CN118165498A - Silicone rubber thermoplastic elastomer with good compatibility of components and preparation method thereof - Google Patents
Silicone rubber thermoplastic elastomer with good compatibility of components and preparation method thereof Download PDFInfo
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- CN118165498A CN118165498A CN202410411348.3A CN202410411348A CN118165498A CN 118165498 A CN118165498 A CN 118165498A CN 202410411348 A CN202410411348 A CN 202410411348A CN 118165498 A CN118165498 A CN 118165498A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 51
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 47
- 229920002725 thermoplastic elastomer Polymers 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920002635 polyurethane Polymers 0.000 claims abstract description 22
- 239000004814 polyurethane Substances 0.000 claims abstract description 22
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical group CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims abstract description 20
- 229940035048 sorbitan monostearate Drugs 0.000 claims abstract description 20
- 235000011076 sorbitan monostearate Nutrition 0.000 claims abstract description 20
- 239000001587 sorbitan monostearate Substances 0.000 claims abstract description 20
- 239000006229 carbon black Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 238000004073 vulcanization Methods 0.000 claims abstract description 15
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 7
- -1 sorbic anhydride Chemical class 0.000 claims abstract description 7
- 239000008117 stearic acid Substances 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000001125 extrusion Methods 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 abstract description 9
- 239000000806 elastomer Substances 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 229920000620 organic polymer Polymers 0.000 abstract description 2
- 230000006835 compression Effects 0.000 description 12
- 238000007906 compression Methods 0.000 description 12
- 239000004952 Polyamide Substances 0.000 description 7
- 229920002647 polyamide Polymers 0.000 description 7
- 239000005060 rubber Substances 0.000 description 7
- 238000004132 cross linking Methods 0.000 description 6
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000004636 vulcanized rubber Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000004433 Thermoplastic polyurethane Substances 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012690 ionic polymerization Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A silicone rubber thermoplastic elastomer with good compatibility of each component and a preparation method thereof belong to the field of organic polymers, wherein the elastomer comprises the following components in parts by weight: 118-123 parts of polyurethane, 79-81 parts of silicon rubber, 19-21 parts of white carbon black, 2-3 parts of compatibilizer and 2-3 parts of vulcanizing agent DBPH. Wherein the compatibilizer is sorbitan monostearate, and the preparation process is prepared by reacting edible industrial stearic acid with sorbic anhydride. The preparation method comprises the following steps of mixing polyurethane with silicon rubber, white carbon black and a compatibilizer, blending for a period of time, then adding a vulcanizing agent in a corresponding proportion, carrying out dynamic vulcanization, and extruding by using a double-screw extruder. According to the invention, through the design of optimized components and the improvement of a combination process, the compatibility of each component of the obtained silicone rubber thermoplastic elastomer is good, and the maximum tensile strength is improved by more than 50%.
Description
Technical Field
The application relates to a silicone rubber thermoplastic elastomer with good compatibility of various components and a preparation method thereof, belonging to the field of organic polymers.
Background
Thermoplastic elastomer (TPE) is a new polymer composite material, which is a polymer or polymer blend made of a polymer which has similar properties to vulcanized rubber at normal temperature and has the same properties as thermoplastic resin after temperature rise, and can be molded or reshaped. The characteristic of TPE, which combines rubber and plastic properties, is due to its unique segmented structure, i.e. the presence of both rubber segments (soft segments) and resin segments (hard segments) consisting of chemical bonds. The hard and soft segments of the appropriate length are coupled in the appropriate order and manner. The former is a high-elasticity chain segment, which contributes elasticity; the interaction between the two molecules is condensed into micro-areas (such as antagonistic micro-areas, ionic micro-areas and the like) which play a role of intermolecular chemical or physical crosslinking points, the crosslinking shows reversible change along with the change of temperature, and when the temperature is increased to a certain temperature, the crosslinking disappears; when cooled to room temperature, the cross-linking functions similarly to the cross-linking of vulcanized rubber; and when the temperature rises above the glass transition temperature or the crystalline melting point of the hard segment, the hard segment softens or melts, the crosslinked network structure is destroyed, and the polymer exhibits plasticity. Compared with the traditional vulcanized rubber, on one hand, the production process of the thermoplastic elastomer does not need vulcanization, the industrial production flow is greatly shortened, and the aim of energy conservation is realized to a great extent; on the other hand, TPE has plastic processing characteristics during processing, so that the problem that the traditional thermosetting rubber is difficult to recycle is fundamentally solved, and great potential economic and social benefits are achieved.
