CN111154265B - Silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanized rubber and preparation method thereof - Google Patents
Silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanized rubber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a silicon rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanized rubber and a preparation method thereof, and relates to a thermoplastic vulcanized rubber and a preparation method thereof, wherein the thermoplastic vulcanized rubber comprises silicon rubber, polybutylene succinate, a filler, a vulcanizing agent, a compatibilizer and an antioxidant, wherein the filler is added into the silicon rubber to increase the viscosity of the silicon rubber, and the compatibilizer is added to improve the compatibility of the silicon rubber and the polybutylene succinate and the viscosity ratio of the silicon rubber and the polybutylene succinate; the silicone rubber/poly (butylene succinate) non-petroleum-based thermoplastic vulcanized rubber with a fine phase structure, excellent mechanical properties, excellent elastic recoverability and good biocompatibility is prepared by a dynamic vulcanization technology, and can be widely applied to the fields of biomedicine, wearable equipment and the like.
Description
Technical Field
The invention relates to a thermoplastic vulcanized rubber and a preparation method thereof, in particular to a silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanized rubber and a preparation method thereof.
Background
Thermoplastic elastomer (TPE) is an elastomer material which has rubber elasticity at normal temperature and can be formed by plastic molding at high temperature. Since TPE has both rubber elasticity and plastic reworkability, it is called third-generation rubber, and is an important direction for rubber development nowadays. Thermoplastic vulcanizate (TPV), as a blended Thermoplastic elastomer, is a new polymeric material prepared by crosslinking a rubber phase in situ at high temperature by dynamic vulcanization technology, and shearing the crosslinked rubber phase into particles under the action of high shear force to disperse the particles into the Thermoplastic. It is noteworthy that dynamic vulcanization improves the mechanical and thermal properties of the blend, with the advantages of a wide variety of types, higher heat and aging resistance than synthetic thermoplastic elastomers. The TPV has the advantages that the processing method is simple, the energy consumption is low, different functions and specialities, excellent rebound resilience, good processability and particularly outstanding recyclability can be endowed by mixing different types of rubber and resin, so that the TPV meets the requirements of environmental protection and resource saving, and is one of the elastomers which are developed most quickly.
The silicon rubber is derived from silicon ore, is prepared independently of petroleum resources, and is a non-petroleum-based rubber material. The silicone rubber has the advantages of flexible molecular chains, low hardness, good elasticity, good electrical insulation, good high and low temperature resistance and good biocompatibility. The poly (butylene succinate) is a bio-based polymer material derived from renewable resources, has biodegradability and is a green cyclic polymer material. The poly (butylene succinate) has good processability, mechanical property, thermal stability, chemical stability and biocompatibility. Therefore, the non-petroleum-based thermoplastic vulcanized rubber is prepared by taking the silicon rubber and the polybutylene succinate as the rubber phase and the plastic phase of the thermoplastic vulcanized rubber through a dynamic vulcanization process, and has great strategic significance for solving the crisis of petroleum resources and developing novel environment-friendly materials. In addition, the silicon rubber and the poly (butylene succinate) have good biocompatibility, and the thermoplastic vulcanized rubber of the silicon rubber and the poly (butylene succinate) has good biocompatibility and partial biodegradability, and can be widely applied to the fields of biomedicine, wearable equipment and the like. However, the compatibility between the nonpolar silicone rubber and the polar polybutylene succinate is poor, and the viscosity difference between the nonpolar silicone rubber and the polar polybutylene succinate is large, so that the rubber is not easy to be sheared and broken into uniform and tiny dispersed phase particles, the microscopic phase structure of the silicone rubber/polybutylene succinate is not fine enough, and the mechanical property and the processability are not ideal. Therefore, for the silicone rubber/polybutylene succinate system, it is difficult to solve the compatibility and viscosity ratio of the two matrices.
