CN109517367B - Conductive thermoplastic dynamic vulcanized silicone rubber and preparation method thereof - Google Patents
Conductive thermoplastic dynamic vulcanized silicone rubber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses conductive thermoplastic dynamic vulcanized silicone rubber and a preparation method thereof. The conductive thermoplastic dynamic vulcanized silicone rubber is prepared from the following raw materials: thermoplastic polyurethane elastomer, silicon rubber compound, conductive filler, cross-linking agent, compatilizer and catalyst. Also discloses a dynamic vulcanization preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber. The conductive thermoplastic dynamic vulcanized silicone rubber prepared by the invention has the characteristics of good conductivity, comfortable hand feeling, recoverability, excellent mechanical property and the like, and can be widely applied to the fields of electronics, electrics, automobiles, war industry, communication and the like.
Description
Technical Field
The invention relates to conductive thermoplastic dynamic vulcanized silicone rubber and a preparation method thereof.
Background
Dynamic vulcanization is a new rubber vulcanization technology, and is a process of melting and blending unvulcanized rubber and a thermoplastic material under the action of high shear, and simultaneously adding a vulcanizing agent to vulcanize the unvulcanized rubber and the thermoplastic material. In this process, the thermoset rubber phase (dispersed phase) is uniformly dispersed in the thermoplastic material (continuous phase) in a certain particle size range, and the rubber phase particles are crosslinked, finally obtaining thermoplastic dynamic vulcanizate (TPV). The main characteristic of dynamic vulcanization is that the rubber phase which is thermosetting is loaded in the thermoplastic material, so that the characteristics of the thermosetting rubber and the thermoplastic plastic are combined, and the processing and recycling of the material are facilitated.
The thermoplastic polyurethane elastomer (TPU) is a thermoplastic elastomer with excellent performance, is polymerized by isocyanate and polyalcohol, has excellent mechanical property, oil resistance and wear resistance, but has poor weather resistance and processability.
The silicone rubber is rubber with a main chain formed by alternating silicon and oxygen atoms, and two organic groups are connected to the silicon atoms, so that the silicone rubber has comfortable hand feeling and good weather resistance, can keep stable mechanical property at the temperature of between 40 ℃ below zero and 200 ℃, and keeps certain toughness, resilience and hardness.
The conductive polymer material is a polymer material with conductivity, and compared with the traditional metal conductive material, the conductive polymer material has the advantages of small density, controllable conductivity, easiness in processing, low cost and the like, and can be used in the fields of sensors, electromagnetic shielding and the like. Meanwhile, the conductive polymer material also has the defects of rough hand feeling, poor mechanical property, unstable quality and the like.
Therefore, the TPU and the silicon rubber are combined together and are endowed with the conductive characteristic, so that the problems can be effectively solved. In the prior literature, US4500688 and CN106751736A both prepare TPU/silicone rubber thermoplastic elastomers through different dynamic vulcanization systems, but the preparation of conductive type thermoplastic dynamic vulcanized silicone rubber is not further studied. CN104098795A obtains a conductive thermoplastic elastomer by simply blending thermoplastic, rubber particles and conductive filler, but the advanced process of dynamic vulcanization is not adopted, and the properties of the prepared product can not well meet the actual use requirements.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the conductive thermoplastic dynamic vulcanized silicone rubber with good conductivity, recoverability and excellent mechanical property by using a dynamic vulcanization method and the preparation method thereof. According to the invention, the thermoplastic dynamic vulcanized silicone rubber with the conductive characteristic is prepared in one step through dynamic vulcanization, and the obtained product has silky handfeel and excellent mechanical property and conductivity.
The technical scheme adopted by the invention is as follows:
the conductive thermoplastic dynamic vulcanized silicone rubber is prepared from the following raw materials in parts by mass: 30-70 parts of thermoplastic polyurethane elastomer, 30-70 parts of silicone rubber compound, 1-30 parts of conductive filler, 1-5 parts of cross-linking agent, 5-20 parts of compatilizer and 0.01-0.5 part of catalyst.
Preferably, in the conductive thermoplastic dynamic vulcanized silicone rubber, the thermoplastic polyurethane elastomer is at least one of polyether TPU and polyester TPU.
Preferably, in the conductive thermoplastic dynamic vulcanized silicone rubber, the shore hardness of the thermoplastic polyurethane elastomer is 60A-95A.
Preferably, in the conductive thermoplastic dynamic silicon sulfide rubber, the silicon rubber compound is white carbon black reinforced methyl vinyl silicone rubber (or called methyl vinyl raw rubber); more preferably, the method for reinforcing the methyl vinyl silicone rubber crude rubber by the white carbon black is a gas phase method or a precipitation method.