According to the difference of the preparation methods, the thermoplastic elastomer is mainly divided into two major types, namely a chemical synthesis type thermoplastic elastomer and a rubber-plastic blending type thermoplastic elastomer, wherein the chemical synthesis type thermoplastic elastomer is singly produced in a polymer form, and the modes of main chain copolymerization, branch copolymerization, ionic polymerization and the like exist, and the rubber-plastic blending is mainly a blend of rubber and resin.
Thermoplastic elastomers which have been industrially produced in the world are various, but have the defect of higher compression set, for example, the permanent compression set of common soft PVC is more than 65%, the permanent compression set of TPVC which is improved is also more than 25%, the silicone rubber/polyurethane dynamic vulcanization thermoplastic elastomer (TPV) has better mechanical property, good fluidity and excellent elasticity at high temperature, and meanwhile, the silicone rubber/polyurethane dynamic vulcanization thermoplastic elastomer (TPV) has the advantages of easy extrusion, low surface friction coefficient, no toxicity and no harm and better touch feeling, thus having better application prospect, but the blend of the silicone rubber and the polyurethane is easy to separate due to the fact that the silicone rubber and the polyurethane are in an incompatible system in terms of thermodynamics, which leads to poorer performance, and the compatibilization is carried out by adding a compatibilizer in the prior art.
CN102690479a discloses a thermoplastic elastomer of polyamide/ethylene vinyl acetate rubber and its preparation method, the thermoplastic elastomer of ethylene vinyl acetate rubber is composed of polyamide, compatilizer and cross-linking agent, in internal mixer, open mill or screw extruder, the compatilizer is added into the polyamide/ethylene vinyl acetate rubber blend at a certain mixing temperature to improve the blending compatibility of polyamide and ethylene vinyl acetate rubber, while shearing, the peroxide cross-linking agent vulcanizes ethylene vinyl acetate rubber, the blend undergoes phase inversion, the polyamide is dispersed in the continuous phase of rubber to be converted into the cross-linked micron-sized rubber particles dispersed in the continuous phase of polyamide, thus obtaining the polyamide/ethylene vinyl acetate rubber blending thermoplastic elastomer with high rubber content and high performance. The method does not obtain better permanent deformation rate, and the effect of the compatilizer does not reach the standard.
CN117247669a discloses a nano silicon dioxide compatibilized silicone rubber/thermoplastic polyurethane blending elastomer and a preparation method thereof. The nano silicon dioxide modified in situ by the silane coupling agent containing double bonds is used as a reinforcing and compatibilizing material. The double bond on the surface of the silicon dioxide improves the crosslinking density of the composite material, increases the compatibility of the two, and further improves the mechanical property of the composite material. The cost is high, and the nano particles can affect the strength of the material.
In summary, the existing compatibilizer has the defects of high cost, environmental protection, toxicity, high permanent compression set ratio of the final product and the like, so that the silicone rubber thermoplastic elastomer which has low cost, environmental protection and good compatibility of all components with good performance is a problem to be solved.
Disclosure of Invention
According to the invention, through the design of optimized components and the improvement of a combination process, the compatibility of each component of the obtained silicone rubber thermoplastic elastomer is good, and the maximum tensile strength is improved by more than 50%.
Specifically: the invention provides a silicone rubber thermoplastic elastomer with good compatibility of various components, which comprises the following components in parts by weight:
118-123 parts of polyurethane, 79-81 parts of silicon rubber, 19-21 parts of white carbon black, 2-3 parts of compatibilizer and 2-3 parts of vulcanizing agent DBPH.