In recent years, thermoplastic vulcanizates based on silicone rubber have been widely noticed and related patents have appeared, for example, patent CN 105924972B discloses a silicone rubber/polyurethane rubber thermoplastic vulcanizate and a preparation method thereof, which adopts ethylene vinyl acetate copolymer or maleic anhydride graft modified silicone rubber as a compatibilizer, and adds filler to silicone rubber to increase the viscosity of silicone rubber, improve the compatibility of silicone rubber and polyurethane and the viscosity ratio of the two. Patent CN 110066519A discloses a silicone rubber/polypropylene thermoplastic vulcanizate and a preparation method thereof, wherein polypropylene grafted maleic anhydride reacts with epoxy silicone oil to generate an ester in the process of rubber-plastic premixing, or the polypropylene grafted maleic anhydride reacts with ethylene-methyl acrylate-glycidyl methacrylate random terpolymer to generate an ester, and the problem of the viscosity ratio and compatibility of silicone rubber and polypropylene is solved by using the two esters as a compatibilizer. However, the plastics phase polyurethane and polypropylene used in patents CN 105924972B and CN 110066519 a are petroleum-based polymer materials. Therefore, the development of the non-petroleum-based silicone rubber thermoplastic vulcanizate is significant.
Disclosure of Invention
The invention aims to provide a silicon rubber/poly butylene succinate non-petroleum-based thermoplastic vulcanizate and a preparation method thereof, wherein the method comprises the steps of adding a filler into the silicon rubber to increase the viscosity of the silicon rubber, and adding a compatibilizer to improve the compatibility of the silicon rubber and the poly butylene succinate and the viscosity ratio of the silicon rubber and the poly butylene succinate; the silicon rubber/polybutylene succinate thermoplastic vulcanizate with fine phase structure, excellent mechanical property, excellent elastic recovery and good biocompatibility is prepared by a dynamic vulcanization technology.
The purpose of the invention is realized by the following technical scheme:
the silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanizate is prepared from the following raw materials in parts by weight:
40-90 parts of silicon rubber;
60-10 parts of polybutylene succinate;
1-35 parts of a filler;
0.2-4 parts of a vulcanizing agent;
0-15 parts of a compatibilizer;
0.5-2 parts of antioxidant.
The silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanizate is prepared from the following raw materials in parts by weight:
55-75 parts of silicon rubber;
45-25 parts of polybutylene succinate;
20-30 parts of a filler;
0.4-2 parts of a vulcanizing agent;
3-10 parts of a compatibilizer;
0.5-1 part of antioxidant.
The silicon rubber/poly (butylene succinate) non-petroleum-based thermoplastic vulcanized rubber is preferably one or a mixture of dimethyl silicon rubber, hydroxyl-terminated silicon rubber, methyl vinyl phenyl silicon rubber or fluorosilicone rubber.
The filler is preferably one or a mixture of more of white carbon black, silane modified white carbon black or silane modified silica.
The silicon rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanizate is preferably one or a mixture of more of diisopropylbenzene peroxide, dibenzoyl peroxide, 2, 5-dimethyl-2, 5-bis (tert-butyl peroxide) hexane or 2, 5-dimethyl-2, 5-bis (tert-butyl peroxide) -3-hexyne.
The silicon rubber/poly (butylene succinate) non-petroleum-based thermoplastic vulcanized rubber is characterized in that the compatibilizer is preferably one or a mixture of hydroxyl-terminated silicone oil, epoxy silicone oil or a silane coupling agent; wherein the hydroxyl silicone oil preferably has a hydroxyl content of 0.08-0.12; wherein the molecular weight of the epoxy silicone oil is preferably 5000-10000, and the epoxy value is 0.02-0.04; among them, the silane coupling agent is preferably 3-isocyanatopropyltrimethoxysilane, vinyltrimethoxysilane, 3-glycidyloxytrimethoxysilane, gamma-mercaptopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane and 3- (2, 3-glycidoxy) propylmethyldiethoxysilane.
The silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanizate is an antioxidant commonly used in the field, and preferably a hindered phenol antioxidant 1010.
A preparation method of silicon rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanized rubber comprises the following preparation steps:
(1) silicon rubber compound: fully and uniformly mixing the silicon rubber and the filler at room temperature to obtain a silicon rubber compound with higher viscosity;
(2) rubber and plastic blending: melting and blending the silicone rubber compound obtained in the step (1) and poly (butylene succinate) at 120-150 ℃, adding an antioxidant, a compatibilizer and a vulcanizing agent in proportion, uniformly mixing, and then discharging to obtain a rubber-plastic blend;
(3) dynamic vulcanization: and (3) adding the rubber-plastic blend obtained in the step (2) into a mixer for dynamic vulcanization to obtain the silicon rubber/polybutylene succinate thermoplastic vulcanizate.
