CN110903654A - Environment-friendly thermoplastic silicone rubber elastomer and preparation method thereof - Google Patents
Environment-friendly thermoplastic silicone rubber elastomer and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an environment-friendly thermoplastic silicone rubber elastomer and a preparation method thereof, wherein the formula of the environment-friendly thermoplastic silicone rubber elastomer comprises the following components in parts by weight: 10-90 parts of silicone rubber, 10-90 parts of polyurethane, 1-10 parts of a compatilizer, 0.5-5 parts of a cross-linking agent, 0.5-5 parts of an auxiliary cross-linking agent and 0.5-5 parts of an antioxidant. A large number of experiments prove that the environment-friendly thermoplastic silicone rubber elastomer prepared by adopting the advanced dynamic vulcanization processing technology and the specific formula has the excellent performances of all components, has very high strength and hardness, and the preparation method has the advantages of simple process, low cost and suitability for wide popularization.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to an environment-friendly thermoplastic silicone rubber elastomer and a preparation method thereof.
Background
Thermoplastic elastomer (TPE) is a material that exhibits elasticity of rubber at normal temperature and can be molded by plasticization at high temperature. Thermoplastic elastomers made by dynamic vulcanization are known as dynamically vulcanized thermoplastic elastomers (TPV). Dynamic Vulcanization (Dynamic Vulcanization) means that rubber and plastic are melt-blended in a mixer with a high shear field and a high temperature field, under the action of a shearing force and a crosslinking agent, the rubber is sheared while being crosslinked to form fine particles, and the fine particles are uniformly dispersed in a plastic continuous phase, wherein vulcanized rubber particles are in a dispersed phase, and the plastic is in a continuous phase.
The dynamic vulcanization is that the rubber phase and the plastic phase are melted under the action of high temperature, the resin is dispersed in the continuous phase rubber phase as a dispersed phase, then the rubber phase is crosslinked under the action of a crosslinking agent and high shear, the viscosity is increased, and the rubber phase is sheared into micron-sized particles to be dispersed in the plastic phase, so that the phase inversion is realized.
The main chain of silicone rubber is composed of alternating silicon and oxygen atoms, and two organic groups are generally attached to the silicon atoms. The silicon rubber has remarkable high and low temperature performance, particularly can still keep flexibility, rebound resilience and the like at the temperature of more than 200 ℃, so that the silicon rubber is concerned by people and the application range is continuously expanded. But the mechanical property is poor, the oil resistance and the solvent resistance are general, and the silicon rubber belongs to thermosetting rubber and cannot be recycled, so that the rapid development of the application of the silicon rubber is greatly limited.
The Polyurethane (TPU) is formed by polymerizing isocyanate monomers and hydroxyl compound monomers, and has good mechanical property, oil resistance, wear resistance, aging resistance and adhesiveness. But the aging resistance and the heat resistance are poor.
The combination of the advantages of silicone rubber and polyurethane is an important method for preparing materials with excellent performance. In the current research, the thermoplastic silicone rubber material prepared by dynamic vulcanization generally has lower strength, complex production process and lower production phase ratio. The problem of poor compatibility of non-polar silicone rubber and polar polyurethane materials cannot be solved by the dynamic vulcanization process, and due to the fact that the viscosity difference of the silicone rubber and the thermoplastic polyurethane elastomer materials is large, the rubber is not easy to shear and break to form uniform and tiny dispersed phase particles in the dynamic vulcanization process, and finally the micro morphology of the silicone rubber polyurethane thermoplastic vulcanized rubber is not fine enough, the mechanical property and the elasticity are poor, and the tensile strength is generally lower than 10 Mpa. In addition, in order to fully vulcanize the silicone rubber, the dynamic vulcanization process generally needs to be carried out in an internal mixer or an extruder for a long mixing time, generally not less than 6min, so that the requirement on the process stability control is high, the performance of the thermoplastic polyurethane elastomer base material is adversely affected by long-time thermal shearing treatment, and meanwhile, precious metal catalysts such as platinum and the like need to be used in the dynamic vulcanization process to initiate crosslinking, so that the cost is high, and platinum black impurities are easy to appear.
Therefore, there is a need to develop an environmentally friendly thermoplastic silicone rubber elastomer with safe storage, environmental protection, moderate hardness and high strength and a preparation method thereof.