Wherein the compatibilizer is sorbitan monostearate, and the preparation process is prepared by reacting edible industrial stearic acid with sorbic anhydride.
The preparation method of the silicone rubber thermoplastic elastomer comprises the following steps of mixing polyurethane, silicone rubber, white carbon black and a compatibilizer, blending for a period of time, adding a vulcanizing agent in a corresponding proportion, carrying out dynamic vulcanization, and extruding by using a double-screw extruder.
Wherein the blending temperature is 180-220 ℃, and the blending is carried out for 9-12 minutes.
Wherein the dynamic vulcanization temperature is 135-150 ℃ and the vulcanization time is 3-60 minutes.
Wherein the extrusion temperature is 170-180 ℃ by using a double screw extruder.
The invention creatively discovers that the sorbitan monostearate can activate the interface between the silicone rubber and the polyurethane, reduce the interfacial tension, strengthen the interfacial binding force, reduce the interfacial tension of the original microcosmic incompatible silicone rubber and polyurethane, and improve the degree and uniformity of phase dispersion, thereby forming a stable morphological structure.
The maximum tensile strength of the obtained silicone rubber thermoplastic elastomer is improved by more than 50%, and the permanent compression deformation rate is reduced to 20-30%.
Detailed Description
Example 1
The silicone rubber thermoplastic elastomer with good compatibility of each component comprises the following components in parts by weight:
polyurethane 120, silicone rubber 80, white carbon black 20, sorbitan monostearate 3 and a vulcanizing agent DBPH 3.
The preparation process of the sorbitan monostearate is that the sorbitan monostearate is prepared by reacting edible industrial stearic acid with sorbic anhydride, and the compatibilizer is the sorbitan monostearate.
The preparation method of the silicone rubber thermoplastic elastomer comprises the following steps of mixing polyurethane, silicone rubber, white carbon black, a compatibilizer and 10 minutes of blending at 200 ℃, then adding a vulcanizing agent in a corresponding proportion, carrying out dynamic vulcanization for 10 minutes at 140 ℃, and extruding at 180 ℃ by using a double-screw extruder.
The tensile strength of the prepared silicone rubber thermoplastic elastomer is 12.6MPa, and the permanent compression set is 26%.
Example 2
The silicone rubber thermoplastic elastomer with good compatibility of each component comprises the following components in parts by weight:
Polyurethane 120, silicone rubber 80, white carbon black 20, sorbitan monostearate 2 and a vulcanizing agent DBPH 3.
The preparation process of the sorbitan monostearate is that the sorbitan monostearate is prepared by reacting edible industrial stearic acid with sorbic anhydride, and the compatibilizer is the sorbitan monostearate.
The preparation method of the silicone rubber thermoplastic elastomer comprises the following steps of mixing polyurethane, silicone rubber, white carbon black, a compatibilizer and 10 minutes of blending at 200 ℃, then adding a vulcanizing agent in a corresponding proportion, carrying out dynamic vulcanization for 10 minutes at 140 ℃, and extruding at 180 ℃ by using a double-screw extruder.
The tensile strength of the prepared silicone rubber thermoplastic elastomer is 13MPa, and the permanent compression deformation rate is 24 percent.
Example 3
The silicone rubber thermoplastic elastomer with good compatibility of each component comprises the following components in parts by weight:
Polyurethane 120, silicone rubber 80, white carbon black 20, sorbitan monostearate 2.5 and a vulcanizing agent DBPH 3.
The preparation process of the sorbitan monostearate is that the sorbitan monostearate is prepared by reacting edible industrial stearic acid with sorbic anhydride, and the compatibilizer is the sorbitan monostearate.
The preparation method of the silicone rubber thermoplastic elastomer comprises the following steps of mixing polyurethane, silicone rubber, white carbon black, a compatibilizer and 10 minutes of blending at 200 ℃, then adding a vulcanizing agent in a corresponding proportion, carrying out dynamic vulcanization for 10 minutes at 140 ℃, and extruding at 180 ℃ by using a double-screw extruder.
