- CN104448837A CN104448837A CN201410783089.3A CN201410783089A CN104448837A CN 104448837 A CN104448837 A CN 104448837A CN 201410783089 A CN201410783089 A CN 201410783089A CN 104448837 A CN104448837 A CN 104448837A
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Abstract
The invention provides a high-temperature-resistant electromagnetic shielding heat-shrinkable tube which consists of the following raw materials in parts by mass: 100 parts of silicon rubber, 10-50 parts of thermoplastic resin, 5-30 parts of a reinforcing agent, 1.5-6 parts of a curing agent, 2-20 parts of silicon oil and 175-543 parts of modified conductive powder. The high-temperature-resistant electromagnetic shielding heat-shrinkable tube is used for cables and connectors requiring electromagnetic protection in a high-temperature environment. Meanwhile, the invention also provides a method for processing the heat-shrinkable tube by using the materials, and the method specifically comprises the steps of cold mixing, hot mixing, blending, extrusion vulcanization and expansion shaping. The heat-shrinkable tube prepared by the method provided by the invention has very good stability, high heat resistance and cold resistance and excellent electromagnetic protection performance, can endure high temperatures of over 200 DEG C for a long time, and can be applied to electric power and electronic industry places with high requirements on heat resistance, cold resistance and electromagnetic interference prevention.
Description
Technical field:
The invention belongs to field of functional materials, relate to material contracting with heat technology, be specifically related to a kind of technology of preparing of high temperature resistant electromagnetic shielding heat-shrink tube.
Background technology:
Material contracting with heat is also known as polymer shape memory material.Will to shrink rapidly to this material of certain temperature with heat source and diminish, its radial shrinkage ratio can reach 50% ~ 80%, is finally coated on outside object tightly, and can show the original form being wrapped by object.Material contracting with heat can play sealing, anticorrosion, the moistureproof and effect such as to continue, in industry widespread uses such as electrician, electric power, communication, oil, building, household electrical appliances and military projects.
The material contracting with heat overwhelming majority is in the market with PE, PVC, PET, EVA etc. for base-material, through mixing, shaping, radiation crosslinking, add thermal enlargement, cooling and shaping is made.Chinese patent CN101824181A discloses a kind of preparation method of magnetically-conductive plastic heat-shrinkable sleeve, method mainly through adding magnetic in EVA, EEA, LDPE, LLDPE or its mixture prepares magnetic conduction heat-shrinkable T bush, the standby magnetic conduction heat-shrinkable T bush of this legal system is functional, can carry out effective magnetic shielding to electromagnetic element.But the high thermal resistancies such as its matrix resin EVA, LDPE are poor, and this type shrinkable tube cannot be applied in the high occasion of temperature requirement.Chinese patent CN103772855A describes a kind of matrix material preparing electromagnetic shielding conductive heat-shrink tube, take PVC as matrix resin, prepare shielding heat-shrink tube by adding metallizing Graphite Powder 99, although capability of electromagnetic shielding is excellent, same resistance to elevated temperatures is poor.
Chinese patent CN101993589A discloses a kind of silicon rubber shrinkable tube, the essentially consist of this heat-shrink tube is silicon rubber and thermoplastic resin, pyrocondensation mechanism is obviously different from said polyolefins heat-shrink tube, its pyrocondensation function depends on the interaction between the screen resilience of silicon rubber and the anchorage force of thermoplastic resin, therefore so this heat-shrink tube does not need radiation crosslinking, complete processing is relatively simple.Because material of main part have employed silicon rubber, therefore resistance to elevated temperatures improves, but containing resins such as EVA, LDPE in its thermoplastic resin adopted, so this heat-shrink tube can't withstand long term exposure more than 200 DEG C.In addition, this heat-shrink tube does not have electro-magnetic screen function, and application is restricted.
The while of not only high temperature resistant but the heat-shrink tube with electro-magnetic screen function there is not yet all open reports.
Summary of the invention:
Object of the present invention is intended to overcome the deficiencies in the prior art, for the cable, the junctor that need electromagnetic protection under hot environment, one of object is to provide a kind of high temperature resistant electromagnetic shielding heat-shrink tube with the electromagnetic protection performance of good stability, high heat resistance, winter hardiness and excellence; Two of object is to provide a kind of preparation method of the high temperature resistant electromagnetic shielding heat-shrink tube for realizing one of object.