Disclosure of Invention
The invention aims to solve the technical problem of providing an environment-friendly thermoplastic silicone rubber elastomer which is safe to store, environment-friendly, moderate in hardness and high in strength, aiming at the existing defects.
In order to solve the technical problems, the invention adopts the technical scheme that the formula of the environment-friendly thermoplastic silicone rubber elastomer comprises the following components in parts by weight: 10-90 parts of silicone rubber, 10-90 parts of polyurethane, 1-10 parts of a compatilizer, 0.5-5 parts of a cross-linking agent, 0.5-5 parts of an auxiliary cross-linking agent and 0.5-5 parts of an antioxidant.
As a preferred technical scheme of the invention, the molecular main chain of the silicon rubber comprises a macromolecular elastic material with silicon atoms and oxygen atoms alternating, the molecular side chain is an organic group, and each macromolecule also comprises at least more than 2 vinyl groups.
As a preferred technical scheme of the invention, the silicon rubber is one or more than two of hydroxyl-terminated silicon rubber, dimethyl silicon rubber, methyl vinyl phenyl silicon rubber and fluorine silicon rubber.
As a preferable technical scheme of the invention, the polyurethane is a polymer polymerized by binary or polybasic isocyanate and binary or polybasic hydroxyl compound, and the polyurethane is polyester polyurethane or polyether polyurethane.
As the preferable technical scheme of the invention, the compatilizer is ethylene vinyl acetate copolymer or maleic anhydride graft modified silicon rubber; the antioxidant is a compound of a hindered phenol antioxidant and a thioester auxiliary antioxidant, and the weight ratio of the hindered phenol antioxidant to the thioester auxiliary antioxidant is 1.2-1.8: 0.4 to 0.9.
As a preferable technical scheme of the invention, the hindered phenol antioxidant is antioxidant 1010 or antioxidant 1098 or antioxidant 2246, and the thioester auxiliary antioxidant is thiodiglycol diacrylate or thiodioctadecyl diacrylate or thiotetradecyl diacrylate.
In a preferred embodiment of the present invention, the crosslinking agent is an organic peroxide, and the organic peroxide is 2, 5-bis (t-butylperoxy) -2, 5-dimethyl-3-hexyne or 2, 5-bis (t-butylperoxy) -2, 5-dimethylhexane, dicumyl peroxide, t-butylperoxyisopropyl carbonate, t-butylcumyl peroxide, or di- (t-butylperoxyisopropyl) benzene.
As a preferred embodiment of the invention, triallyl cyanurate (TAC) or triallyl isocyanurate (TAIC) or trimethylolpropane trimethacrylate (TMPTMA) or N, N-m-phenylene bismaleimide (HA-8) or sulfur (S) is used.
By adopting the technical scheme, the thermoplastic silicone rubber elastomer is prepared by adopting an advanced dynamic vulcanization processing technology and a specific formula, the components in the formula act synergistically, the crosslinked silicone rubber particles are used as a dispersed phase to play a role in improving elasticity, the polyurethane is used as a matrix to still keep the original thermoplastic fluidity, and the original physical properties are kept, so that the thermoplastic silicone rubber elastomer has very high strength and hardness, and when the hardness is up to 60A, the strength is up to 20 MPa.
The invention also aims to solve the technical problem of providing a preparation method of an environment-friendly thermoplastic silicone rubber elastomer with moderate hardness, high strength, easy processing and low cost, aiming at the existing defects.
In order to solve the technical problems, the invention adopts the technical scheme that the preparation method of the environment-friendly thermoplastic silicone rubber elastomer specifically comprises the following steps:
(1) the preparation method comprises the following steps of (1) mixing silicon rubber, polyurethane, a compatilizer and an antioxidant in parts by weight, putting the mixture into an internal mixer, carrying out internal mixing for 15-30 min at the internal mixing temperature of 170-195 ℃, enabling the silicon rubber as a dispersed phase to be uniformly distributed in a polyurethane continuous phase, and granulating in a single screw after the silicon rubber is completely melted to obtain intermediate particles;
(2) the non-crosslinked thermoplastic elastomer matrix, the auxiliary crosslinking agent, the crosslinking agent and the antioxidant are prepared according to the weight parts, and after being uniformly mixed, the mixture is extruded and granulated on a double-screw extruder by adopting a dynamic vulcanization process, wherein the rotating speed is 200-500 r/min, and the extrusion temperature is 150-220 ℃, so that the environment-friendly thermoplastic elastomer material is obtained.
