CN112029200B - Low-density thermoplastic dynamic vulcanized rubber material and preparation method and application thereof - Google Patents
Low-density thermoplastic dynamic vulcanized rubber material and preparation method and application thereof Download PDFInfo
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- CN112029200B CN112029200B CN202010790038.9A CN202010790038A CN112029200B CN 112029200 B CN112029200 B CN 112029200B CN 202010790038 A CN202010790038 A CN 202010790038A CN 112029200 B CN112029200 B CN 112029200B
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- 239000000463 material Substances 0.000 title claims abstract description 73
- 229920001169 thermoplastic Polymers 0.000 title claims abstract description 62
- 239000004416 thermosoftening plastic Substances 0.000 title claims abstract description 61
- 239000004636 vulcanized rubber Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 56
- 239000011521 glass Substances 0.000 claims abstract description 55
- 239000011324 bead Substances 0.000 claims abstract description 50
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 32
- 239000004743 Polypropylene Substances 0.000 claims abstract description 29
- -1 polypropylene Polymers 0.000 claims abstract description 29
- 229920001155 polypropylene Polymers 0.000 claims abstract description 28
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 27
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 27
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 24
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 42
- 238000002156 mixing Methods 0.000 claims description 24
- 238000001125 extrusion Methods 0.000 claims description 23
- 238000005469 granulation Methods 0.000 claims description 22
- 230000003179 granulation Effects 0.000 claims description 22
- 150000002978 peroxides Chemical class 0.000 claims description 22
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 22
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 21
- 229940124543 ultraviolet light absorber Drugs 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000003566 sealing material Substances 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 abstract description 14
- 238000007906 compression Methods 0.000 abstract description 9
- 230000006835 compression Effects 0.000 abstract description 9
- 239000000945 filler Substances 0.000 abstract description 5
- 230000005484 gravity Effects 0.000 abstract description 3
- 239000002250 absorbent Substances 0.000 abstract description 2
- 230000002745 absorbent Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000000465 moulding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 229920001971 elastomer Polymers 0.000 description 8
- 229920002635 polyurethane Polymers 0.000 description 8
- 239000004814 polyurethane Substances 0.000 description 8
- 230000004048 modification Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 5
- 238000007789 sealing Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical group [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- 239000005662 Paraffin oil Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
- 229920001276 ammonium polyphosphate Polymers 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000006084 composite stabilizer Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000000744 eyelid Anatomy 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012764 mineral filler Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 239000011701 zinc Substances 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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16J—PISTONS; CYLINDERS; SEALINGS
- F16J15/00—Sealings
- F16J15/02—Sealings between relatively-stationary surfaces
- F16J15/06—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces
- F16J15/10—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing
- F16J15/102—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing characterised by material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a low-density thermoplastic dynamic vulcanized rubber material, a preparation method and application thereof, wherein the raw materials comprise the following components in parts by weight: 10-25 parts of polypropylene resin, 25-40 parts of ethylene propylene diene monomer rubber, 10-40 parts of hollow glass beads, 1-15 parts of filler, 0.3-0.7 part of cross-linking agent, 0.1-0.3 part of ultraviolet light absorbent, 1-4 parts of coupling agent and 0.1-0.3 part of antioxidant. The glass beads in the low-density thermoplastic dynamic vulcanized rubber material are uniformly dispersed, the processability is good, the material density is low, and the glass beads are only 0.6-0.9g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The compression set is low, which is only 24-30%; the material has good processability, easy molding, low use cost, low specific gravity and low pollution, and is beneficial to energy conservation and emission reduction.
Description
Technical Field
The invention relates to the technical field of material science, in particular to a low-density thermoplastic dynamic vulcanized rubber material, a preparation method and application thereof.
Background
Thermoplastic dynamic vulcanized rubber (Thermoplastic dynamic Vulcanizate, TPV for short) is formed by dispersing high-vulcanized Ethylene Propylene Diene Monomer (EPDM) in a continuous polypropylene resin (PP) in a sea-island form, and the low-density thermoplastic dynamic vulcanized rubber material is similar to rubber at the use temperature, has excellent compression rebound resilience, is characterized by thermoplastic plastic at high temperature, and can be rapidly processed and molded in an extrusion, injection molding and other forms. Compared with the traditional EPDM material, the prior low-density thermoplastic dynamic vulcanized rubber material has similar mechanical properties, and the low-density thermoplastic dynamic vulcanized rubber material has small specific gravity (the density of the conventional low-density thermoplastic dynamic vulcanized rubber material is 0.95 g/cm) 3 The EPDM density was 1.2g/cm 3 Above), can be recycled, etc. But the low-density thermoplastic dynamic vulcanized rubber material has higher cost and poorer economy, and can not completely replace the traditional EPDM material.