An object of the present invention realizes by following technical measures:
This is high temperature resistant, and electromagnetic shielding heat-shrink tube is made up of the raw material of following proportion by weight:
An object of the present invention also realizes by following technical measures:
Described silicon rubber is that one or both in methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, trifluoropropyl siloxane mix with any proportioning; Described silicon rubber medium vinyl content is 0.03 ~ 0.2% weight.
Described thermoplastic resin is methyl silicon resin, one or both in vinyl polysiloxane, phenyl polysiloxane, penylene silicone resin, polyvinylidene difluoride (PVDF) mix with any proportioning.
Described strengthening agent is the thermal silica or the precipitated silica that adopt hexamethyldisilazane process.
Described vulcanizing agent is 2, the mixture that one in 4-dichlorobenzoperoxide (DCBP), benzoyl peroxide (BP) or 2,4-dichlorobenzoperoxide, benzoyl peroxide mix with any proportioning with cyanacrylate (TAIC).
Described silicone oil is the mixture that a kind of or methyl-silicone oil in methyl-silicone oil, vinyl silicone oil mixes with any proportioning with vinyl silicone oil.
Described denatured conductive powder refers to the process of conductive powder body vinyl silicane coupling agent, to improve the affinity of resin to powder, thus increases the addition of powder; Described conductive powder body is one or more powders mixed with any proportioning of silver powder, nickel powder, silver-plated copper powder, silvered aluminum powder, silver-plated glass beads, silver-plated nickel powder, Ni-coated graphite, its shape includes but not limited to sheet, spherical and dendroid, and median size is not more than 50 μm.
The described concrete treatment process of denatured conductive powder is:
In 100 ~ 150 mass parts industrial spirit, add the vinyl silicane coupling agent of 0.35 ~ 10.9 mass parts, then add the conductive powder body that 175 ~ 543 mass parts median sizes are not more than 50 μm, pour in pallet after stirring 30min and dry.
Two of object of the present invention realizes by following technical measures:
Prepare the method for high temperature resistant electromagnetic shielding heat-shrink tube with the raw material of one of above-mentioned purpose, this preparation method carries out as follows:
A. cold mixed: to get silicon rubber, strengthening agent and silicone oil and mix in vacuum kneader, then vacuumize 0.5 ~ 2h, obtain rubber unvulcanizate;
B. heat is mixed: the rubber unvulcanizate after cold for a step mixing is heated to 150 ~ 175 DEG C, and add thermoplastic resin, mix, in two roller mill slice after taking-up, cool to room temperature, obtains sheet rubber unvulcanizate;
C. blended: to be inserted in two roller mill by the sheet rubber unvulcanizate after mixed for b step heat, it is evenly mixing then to add linking agent, then it is blended to add denatured conductive powder, mixing evenly after slice;
D. extrude sulfuration: the sheet rubber unvulcanizate after step c is blended is first extruded through Teh Extrusion Press for Extruding Silicone Rubber Products, and then through warm air drying tunnel sulfuration sizing, obtain elastic rubber tube;
E. expand sizing: the elastic rubber tube of Step d is heated to more than the fusing point of thermoplastic resin, use external force to make it expand, then quenching sizing, obtains product.
The cable of electromagnetic protection, junctor is needed under the present invention is directed to hot environment, a kind of high temperature resistant electromagnetic shielding heat-shrink tube is provided, electromagnetic shielding heat-shrink tube of the present invention, there is the electromagnetic protection performance of good stability, high heat resistance, winter hardiness and excellence, energy withstand long term exposure more than 200 DEG C high temperature, can be applied to the electric power, the electronic industry place that heat-resisting, cold-resistant, anti-electromagnetic interference are had to high request.
Embodiment:
Below in conjunction with embodiment, the technical scheme that the present invention proposes is further described, but not as the restriction to technical scheme.