By adopting the technical scheme, firstly preparing an intermediate, then crosslinking the intermediate, and melting and blending unvulcanized raw rubber and unvulcanized polyurethane in a high-temperature and high-shear double screw (the parameters of the adopted double screw extruder are that the length-diameter ratio is 30-70, the rotating speed is 100-1000 r/min, and the temperature of each area of the screw can be stably maintained between 100-230 ℃), so that under the action of a crosslinking agent, silicone rubber is completely subjected to crosslinking reaction and is crushed into micron-sized vulcanized rubber particles which are uniformly dispersed in a polyurethane phase, and then extruding and granulating by adopting the double screw, the structure is very stable, the performance of the elastomer is greatly improved, and the environment-friendly thermoplastic silicone rubber elastomer is obtained; the prepared environment-friendly thermoplastic silicone rubber elastomer has the excellent performances of all components, and has very high hardness and strength, and when the hardness is as high as 60A, the strength is as high as 20 MPa; the preparation method has the advantages of simple process, low cost and wide application.
By adopting the environment-friendly thermoplastic silicone rubber elastomer and the preparation method thereof, the invention has the following beneficial effects:
(1) the adopted raw materials have wide sources, controllable cost and low cost;
(2) the preparation process is simple, and common TPV manufacturing equipment can be used without additional equipment modification or investment;
(3) the environment-friendly thermoplastic dynamic vulcanized elastomer prepared by the invention has high strength and high hardness, and when the hardness reaches 60A, the strength can reach more than 20 MPa.
Detailed Description
The preparation method of the environment-friendly thermoplastic silicone rubber elastomer specifically comprises the following steps:
(1) mixing silicon rubber, polyurethane, a compatilizer and an antioxidant in parts by weight, putting the mixture into an internal mixer, carrying out internal mixing at the temperature of 170 ℃ for 20min, and granulating the mixture in a single screw after all the mixture is melted to obtain intermediate particles;
(2) the non-crosslinked thermoplastic elastomer matrix, the auxiliary crosslinking agent, the crosslinking agent and the antioxidant are prepared according to the weight parts, and after being uniformly mixed, the mixture is extruded and granulated on a double-screw extruder by adopting a dynamic vulcanization process, wherein the rotating speed is 350 r/min, and the extrusion temperature is 150-220 ℃, so that the environment-friendly thermoplastic elastomer material is obtained. The dynamic vulcanization process comprises the steps of melting and blending unvulcanized raw rubber in a thermoplastic elastomer intermediate and unvulcanized polyurethane in a high-temperature and high-shear twin-screw, simultaneously, under the action of a crosslinking agent, completely performing crosslinking reaction on the silicone rubber, crushing the silicone rubber into micron-sized vulcanized rubber particles, uniformly dispersing the micron-sized vulcanized rubber particles in a polyurethane phase, and greatly improving the performance of the elastomer due to the very stable structure, thereby finally obtaining the environment-friendly thermoplastic silicone rubber elastomer.
The following examples 1 to 3 all adopt the preparation method of the environment-friendly thermoplastic silicone rubber elastomer, and are different in the proportion of raw materials, as shown in table 1.
Example 1: adding 90 parts of silicone rubber, 10 parts of polyurethane, 3 parts of compatilizer and 1 part of antioxidant into an internal mixer, carrying out internal mixing at the temperature of 170 ℃ for 20min, and then adding into a single-screw extruder to form intermediate particles; uniformly mixing the prepared intermediate particles, 1 part of cross-linking agent and 3 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder; extrusion temperature zone one: 150 ℃, zone two: 160 ℃, three zones: 170 ℃, four zones: 180 ℃, five zones: 190 ℃, six zones: 200 ℃, seven zones: 210 ℃, eight zones: 220 ℃, nine zones: 220 ℃, ten zones: 220 ℃, eleven zones: 210 ℃, twelve zones: 200 ℃, thirteen zones: extruding finished granules at 190 ℃ and the rotating speed of 350 r/min to obtain an environment-friendly thermoplastic elastomer material; the results of the sample property test are shown in Table 2.