Preferably, the conductive thermoplastic dynamic silicon sulfide rubber has a vinyl molar content of 0.04-0.5% in the silicon rubber compound.
Preferably, in the conductive thermoplastic dynamic silicon sulfide rubber, the conductive filler is at least one of carbon black, carbon fiber, graphite powder, graphene, carbon nano tube, hard carbon, carbon microsphere, silver powder, nickel powder and copper powder; more preferably, the conductive filler is at least one of carbon black, carbon fiber, graphite powder, silver powder, nickel powder and copper powder.
Preferably, in the conductive thermoplastic dynamic silicon sulfide rubber, the particle size of the conductive filler is 0.1-40 μm.
Preferably, in the conductive thermoplastic dynamic silicon sulfide rubber, the cross-linking agent is siloxane containing Si-H bonds; more preferably, the cross-linking agent is hydrogen-containing silicone oil, and the molar content of Si-H bonds in the cross-linking agent is 0.4-2%.
Preferably, in the conductive thermoplastic dynamic vulcanized silicone rubber, the compatilizer is at least one of ethylene acrylic acid copolymer (EAA), ethylene methyl acrylate copolymer (EMA) and ethylene vinyl acetate copolymer (EVA).
Preferably, in the conductive thermoplastic dynamic vulcanized silicone rubber, the catalyst is a platinum catalyst; further, the platinum-based catalyst is selected from metallic platinum, platinum black, a platinum-supported catalyst, or a platinum-containing alloy.
The preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber comprises the following steps:
1) in an internal mixer or an extruder, melting and blending the thermoplastic polyurethane elastomer, the silicone rubber compound, the conductive filler, the cross-linking agent and the compatilizer, extruding and granulating to obtain a premix;
2) and mixing the premix with a catalyst, adding the mixture into a double-screw extruder to perform dynamic vulcanization reaction, extruding and granulating to obtain the conductive thermoplastic dynamic vulcanized silicone rubber.
Preferably, in step 1) of the preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber, the melt blending process parameters are as follows: the temperature is 160-200 ℃, the time is 3-10 min, and the rotating speed is 30-100 r/min.
Preferably, in step 2) of the preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber, the process parameters of the twin-screw extruder are as follows: the processing temperature is 170-210 ℃, the screw rotating speed is 200-320 r/min, and the dynamic vulcanization reaction time is 1-4 min.
The invention has the beneficial effects that:
the conductive thermoplastic dynamic vulcanized silicone rubber prepared by the invention has the characteristics of good conductivity, comfortable hand feeling, recoverability, excellent mechanical property and the like, and can be widely applied to the fields of electronics, electrics, automobiles, war industry, communication and the like.
Compared with the prior art, the invention has the following advantages:
1) according to the invention, through a dynamic vulcanization technology, dynamic crosslinking of the silicon rubber in a thermoplastic polyurethane elastomer melt is realized under the action of high-temperature shearing in the extrusion process, uniform dispersion of the conductive filler in a polymer is realized, the conductivity of the material is improved, and the performance loss caused by repeated processing of the dynamic vulcanized silicon rubber for realizing functionalization is avoided.
2) The invention realizes the thermodynamic compatibility of the thermoplastic polyurethane elastomer with larger polarity difference and the silicon rubber by adding the compatilizer, and simultaneously realizes the thermodynamic compatibility of an organic high polymer material phase and an inorganic conductive material phase, so that the prepared conductive thermoplastic dynamic silicon sulfide rubber has excellent mechanical property (the tensile strength can reach 20MPa) and conductive property (the volume resistivity can reach 0.1 omega cm).
3) The raw materials and processing equipment used in the invention are common industrial raw materials and equipment, are convenient to use and low in cost, can realize large-scale industrial production, have no solvent or toxic volatile gas pollution, meet the requirements of environmental protection, and have practical significance.
Detailed Description
The present invention will be described in further detail with reference to specific examples, which should not be construed as limiting the scope of the present invention. The starting materials/equipment used in the examples were all available from conventional commercial sources unless otherwise specified. The methods for detecting the performance parameters of the silicone rubber are standard test methods known in the art unless otherwise specified.
Examples 1 to 3 and comparative example 1
The compositions of the silicone rubbers of examples 1 to 3 and comparative example 1 are shown in table 1, and the compositions described in table 1 are all parts by mass.