Embodiment 1:
A. the modification of conductive powder body: in 100 mass parts industrial spirit, add the vinyltriethoxysilane (A-151) of 0.35 mass parts, add the ball shape silver powder that 175 mass parts median sizes are 30 μm again, stir to pour in pallet after 30min dry for subsequent use;
B. cold mixed: to be the methyl vinyl silicone rubber of 0.03% by 100 mass parts contents of ethylene, 30 mass parts adopt the thermal silica of hexamethyldisilazane process, 2 mass parts methyl-silicone oils mix on Banbury mixer, then vacuumize 2h;
C. heat is mixed: the rubber unvulcanizate after cold for b step mixing is heated to 175 DEG C, and add 50 mass parts methyl silicon resins and mix, in two roller mill slice after taking-up, cool to room temperature is for subsequent use;
D. blended: 2, the 4-dichlorobenzoperoxides (DCBP) sheet rubber unvulcanizate first being added 1.5 mass parts in two roller mill are evenly mixing, and then the denatured conductive powder of 175 mass parts adding a step is blended, mixing evenly rear slice;
E. extrude sulfuration: extrude on Teh Extrusion Press for Extruding Silicone Rubber Products after the sheet rubber unvulcanizate after Step d is blended is cut into little bar, then through warm air drying tunnel sulfuration sizing, make elastic rubber tube;
F. expand sizing: the elastic rubber tube of step e is heated to more than 175 DEG C, then make it expand, then quenching sizing.
This heat-shrink tube smooth in appearance, radial shrinkage ratio 55%, volume specific resistance 0.097 Ω cm, effectiveness of shielding 45 ~ 55dB (30MHz ~ 1.5GHz) after shrinking.
Embodiment 2:
A. the modification of conductive powder body: in 150 mass parts industrial spirit, add the vinyltriethoxysilane (A-151) of 10.8 mass parts, add the ball shape silver powder that 543 mass parts median sizes are 50 μm again, stir to pour in pallet after 30min dry for subsequent use;
B. cold mixed: to be the methyl vinyl silicone rubber of 0.2% by 100 mass parts contents of ethylene, 5 mass parts adopt the thermal silica of hexamethyldisilazane process, 20 mass parts methyl-silicone oils mix on Banbury mixer, then vacuumize 2h;
C. heat is mixed: the rubber unvulcanizate after cold for b step mixing is heated to 150 DEG C, and add 10 mass parts methyl silicon resins and mix, in two roller mill slice after taking-up, cool to room temperature is for subsequent use;
D. blended: 2, the 4-dichlorobenzoperoxides (DCBP) sheet rubber unvulcanizate first being added 6 mass parts in two roller mill are evenly mixing, and then the denatured conductive powder of 543 mass parts adding a step is blended, mixing evenly rear slice;
E. extrude sulfuration: extrude on Teh Extrusion Press for Extruding Silicone Rubber Products after the sheet rubber unvulcanizate after Step d is blended is cut into little bar, then through warm air drying tunnel sulfuration sizing, make elastic rubber tube;
F. expand sizing: the elastic rubber tube of step e is heated to more than 175 DEG C, then make it expand, then quenching sizing.
This heat-shrink tube smooth in appearance, radial shrinkage ratio 50%, volume specific resistance 0.0012 Ω cmcm, effectiveness of shielding 80 ~ 90dB (30MHz ~ 1.5GHz) after shrinking.
Embodiment 3:
A. the modification of conductive powder body: in 120 mass parts industrial spirit, add the vinyltriethoxysilane (A-151) of 4.5 mass parts, add the ball shape silver powder that 360 mass parts median sizes are 5 μm again, stir to pour in pallet after 30min dry for subsequent use.
B. cold mixed: to be the methyl vinyl silicone rubber of 0.1% by 100 mass parts contents of ethylene, 15 mass parts adopt the thermal silica of hexamethyldisilazane process, 10 mass parts methyl-silicone oils mix on Banbury mixer, then vacuumize 2h;
C. heat is mixed: the rubber unvulcanizate after cold for b step mixing is heated to 160 DEG C, and add 30 mass parts methyl silicon resins and mix, in two roller mill slice after taking-up, cool to room temperature is for subsequent use;
D. blended: 2, the 4-dichlorobenzoperoxides (DCBP) sheet rubber unvulcanizate first being added 4.2 mass parts in two roller mill are evenly mixing, and then the denatured conductive powder of 360 mass parts adding a step is blended, mixing evenly rear slice;
E. extrude sulfuration: extrude on Teh Extrusion Press for Extruding Silicone Rubber Products after the sheet rubber unvulcanizate after Step d is blended is cut into little bar, then through warm air drying tunnel sulfuration sizing, make elastic rubber tube;
F. expand sizing: the elastic rubber tube of step e is heated to more than 175 DEG C, then make it expand, then quenching sizing.