According to the preparation method of the silicone rubber/poly (butylene succinate) non-petroleum-based thermoplastic vulcanizate, the mixer is preferably a double-screw extruder, an internal mixer or an open mill, the dynamic vulcanization temperature is 160-200 ℃, and the vulcanization time is 5-15 min.
The invention has the advantages and effects that:
(1) the invention selects non-petroleum-based silicon rubber as a rubber phase and environment-friendly polybutylene succinate as a plastic phase, reduces the dependence on non-renewable resources of petroleum and meets the requirements of the sustainable development strategy. The silicone rubber and the poly (butylene succinate) have good biocompatibility, and the thermoplastic vulcanized rubber of the silicone rubber and the poly (butylene succinate) can be widely applied to the fields of biomedical treatment, wearable equipment and the like.
(2) The invention firstly prepares the silicon rubber compound with higher viscosity to solve the problem of difficult rubber crushing caused by larger viscosity difference between pure silicon rubber and poly butylene succinate; then, a compatibilizer is added into the rubber-plastic blending, so that the compatibility of the silicon rubber and the poly butylene succinate is improved; finally, the silicon rubber/polybutylene succinate thermoplastic vulcanizate with fine structure and excellent performance is prepared by dynamic vulcanization.
(3) The silicone rubber/polybutylene succinate thermoplastic vulcanized rubber prepared by the invention has the advantages of tensile strength of 3-14 MPa, elongation at break of 150-600%, hardness (Shore) of 50-90A and tensile recovery rate of 70-90%. The prepared thermoplastic vulcanized rubber sample has smooth and flat surface, has the elasticity of rubber and the fluidity of plastics, and can expand the application fields of silicone rubber and poly (butylene succinate).
Detailed Description
The invention is further described with reference to the following examples, but the scope of the invention is not limited thereto.
Example 1:
the silicon rubber and the poly butylene succinate are dynamically vulcanized according to the following formula, and the components are calculated according to parts by mass.
Dimethyl silicone rubber 50
Polybutylene succinate 50
White carbon black 10
Dicumyl peroxide 0.5
Hydroxy silicone oil 5
Antioxidant 10100.5
The preparation process comprises the following steps:
(1) silicon rubber compound: according to the formula, the dimethyl silicone rubber and the white carbon black are fully and uniformly mixed in an internal mixer at room temperature and 60 rpm to prepare the silicone rubber compound with high viscosity.
(2) Rubber and plastic blending: mixing polybutylene succinate with silicone rubber compound at 120 ℃, adding hydroxyl silicone oil, antioxidant 1010 and dicumyl peroxide according to a proportion, uniformly mixing, discharging, and cooling to room temperature to obtain a rubber-plastic premix;
(3) dynamic vulcanization: and (3) placing the rubber-plastic premix in an internal mixer, dynamically vulcanizing at the temperature of 170 ℃ and the rotation speed of 80 rpm for 8 minutes to obtain the silicon rubber/polybutylene succinate thermoplastic vulcanizate.
The thermoplastic vulcanizates obtained were prepared according to the standard 2mm thick sheets and tested for their properties, the physical and mechanical properties of which are given in Table 1.
Example 2:
the silicon rubber and the poly butylene succinate are dynamically vulcanized according to the following formula, and all the components are calculated according to parts by mass.
Dimethyl silicone rubber 70
Polybutylene succinate 30
White carbon black 30
Dicumyl peroxide 0.7
Hydroxysilicone oils 10
Antioxidant 10101
The preparation process comprises the following steps:
according to the same preparation method as the embodiment 1, the silicon rubber/polybutylene succinate thermoplastic vulcanizate is prepared.
The thermoplastic vulcanizates obtained were prepared according to the standard 2mm thick sheets and tested for their properties, the physical and mechanical properties of which are given in Table 1.
Example 3:
the silicon rubber and the poly butylene succinate are dynamically vulcanized according to the following formula, and all the components are calculated according to parts by mass.
Dimethyl silicon rubber 80
Polybutylene succinate 20
White carbon black 30
Dicumyl peroxide 0.8
Hydroxysilicone oils 10
Antioxidant 10100.5
The preparation process comprises the following steps:
(1) silicon rubber compound: according to the formula, the dimethyl silicone rubber and the white carbon black are fully and uniformly mixed in an internal mixer at room temperature and 70 rpm to prepare the silicone rubber compound with high viscosity.