TABLE 1 Silicone rubber compositions of examples 1-3 and comparative example 1
The preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber of the embodiments 1 to 3 is as follows:
step one), adding a thermoplastic polyurethane elastomer (TPU), a silicone rubber compound, a compatilizer, a crosslinking agent and a conductive filler in a formula shown in Table 1 into an internal mixer, setting the temperature at 170 ℃, the rotating speed at 40rpm, and the internal mixing time for 5min, and extruding and granulating to obtain a premix. The thermoplastic polyurethane elastomer used in examples 1 to 3 was WHT-8285 (polyether) from Wanhua chemical company, the silicone rubber compound was EN-5150A from Dongjue organosilicon company, the compatibilizer was EVA, the crosslinking agent was hydrogen-containing silicone oil from Dow Corning company, the model was JHF-901, the platinum catalyst was RD7 platinum catalyst from Dow Corning company, and the particle size of the selected conductive filler was 40 μm.
And step two), adding the premix obtained in the step one into a catalyst platinum in a formula shown in Table 1, uniformly mixing, adding into a double-screw extruder, setting the temperature at 190 ℃ and the rotating speed of screws at 250rpm, carrying out dynamic vulcanization reaction for 2min, and extruding and granulating to obtain the conductive thermoplastic dynamic vulcanized silicone rubber. The obtained conductive thermoplastic dynamic vulcanized silicone rubber has uniform appearance and comfortable hand feeling.
The silicone rubber of comparative example 1 was prepared as follows:
according to the process parameters of examples 1-3, but without adding a cross-linking agent and a catalyst, the formulations in table 1 were prepared by a non-dynamic vulcanization method to obtain samples.
The performance parameters of examples 1-3 and comparative example 1 are shown in Table 2.
TABLE 2 Silicone rubber Performance parameters for examples 1-3 and comparative example 1
As can be seen by comparison, the conductivity of examples 1-3 prepared by dynamic vulcanization is not much different from that of comparative example 1 prepared by non-dynamic vulcanization, but the mechanical properties of the conductive rubber are obviously better than those of comparative example 1.
Examples 4 to 6 and comparative example 2
The compositions of the silicone rubbers of examples 4 to 6 and comparative example 2 are shown in table 3, and the compositions described in table 3 are all parts by mass.
TABLE 3 Silicone rubber compositions for examples 4-6 and comparative example 2
The preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber of the embodiment 4-6 comprises the following steps:
step one), adding a thermoplastic polyurethane elastomer (TPU), a silicone rubber compound, a compatilizer, a crosslinking agent and a conductive filler in a formula shown in Table 3 into an internal mixer, setting the temperature at 180 ℃, the rotating speed at 60rpm, and the internal mixing time for 7min, and extruding and granulating to obtain a premix. The thermoplastic polyurethane elastomer used in examples 4 to 6 was S-185ALL (polyester) from Taiwan Queen corporation, the silicone rubber compound was EN-8151 from Dongjue Silicone corporation, the compatibilizer was ethylene acrylic acid copolymer (EAA), the crosslinking agent was hydrogen-containing silicone oil from Dow Corning corporation, model number was JHF-901, the platinum catalyst was RD7 platinum catalyst from Dow Corning corporation, and the particle size of the selected conductive filler was 30 μm.
And step two), adding the premix obtained in the step one into a catalyst platinum in a formula shown in Table 3, uniformly mixing, adding into a double-screw extruder, setting the temperature at 200 ℃, setting the rotating speed of screws at 300rpm, carrying out dynamic vulcanization reaction for 3min, and carrying out extrusion granulation to obtain the conductive thermoplastic dynamic vulcanized silicone rubber. The prepared conductive thermoplastic dynamic vulcanized silicone rubber has uniform appearance and comfortable hand feeling.
The silicone rubber of comparative example 2 was prepared as follows:
the formulations in Table 3 were prepared according to the process parameters of examples 4-6, but without the addition of a compatibilizer to obtain samples.
The performance parameters of examples 4-6 and comparative example 2 are shown in Table 4.
TABLE 4 Silicone rubber Performance parameters for examples 4-6 and comparative example 2
As can be seen by comparison, the performance of examples 4-6 prepared by dynamic vulcanization after the addition of the compatibilizer is significantly better than that of comparative example 2.
Examples 7 to 10 and comparative example 3
The compositions of the silicone rubbers of examples 7 to 10 and comparative example 3 are shown in table 5, and the compositions described in table 5 are all parts by mass.