This heat-shrink tube smooth in appearance, radial shrinkage ratio 53%, volume specific resistance 0.0075 Ω cm, effectiveness of shielding 65 ~ 75dB (30MHz ~ 1.5GHz) after shrinking.
Embodiment 4:
Methyl vinyl silicone rubber is replaced, others were same as embodiment 1-3 unlike with methyl phenyl vinyl silicone rubber.
Embodiment 5:
Methyl vinyl silicone rubber is replaced, others were same as embodiment 1-3 unlike with trifluoropropyl siloxane.
Embodiment 6:
Methyl vinyl silicone rubber is replaced, others were same as embodiment 1-3 with any proportioning mixing unlike with two in methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, trifluoropropyl siloxane kind.
Embodiment 7:
Methyl silicon resin is replaced, others were same as embodiment 1-6 unlike with vinyl polysiloxane.
Embodiment 8:
Methyl silicon resin is replaced, others were same as embodiment 1-7 unlike with phenyl polysiloxane.
Embodiment 9:
Methyl silicon resin is replaced, others were same as embodiment 1-7 unlike with penylene silicone resin.
Embodiment 10:
Methyl silicon resin is replaced, others were same as embodiment 1-7 unlike with polyvinylidene difluoride (PVDF).
Embodiment 11:
Methyl silicon resin is replaced, others were same as embodiment 1-7 with any proportioning mixing unlike with two kinds in methyl silicon resin, vinyl polysiloxane, phenyl polysiloxane, penylene silicone resin, polyvinylidene difluoride (PVDF).
Embodiment 12:
Unlike the thermal silica of the precipitated silica replacement hexamethyldisilazane process with hexamethyldisilazane process, others were same as embodiment 1-11.
Embodiment 13:
2,4-dichlorobenzoperoxide is replaced, others were same as embodiment 1-12 unlike with benzoyl peroxide.
Embodiment 14:
2,4-dichlorobenzoperoxide is replaced, others were same as embodiment 1-12 with the mixture of any proportioning unlike with 2,4-dichlorobenzoperoxide, benzoyl peroxide and cyanacrylate.
Embodiment 15:
Methyl-silicone oil is replaced, others were same as embodiment 1-14 unlike with vinyl silicone oil.
Embodiment 16:
Methyl-silicone oil is replaced, others were same as embodiment 1-14 unlike the mixture mixed with any proportioning with methyl-silicone oil and vinyl silicone oil.
Embodiment 17:
Replace silver powder unlike with nickel powder, the shape of nickel powder includes but not limited to sheet, spherical, others were same as embodiment 1-16.
Embodiment 18:
Replace silver powder unlike with silver-plated copper powder, the shape of silver-plated copper powder includes but not limited to sheet, spherical and dendroid, others were same as embodiment 1-16.
Embodiment 19:
Replace silver powder unlike with silvered aluminum powder, the shape of silvered aluminum powder includes but not limited to sheet, spherical, others were same as embodiment 1-16.
Embodiment 20:
Replace silver powder unlike with silver-plated glass beads, the shape of silver-plated glass beads includes but not limited to spherical, others were same as embodiment 1-16.
Embodiment 21:
Replace silver powder unlike with silver-plated nickel powder, the shape of silver-plated nickel powder includes but not limited to sheet, spherical, others were same as embodiment 1-16.
Embodiment 22:
Replace silver powder unlike with Ni-coated graphite, the shape of Ni-coated graphite includes but not limited to sheet, others were same as embodiment 1-16.
Embodiment 23:
Silver powder is replaced unlike with several powders mixed with any proportioning in silver powder, nickel powder, silver-plated copper powder, silvered aluminum powder, silver-plated glass beads, silver-plated nickel powder, Ni-coated graphite, the shape of silver powder, nickel powder, silver-plated copper powder, silvered aluminum powder, silver-plated glass beads, silver-plated nickel powder, Ni-coated graphite includes but not limited to sheet, spherical and dendroid, others were same as embodiment 1-16.