(2) Rubber and plastic blending: mixing poly (butylene succinate) and silicone rubber compound at 140 ℃, adding hydroxyl silicone oil, antioxidant 1010 and dicumyl peroxide according to a proportion, uniformly mixing, discharging, and cooling to room temperature to obtain a rubber-plastic premix;
(3) dynamic vulcanization: and (3) placing the rubber-plastic premix into an internal mixer, dynamically vulcanizing at the temperature of 170 ℃ and the rotation speed of 100 rpm for 8 minutes to obtain the silicon rubber/polybutylene succinate thermoplastic vulcanizate.
The thermoplastic vulcanizates obtained were prepared according to the standard 2mm thick sheets and tested for their properties, the physical and mechanical properties of which are given in Table 1.
Example 4:
the silicon rubber and the poly butylene succinate are dynamically vulcanized according to the following formula, and all the components are calculated according to parts by mass.
Dimethyl silicon rubber 60
Polybutylene succinate 40
Silane modified white carbon black 20
Dicumyl peroxide 0.6
Epoxy silicone oil 5
Antioxidant 10100.5
The preparation process comprises the following steps:
(1) silicon rubber compound: according to the formula, the dimethyl silicone rubber and the silane modified white carbon black are fully and uniformly mixed in an internal mixer at room temperature and 60 rpm to prepare the silicone rubber compound with high viscosity.
(2) Rubber and plastic blending: mixing polybutylene succinate with silicone rubber compound at 130 ℃, adding epoxy silicone oil, antioxidant 1010 and dicumyl peroxide according to a proportion, uniformly mixing, discharging, and cooling to room temperature to obtain a rubber-plastic premix;
(3) dynamic vulcanization: and (3) placing the rubber-plastic premix into an internal mixer, dynamically vulcanizing at the temperature of 170 ℃ and the rotation speed of 90 rpm for 10 minutes to obtain the silicon rubber/polybutylene succinate thermoplastic vulcanizate.
The thermoplastic vulcanizates obtained were prepared according to the standard 2mm thick sheets and tested for their properties, the physical and mechanical properties of which are given in Table 1.
Example 5:
the silicon rubber and the poly butylene succinate are dynamically vulcanized according to the following formula, and all the components are calculated according to parts by mass.
Dimethyl silicone rubber 70
Polybutylene succinate 30
Silane modified silica 20
Dicumyl peroxide 1
3-glycidyloxytrimethoxysilane 5
Antioxidant 10101
The preparation process comprises the following steps:
according to the same preparation method as the embodiment 4, the silicon rubber/polybutylene succinate thermoplastic vulcanizate is prepared.
The thermoplastic vulcanizates obtained were prepared according to the standard 2mm thick sheets and tested for their properties, the physical and mechanical properties of which are given in Table 1.
Example 6:
the silicon rubber and the poly butylene succinate are dynamically vulcanized according to the following formula, and all the components are calculated according to parts by mass.
Dimethyl silicon rubber 65
Polybutylene succinate 35
White carbon black 30
Dicumyl peroxide 1
Hydroxy silicone oil 5
Epoxy silicone oil 5
Antioxidant 10100.5
The preparation process comprises the following steps:
(1) silicon rubber compound: according to the formula, the dimethyl silicone rubber, the hydroxyl silicone oil and the white carbon black are fully and uniformly mixed in an open mill at normal temperature, and the silicone rubber compound with high viscosity is prepared.
(2) Rubber and plastic blending: mixing poly (butylene succinate) with silicone rubber compound at 130 ℃, adding epoxy silicone oil, an antioxidant 1010 and dicumyl peroxide according to a proportion, discharging after uniform mixing, and cooling to room temperature to obtain a rubber-plastic premix;
(3) dynamic vulcanization: and (3) placing the rubber-plastic premix into an internal mixer, dynamically vulcanizing at the temperature of 170 ℃ and the rotation speed of 90 rpm for 10 minutes to obtain the silicon rubber/polybutylene succinate thermoplastic vulcanizate.
The thermoplastic vulcanizates obtained were prepared according to the standard 2mm thick sheets and tested for their properties, the physical and mechanical properties of which are given in Table 1.