TABLE 5 Silicone rubber compositions of examples 7-10 and comparative example 3
The preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber of the embodiment 7-10 comprises the following steps:
step one), adding a thermoplastic polyurethane elastomer (TPU), a silicone rubber compound, a compatilizer, a crosslinking agent and a conductive filler in a formula shown in Table 5 into an internal mixer, setting the temperature at 190 ℃, the rotating speed at 80rpm, and the internal mixing time for 4min, and extruding and granulating to obtain a premix. The thermoplastic polyurethane elastomer used in examples 7 to 10 was WHT-8285 available from Wanhua chemical company, the silicone rubber compound was EN-5150A available from Token organosilicon company, the crosslinking agent was hydrogen-containing silicone oil available from Dow Corning company, model number was JHF-901, the platinum catalyst was RD7 platinum catalyst available from Dow Corning company, and the particle size of the selected conductive filler was 10 μm.
And step two), adding the premix obtained in the step one into a catalyst platinum in a formula shown in Table 5, uniformly mixing, adding into a double-screw extruder, setting the temperature at 210 ℃, setting the rotating speed of screws at 320rpm, carrying out dynamic vulcanization reaction for 1min, and extruding and granulating to obtain the conductive thermoplastic dynamic vulcanized silicone rubber. The prepared conductive thermoplastic dynamic vulcanized silicone rubber has uniform appearance and comfortable hand feeling.
The silicone rubber of comparative example 3 was prepared as follows:
step one) the formulations in table 5 were prepared according to the process parameters of examples 7-10, but without the addition of conductive fillers, to obtain a premix.
And step two), adding the premix obtained in the step one into a conductive filler in a formula shown in Table 5, performing blending extrusion in a double-screw extruder at the set temperature of 210 ℃ and the screw rotation speed of 320rpm, and performing extrusion granulation to obtain a sample. Comparative example 3 can be considered to be prepared by a non-dynamic vulcanization process, since the formulation of comparative example 3 is free of cross-linking agent and catalyst components.
The performance parameters of examples 7-10 and comparative example 3 are shown in Table 6.
TABLE 6 Silicone rubber Performance parameters for examples 7-10 and comparative example 3
As can be seen by comparison, the performances of examples 7-10 prepared by dynamic vulcanization are obviously superior to those of comparative example 3.
Examples 11 to 13 and comparative example 4
The compositions of the silicone rubbers of examples 11 to 13 and comparative example 4 are shown in table 7, and the compositions described in table 7 are all parts by mass.
TABLE 7 Silicone rubber compositions of examples 11-13 and comparative example 4
The preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber of examples 11 to 13 is as follows:
step one), adding a thermoplastic polyurethane elastomer (TPU), a silicone rubber compound, a compatilizer, a crosslinking agent and a conductive filler in a formula shown in Table 7 into an internal mixer, setting the temperature at 160 ℃, the rotating speed at 80rpm, and the internal mixing time for 3min, and extruding and granulating to obtain a premix. The thermoplastic polyurethane elastomer used in examples 11 to 13 was WHT-8285 available from Wanhua chemical company, the silicone rubber compound was EN-5150A available from Token organosilicon company, the compatibilizer was EMA, the crosslinking agent was hydrogen-containing silicone oil available from Dow Corning company, the type was JHF-901, the platinum catalyst was RD7 platinum catalyst available from Dow Corning company, and the particle size of the selected conductive carbon black was 0.1. mu.m.
And step two), adding the premix obtained in the step one into a catalyst platinum in a formula shown in Table 7, uniformly mixing, adding into a double-screw extruder, setting the temperature at 170 ℃, setting the rotating speed of screws at 200rpm, carrying out dynamic vulcanization reaction for 4min, and extruding and granulating to obtain the conductive thermoplastic dynamic vulcanized silicone rubber. The prepared conductive thermoplastic dynamic vulcanized silicone rubber has uniform appearance and comfortable hand feeling.
The silicone rubber of comparative example 4 was prepared as follows:
step one) the formulations in Table 7 were prepared according to the process parameters of examples 11-13, but without the addition of a cross-linking agent and a catalyst, to give a premix.
And step two), blending and extruding the premix in the step one in a double-screw extruder, setting the temperature at 170 ℃ and the rotating speed of the screw at 200rpm, and extruding and granulating to obtain a sample.
The performance parameters of examples 11-13 and comparative example 4 are shown in Table 8.
TABLE 8 Silicone rubber Performance parameters for examples 11-13 and comparative example 4
As can be seen by comparison, the performances of examples 11-13 prepared by dynamic vulcanization using different cross-linking agents and catalyst ratios are significantly better than those of comparative example 4 prepared by a non-dynamic vulcanization method.