Claims (9)
1. a high temperature resistant electromagnetic shielding heat-shrink tube, is characterized in that it is made up of the raw material of following proportion by weight:
Silicon rubber 100 thermoplastic resin 10 ~ 50 strengthening agent 5 ~ 30
Vulcanizing agent 1.5 ~ 6 silicone oil 2 ~ 20 denatured conductive powder 175 ~ 543.
2. the high temperature resistant electromagnetic shielding heat-shrink tube of one according to claim 1, is characterized in that described silicon rubber is that one or both in methyl vinyl silicone rubber, methyl phenyl vinyl silicone rubber, trifluoropropyl siloxane mix with any proportioning.
3. the high temperature resistant electromagnetic shielding heat-shrink tube of one according to claim 2, is characterized in that described silicon rubber medium vinyl content is 0.03 ~ 0.2% weight.
4. the high temperature resistant electromagnetic shielding heat-shrink tube of one according to claim 1, is characterized in that described thermoplastic resin is methyl silicon resin, one or both in vinyl polysiloxane, phenyl polysiloxane, penylene silicone resin, polyvinylidene difluoride (PVDF) mixes with any proportioning.
5. the high temperature resistant electromagnetic shielding heat-shrink tube of one according to claim 1, is characterized in that described strengthening agent is the thermal silica or the precipitated silica that adopt hexamethyldisilazane process.
6. the high temperature resistant electromagnetic shielding heat-shrink tube of one according to claim 1, it is characterized in that described vulcanizing agent is 2, the mixture that one in 4-dichlorobenzoperoxide, benzoyl peroxide or 2,4-dichlorobenzoperoxide, benzoyl peroxide mix with any proportioning with cyanacrylate.
7. the high temperature resistant electromagnetic shielding heat-shrink tube of one according to claim 1, is characterized in that described silicone oil is the mixture that a kind of or methyl-silicone oil in methyl-silicone oil, vinyl silicone oil mixes with any proportioning with vinyl silicone oil.
8. the high temperature resistant electromagnetic shielding heat-shrink tube of one according to claim 7, it is characterized in that described conductive powder body is one or more powders mixed with any proportioning of silver powder, nickel powder, silver-plated copper powder, silvered aluminum powder, silver-plated glass beads, silver-plated nickel powder, Ni-coated graphite, its shape includes but not limited to sheet, spherical and dendroid.
9. prepare a method for high temperature resistant electromagnetic shielding heat-shrink tube with raw material according to claim 1, it is characterized in that this preparation method carries out as follows:
A. cold mixed: to get silicon rubber, strengthening agent and silicone oil and mix in vacuum kneader, then vacuumize 0.5 ~ 2h, obtain rubber unvulcanizate;
B. heat is mixed: the rubber unvulcanizate after cold for a step mixing is heated to 150 ~ 175 DEG C, and add thermoplastic resin, mix, in two roller mill slice after taking-up, cool to room temperature, obtains sheet rubber unvulcanizate;
C. blended: to be inserted in two roller mill by the sheet rubber unvulcanizate after mixed for b step heat, it is evenly mixing then to add linking agent, then it is blended to add denatured conductive powder, mixing evenly after slice;
D. extrude sulfuration: the sheet rubber unvulcanizate after step c is blended is first extruded through Teh Extrusion Press for Extruding Silicone Rubber Products, and then through warm air drying tunnel sulfuration sizing, obtain elastic rubber tube;
E. expand sizing: the elastic rubber tube of Step d is heated to more than the fusing point of thermoplastic resin, use external force to make it expand, then quenching sizing, obtains product.
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Cited By (7)
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| 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 |
| CN112812564A (en) * | 2021-01-05 | 2021-05-18 | 河北兹尔新材料科技有限公司 | High-temperature-resistant silica gel sleeve and preparation method thereof |
| CN116021815A (en) * | 2022-12-27 | 2023-04-28 | 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 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| 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 |
| CN112812564A (en) * | 2021-01-05 | 2021-05-18 | 河北兹尔新材料科技有限公司 | High-temperature-resistant silica gel sleeve and preparation method thereof |
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| CN116021815A (en) * | 2022-12-27 | 2023-04-28 | 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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