Comparative example 1:
100 g of silicon rubber and 30g of silicon dioxide are uniformly mixed in an open mill at normal temperature, and 1 g of dicumyl peroxide is added to prepare the silicon rubber compound. And vulcanizing at the temperature of 170 ℃ for 10min in a flat vulcanizing machine to obtain a vulcanized silicone rubber sample.
TABLE 1 results of performance testing of thermoplastic vulcanizates prepared in inventive and comparative examples
Claims (2)
1. The silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanizate is characterized by being prepared from the following raw materials in parts by weight:
55-75 parts of silicon rubber;
45-25 parts of polybutylene succinate;
20-30 parts of a filler;
0.4-2 parts of a vulcanizing agent;
3-10 parts of a compatibilizer;
0.5-1 part of antioxidant;
the preparation method of the silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanized rubber comprises the following preparation steps:
(1) silicon rubber compound: fully and uniformly mixing the silicon rubber and the filler at room temperature to obtain a silicon rubber compound with higher viscosity;
(2) rubber and plastic blending: melting and blending the silicone rubber compound obtained in the step (1) and poly (butylene succinate) at 120-150 ℃, adding an antioxidant, a compatibilizer and a vulcanizing agent in proportion, uniformly mixing, and discharging to obtain a rubber-plastic blend;
(3) dynamic vulcanization: adding the rubber-plastic blend obtained in the step (2) into a mixer for dynamic vulcanization to obtain silicon rubber/polybutylene succinate thermoplastic vulcanizate;
the compatibilizer comprises one or a mixture of a plurality of hydroxyl-terminated silicone oil, epoxy silicone oil or silane coupling agent; wherein the hydroxyl content of the hydroxyl silicone oil is 0.08-0.12; wherein the epoxy silicone oil comprises the molecular weight of 5000-10000 and the epoxy value of 0.02-0.04; wherein the silane coupling agent comprises 3-isocyanopropyltrimethoxysilane, vinyl trimethoxy silane, 3-glycidyloxytrimethoxysilane, gamma-mercaptopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane and 3- (2, 3-glycidoxy) propylmethyldiethoxysilane;
the silicon rubber comprises one or more blends of dimethyl silicon rubber, hydroxyl-terminated silicon rubber, methyl vinyl phenyl silicon rubber or fluorosilicone rubber;
the filler comprises one or a mixture of more of white carbon black, silane modified white carbon black or silane modified silica;
the vulcanizing agent comprises one or a mixture of more of diisopropylbenzene peroxide, dibenzoyl peroxide, 2, 5-dimethyl-2, 5-bis (tert-butyl peroxide) hexane or 2, 5-dimethyl-2, 5-bis (tert-butyl peroxide) -3-hexyne;
the antioxidant is hindered phenol antioxidant 1010.
2. The silicone rubber/polybutylene succinate non-petroleum-based thermoplastic vulcanizate according to claim 1, wherein the mixer comprises a twin-screw extruder, an internal mixer or an open mill, the dynamic vulcanization temperature is 160-200 ℃, and the vulcanization time is 5-15 min.
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| CN105837867A (en) * | 2016-04-12 | 2016-08-10 | 沈阳化工大学 | Method of preparing TPV material from eucommia ulmoides and polyolefin thermoplastic resin |
| CN106280474A (en) * | 2016-08-23 | 2017-01-04 | 陈建琴 | A kind of cable high abrasion silastic material |
| CN110066519A (en) * | 2018-01-22 | 2019-07-30 | 北京化工大学 | A kind of silicon rubber/polypropylene thermoplastic vulcanizate and preparation method thereof |
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| US20070213431A1 (en) * | 2004-06-29 | 2007-09-13 | Polyone Corporation | Compatibilized thermoplastic elastomer compositions |
| WO2008026632A1 (en) * | 2006-09-01 | 2008-03-06 | Kaneka Corporation | Thermoplastic elastomer composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105837867A (en) * | 2016-04-12 | 2016-08-10 | 沈阳化工大学 | Method of preparing TPV material from eucommia ulmoides and polyolefin thermoplastic resin |
| CN106280474A (en) * | 2016-08-23 | 2017-01-04 | 陈建琴 | A kind of cable high abrasion silastic material |
| CN110066519A (en) * | 2018-01-22 | 2019-07-30 | 北京化工大学 | A kind of silicon rubber/polypropylene thermoplastic vulcanizate and preparation method thereof |
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