The tensile strength of the prepared silicone rubber thermoplastic elastomer is 14MPa, and the permanent compression deformation rate is 22 percent.
Comparative example 1
The silicone rubber thermoplastic elastomer comprises the following components in parts by weight:
Polyurethane 120, silicone rubber 80, white carbon black 20 and vulcanizing agent DBPH 3.
The preparation method of the silicone rubber thermoplastic elastomer comprises the following steps of mixing polyurethane, silicone rubber and white carbon black at 200 ℃, blending for 10 minutes, then adding a vulcanizing agent in a corresponding proportion, carrying out dynamic vulcanization at 140 ℃ for 10 minutes, and extruding at 180 ℃ by using a double-screw extruder.
The tensile strength of the prepared silicone rubber thermoplastic elastomer is 8MPa, and the permanent compression deformation rate is 46%.
Comparative example 2
The silicone rubber thermoplastic elastomer with good compatibility of each component comprises the following components in parts by weight:
polyurethane 120, silicone rubber 80, white carbon black 20, sorbitan monostearate 4 and a vulcanizing agent DBPH 3.
The preparation process of the sorbitan monostearate is that the sorbitan monostearate is prepared by reacting edible industrial stearic acid with sorbic anhydride, and the compatibilizer is the sorbitan monostearate.
The preparation method of the silicone rubber thermoplastic elastomer comprises the following steps of mixing polyurethane, silicone rubber, white carbon black, a compatibilizer and 10 minutes of blending at 200 ℃, then adding a vulcanizing agent in a corresponding proportion, carrying out dynamic vulcanization for 10 minutes at 140 ℃, and extruding at 180 ℃ by using a double-screw extruder.
The tensile strength of the prepared silicone rubber thermoplastic elastomer is 11MPa, and the permanent compression deformation rate is 31 percent.
Maximum tensile strength, measured according to GB/T1040-1992.
Permanent compression set, tested according to GB/T1683-1981 standard.
From the above examples, it can be seen that the invention has better technical effect by adding a specific amount of compatibilizer, and that the strength and compression resistance are obviously insufficient without adding compatibilizer, but if more compatibilizer is added, adverse reactions such as agglomeration are caused, but the performance is affected. Therefore, the silicone rubber thermoplastic elastomer with good compatibility of each component prepared by the invention is nontoxic and harmless, has better performance and low cost, and is suitable for products such as notebook computers, earphone, various mobile phone shells or automobile interiors and the like.
The embodiments disclosed in the specification are exemplary, and the claims are intended to cover all embodiments of the invention, and all modifications and equivalent arrangements of the embodiments are possible within the scope of the invention.
Claims (6)
1. The silicone rubber thermoplastic elastomer with good compatibility of each component comprises the following components in parts by weight:
118-123 parts of polyurethane, 79-81 parts of silicon rubber, 19-21 parts of white carbon black, 2-3 parts of compatibilizer and 2-3 parts of vulcanizing agent DBPH.
2. The thermoplastic elastomer of claim 1, wherein the compatibilizer is sorbitan monostearate prepared by reacting technical stearic acid with sorbic anhydride.
3. The method for preparing the silicone rubber thermoplastic elastomer with good compatibility of each component according to claims 1-2, which comprises the following steps of mixing polyurethane with silicone rubber, white carbon black and a compatibilizer, blending for a period of time, adding a vulcanizing agent in a corresponding proportion, carrying out dynamic vulcanization, and extruding by using a double-screw extruder.
4. The process according to claim 3, wherein the blending temperature is 180 to 220℃and the blending is carried out for 9 to 12 minutes.
5. The process according to claim 3, wherein the dynamic vulcanization temperature is 135 to 150℃and the vulcanization time is 3 to 60 minutes.
6. The process according to claim 3, wherein the extrusion temperature is 170 to 180℃using a twin-screw extruder.
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-
2024
- 2024-04-08 CN CN202410411348.3A patent/CN118165498A/en active Pending
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| WO2008097571A1 (en) * | 2007-02-06 | 2008-08-14 | World Properties, Inc. | Conductive polymer foams, method of manufacture, and uses thereof |
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