Example 2: adding 80 parts of silicone rubber, 20 parts of polyurethane, 10 parts of compatilizer and 1 part of antioxidant into an internal mixer, carrying out internal mixing at the temperature of 170 ℃ for 20min, and then adding into a single-screw extruder to form intermediate particles; uniformly mixing the prepared intermediate particles, 1 part of cross-linking agent and 3 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder; extruding finished granules at the extrusion temperature of 150-220 ℃ and the rotation speed of 350 r/min to obtain an environment-friendly thermoplastic elastomer material; the results of the sample property test are shown in Table 2.
Example 3: adding 70 parts of silicone rubber, 30 parts of polyurethane, 10 parts of compatilizer and 1 part of antioxidant into an internal mixer, carrying out internal mixing at the temperature of 170 ℃ for 20min, and then adding into a single-screw extruder to form intermediate particles; uniformly mixing the prepared intermediate particles, 1 part of cross-linking agent and 5 parts of auxiliary cross-linking agent in a mixer, and adding the mixture into a double-screw extruder; extruding finished granules at the extrusion temperature of 150-220 ℃ and the rotation speed of 350 r/min to obtain an environment-friendly thermoplastic elastomer material; the results of the sample property test are shown in Table 2.
In examples 1 to 3, the specific components are shown in table 1 below;
TABLE 1 raw material formulation (unit: parts by weight) of the environmentally friendly thermoplastic silicone rubber elastomer of examples 1 to 3
| Raw materials | Example 1 | Example 2 | Example 3 |
| Silicone rubber | 90 | 80 | 70 |
| Polyurethane | 10 | 20 | 30 |
| Compatilizer | 3 | 10 | 10 |
| Crosslinking agent | 1 | 1 | 1.0 |
| Auxiliary crosslinking agent | 3 | 3 | 5 |
| Antioxidant agent | 1.0 | 1.0 | 1.0 |
Wherein, the raw materials for preparing the environment-friendly thermoplastic silicone rubber elastomer in the above examples 1 to 3 are selected as follows,
silicon rubber brand: TR-70, Dow Corning;
polyurethane brand: TEXIN RxT70A, bayer, germany;
compatibilizers, EVA-1104, DuPont, USA;
crosslinking agents, dicumyl peroxide, DCP, hadamard reagent ltd;
co-crosslinking agent, TAIC, hadamard reagent ltd;
antioxidants, Irganox1010/Irgafos168, Pasteur, Germany;
table 2 results of performance test of the eco-friendly thermoplastic silicone rubber elastomers prepared in examples 1 to 3
As can be seen from the performance test results of table 2, as the content of polyurethane increases, the hardness of the thermoplastic silicone rubber elastomer gradually increases and the tensile strength gradually increases, just confirming the tensile properties of the material provided by polyurethane as a continuous phase.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (10)
1. The environment-friendly thermoplastic silicone rubber elastomer is characterized in that the formula of the environment-friendly thermoplastic silicone rubber elastomer is composed of the following components in parts by weight: 10-90 parts of silicone rubber, 10-90 parts of polyurethane, 1-10 parts of a compatilizer, 0.5-5 parts of a cross-linking agent, 0.5-5 parts of an auxiliary cross-linking agent and 0.5-5 parts of an antioxidant.
2. The environmentally friendly thermoplastic silicone rubber elastomer according to claim 1, wherein the molecular main chain of the silicone rubber comprises a macromolecular elastic material in which silicon atoms and oxygen atoms are alternated, the molecular side chain is an organic group, and each macromolecule further comprises at least 2 vinyl groups.
3. The environment-friendly thermoplastic silicone rubber elastomer according to claim 2, wherein the silicone rubber is one or two or more of hydroxyl-terminated silicone rubber, dimethyl silicone rubber, methyl vinyl phenyl silicone rubber, and fluorosilicone rubber.
4. The environment-friendly thermoplastic silicone rubber elastomer according to claim 1, wherein the polyurethane is a polymer obtained by polymerizing a di-or poly-isocyanate and a di-or poly-hydroxyl compound, and the polyurethane is polyester polyurethane or polyether polyurethane.