Claims (3)
1. An electrically conductive thermoplastic dynamic silicone sulfide rubber characterized by: the composite material is prepared from the following raw materials in parts by mass: 60 parts of thermoplastic polyurethane elastomer, 40 parts of silicone rubber compound, 10 parts of conductive filler, 2 parts of cross-linking agent, 10 parts of compatilizer and 0.1 part of catalyst; or 60 parts of thermoplastic polyurethane elastomer, 40 parts of silicon rubber compound, 10 parts of conductive filler, 2 parts of cross-linking agent, 20 parts of compatilizer and 0.1 part of catalyst;
the Shore hardness of the thermoplastic polyurethane elastomer is 60-95A;
the silicone rubber compound is methyl vinyl silicone rubber reinforced by white carbon black; the molar content of vinyl in the silicon rubber compound is 0.04-0.5%;
the conductive filler is copper powder or nickel powder; the particle size of the conductive filler is 0.1-40 μm;
the cross-linking agent is hydrogen-containing silicone oil, and the molar content of Si-H bonds in the cross-linking agent is 0.4-2%;
the compatilizer is ethylene acrylic acid copolymer;
the preparation method of the conductive thermoplastic dynamic vulcanized silicone rubber comprises the following steps:
1) in an internal mixer or an extruder, melting and blending the thermoplastic polyurethane elastomer, the silicone rubber compound, the conductive filler, the cross-linking agent and the compatilizer, extruding and granulating to obtain a premix;
2) mixing the premix with a catalyst, adding the mixture into a double-screw extruder to perform dynamic vulcanization reaction, extruding and granulating to obtain conductive thermoplastic dynamic vulcanized silicone rubber;
in the step 1), the melt blending process parameters are as follows: the temperature is 160-200 ℃, the time is 3-10 min, and the rotating speed is 30-100 r/min;
in the step 2), the technological parameters of the double-screw extruder are as follows: the processing temperature is 170-210 ℃, the screw rotating speed is 200-320 r/min, and the dynamic vulcanization reaction time is 1-4 min.
2. An electrically conductive thermoplastic dynamic silicone sulfide rubber according to claim 1, wherein: the catalyst is a platinum catalyst.
3. The method for preparing an electrically conductive thermoplastic dynamic silicone sulfide rubber as claimed in any one of claims 1 to 2, wherein: the method comprises the following steps:
1) in an internal mixer or an extruder, melting and blending the thermoplastic polyurethane elastomer, the silicone rubber compound, the conductive filler, the cross-linking agent and the compatilizer, extruding and granulating to obtain a premix;
2) mixing the premix with a catalyst, adding the mixture into a double-screw extruder to perform dynamic vulcanization reaction, extruding and granulating to obtain conductive thermoplastic dynamic vulcanized silicone rubber;
in the step 1), the melt blending process parameters are as follows: the temperature is 160-200 ℃, the time is 3-10 min, and the rotating speed is 30-100 r/min;
in the step 2), the technological parameters of the double-screw extruder are as follows: the processing temperature is 170-210 ℃, the screw rotating speed is 200-320 r/min, and the dynamic vulcanization reaction time is 1-4 min.
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| CN110564042A (en) * | 2019-09-20 | 2019-12-13 | 深圳市宏商材料科技股份有限公司 | composition for preparing conductive heat-shrinkable composite material, conductive heat-shrinkable composite material and preparation method thereof |
| CN110885491A (en) * | 2019-12-20 | 2020-03-17 | 中南大学湘雅医院 | Conductive photosensitive resin for photocuring 3D printing and preparation method thereof |
| CN112143231B (en) * | 2020-08-21 | 2022-03-29 | 北京化工大学 | Silicone rubber/polyurethane thermoplastic vulcanized rubber and preparation method and application thereof |
| CN113999517A (en) * | 2021-10-12 | 2022-02-01 | 中广核三角洲（江苏）塑化有限公司 | Antistatic dynamic vulcanized silicone rubber thermoplastic elastomer and preparation method thereof |
| CN114058187A (en) * | 2021-12-03 | 2022-02-18 | 东莞市蔚美硅材料科技有限公司 | Silicone rubber with low permanent deformation at break and preparation method thereof |
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| AR066616A1 (en) * | 2007-07-27 | 2009-09-02 | Dow Global Technologies Inc | COMPOSITIONS OF THERMOPLASTIC POLYURETHANE (TPU), POLIBUTADIEN AND POLYBIDE BASED TPU |
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