5. The environment-friendly thermoplastic silicone rubber elastomer according to claim 1, wherein the compatibilizer is an ethylene vinyl acetate copolymer or a maleic anhydride graft-modified silicone rubber; the antioxidant is a compound of a hindered phenol antioxidant and a thioester auxiliary antioxidant, and the weight ratio of the hindered phenol antioxidant to the thioester auxiliary antioxidant is 1.2-1.8: 0.4 to 0.9.
6. The environment-friendly thermoplastic silicone rubber elastomer according to claim 5, wherein the hindered phenolic antioxidant is antioxidant 1010 or antioxidant 1098 or antioxidant 2246, and the thioester-based auxiliary antioxidant is thiobisdodecanediol diacrylate or thiobisoctadecyl diacrylate or thiobistetradecyl diacrylate.
7. The environmentally friendly thermoplastic silicone rubber elastomer according to claim 6, wherein the crosslinking agent is an organic peroxide, and the organic peroxide is 2, 5-bis-butylperoxy-2, 5-dimethyl-3-hexyne or 2, 5-bis-butylperoxy-2, 5-dimethylhexane or dicumyl peroxide or t-butylperoxyisopropyl carbonate or t-butylcumyl peroxide or di-t-butylperoxyisopropyl benzene.
8. The environmentally friendly thermoplastic silicone rubber elastomer according to claim 7, wherein the co-crosslinking agent is triallyl cyanurate (TAC) or triallyl isocyanurate (TAIC) or trimethylolpropane trimethacrylate (TMPTMA) or N, N-m-phenylene bismaleimide (HA-8) or sulfur (S).
9. The preparation method of the environment-friendly thermoplastic silicone rubber elastomer according to any one of claims 1 to 8, comprising the following steps:
(1) the preparation method comprises the following steps of (1) mixing silicon rubber, polyurethane, a compatilizer and an antioxidant in parts by weight, putting the mixture into an internal mixer, carrying out internal mixing for 15-30 min at the internal mixing temperature of 170-195 ℃, enabling the silicon rubber as a dispersed phase to be uniformly distributed in a polyurethane continuous phase, and granulating in a single screw after the silicon rubber is completely melted to obtain intermediate particles;
(2) the non-crosslinked thermoplastic elastomer matrix, the auxiliary crosslinking agent, the crosslinking agent and the antioxidant are prepared according to the weight parts, and after being uniformly mixed, the mixture is extruded and granulated on a double-screw extruder by adopting a dynamic vulcanization process, wherein the rotating speed is 200-500 r/min, and the extrusion temperature is 150-220 ℃, so that the environment-friendly thermoplastic elastomer material is obtained.
10. The method for preparing the environment-friendly thermoplastic silicone rubber elastomer according to any one of claims 1 to 8, wherein the environment-friendly thermoplastic silicone rubber elastomer is applied to the fields of buildings, medical instruments and cables.
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| CN114044878A (en) * | 2021-11-25 | 2022-02-15 | 安徽昊华环保科技有限公司 | Preparation process of heat-resistant high-hardness polyurethane screen elastomer |
| CN114989542A (en) * | 2022-06-20 | 2022-09-02 | 浙江新洁新材料科技有限公司 | PVC modified silica gel hose and production process thereof |
| CN115340727A (en) * | 2022-08-17 | 2022-11-15 | 万华化学（宁波）有限公司 | Polypropylene alloy with high surface hardness and preparation method and application thereof |
| KR20230073665A (en) * | 2021-11-19 | 2023-05-26 | 경상국립대학교산학협력단 | Thermoplastic vulcanizate comprising fluorosilicone rubber and method for preparing the same |
| CN116396617A (en) * | 2023-04-28 | 2023-07-07 | 杭州老板电器股份有限公司 | Refrigerator sealing strip material and preparation method thereof |
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| CN115340727A (en) * | 2022-08-17 | 2022-11-15 | 万华化学（宁波）有限公司 | Polypropylene alloy with high surface hardness and preparation method and application thereof |
| CN115340727B (en) * | 2022-08-17 | 2023-10-17 | 万华化学（宁波）有限公司 | Polypropylene alloy with high surface hardness and preparation method and application thereof |
| CN116396617A (en) * | 2023-04-28 | 2023-07-07 | 杭州老板电器股份有限公司 | Refrigerator sealing strip material and preparation method thereof |
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