CN106751007a discloses a preparation method of a high-strength low-density thermoplastic vulcanized rubber material: ethylene propylene diene monomer, modified polyurethane, composite filler, paraffin oil, si69, ammonium polyphosphate, magnesium hydroxide, zinc borate, epoxidized soybean oil, ca/Zn composite stabilizer and anti-aging agent are mixed by an internal mixer, and then are granulated by a single screw extruder to obtain rubber particles, and the rubber particles are subjected to dynamic vulcanization and secondary dynamic vulcanization with polypropylene to obtain the high-strength low-density thermoplastic vulcanized rubber material. Firstly, polyurethane is selected as a composite reinforced base material of rubber, and hard monomers such as 2, 4-toluene diisocyanate, 1, 4-butanediol and the like are selected as the monomers of the polyurethane, so that the final material is biased to a rubber material with high hardness and high strength, but lower compression set rate is brought, and the polyurethane is not suitable for being used as a material requiring high rebound retention rate such as an automobile sealing member. In addition, the neutralization and capping process of polyurethane uses triethylamine, which has strong ammonia odor, continuously and slowly stimulates eyelid and mucous membrane, and the odor pollution of the final material can make the polyurethane unsuitable for being used as a material of an automotive interior sealing part and the like. Secondly, polyurethane is selected as a surface modification material of the hollow glass beads, so that the cost of polyurethane raw materials is high, the preparation process is complex, and the method is not suitable for large-scale production. Thirdly, the adding amount of the hollow glass beads in the method is less than 1% of the raw materials, so that the density of the material is reduced to 0.9, and compared with the density of a conventional low-density thermoplastic dynamic vulcanized rubber material, the hollow glass beads have no obvious difference and limited light weight effect.
Disclosure of Invention
The invention provides a low-density thermoplastic dynamic vulcanized rubber material, and a preparation method and application thereof, so as to solve the problems of high density, insufficient light weight and high compression set of the existing thermoplastic dynamic vulcanized rubber material.
The invention provides a low-density thermoplastic dynamic vulcanized rubber material, which comprises the following raw materials in parts by weight: 10-25 parts of polypropylene resin, 25-40 parts of ethylene propylene diene monomer rubber, 10-40 parts of hollow glass beads, 1-15 parts of filler, 0.3-0.7 part of cross-linking agent, 0.1-0.3 part of ultraviolet light absorbent, 1-4 parts of coupling agent and 0.1-0.3 part of antioxidant.
Preferably, the true density of the hollow glass beads is 0.13-0.7g/cm 3 The compressive strength is 2-200MPa, and the average grain diameter is 30-125 μm. Further preferably, the hollow glass microspheres have a true density of 0.37 to 0.5g/cm 3 The compressive strength is 50-200MPa, and the average particle diameter is 30-70 μm.
Preferably, the crosslinking agent is a phenolic resin or a peroxide crosslinking agent, more preferably a peroxide crosslinking agent.
Preferably, the filler is one or more of calcium carbonate, talcum powder and diatomite, and more preferably talcum powder.
Preferably, the coupling agent is one or more of KH550, KH560, KH570, KH591, more preferably KH570.
The invention provides a method for preparing a low-density thermoplastic dynamic vulcanized rubber material, which comprises the following steps:
mixing a coupling agent with the hollow glass beads to obtain modified hollow glass beads;
uniformly mixing polypropylene resin, ethylene propylene diene monomer, filler, cross-linking agent, ultraviolet light absorber and antioxidant to obtain a mixed raw material;
adding the mixed raw materials and the modified hollow glass beads into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 150-230 ℃, and cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
The method has the advantages of simple process, convenient operation and low cost, and is suitable for mass production.
Preferably, the hollow glass bead modification method comprises the following steps: and (3) proportionally adding the hollow glass beads and a coupling agent into an ethanol water solution with the volume concentration of 3-10%, stirring at 60-90 ℃ for reaction for 0.5-4h, filtering and flushing by using absolute ethanol after the reaction is finished, and drying the obtained solid for 6-15h to obtain the modified hollow glass beads.
Preferably, the mixing temperature is 50-80 ℃ and the mixing time is more than 20 min.
The invention also provides application of the low-density thermoplastic dynamic vulcanized rubber material as a sealing material, wherein the glass beads in the low-density thermoplastic dynamic vulcanized rubber material are uniformly dispersed, the processability is good, and the material density is lowOnly 0.6-0.9g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the The compression set is low, only 24-30%.
Compared with the prior art, the invention has the following advantages:
according to the invention, the hollow glass beads modified by the coupling agent are added into a matrix compounded by the polypropylene resin and the ethylene propylene diene monomer, so that on one hand, the dispersion uniformity of the hollow glass beads in the matrix is increased, on the other hand, the bonding strength of the polypropylene resin, the ethylene propylene diene monomer and the hollow glass beads is increased, and the density is only 0.6-0.9g/cm 3 A low density thermoplastic dynamic vulcanizate of (2); the material also has higher elasticity, the compression set is only 24-30%, and the material can be used as a sealing material for vehicles (such as automobile interior sealing strips), has good processing performance, is easy to form, has low use cost and low specific gravity, is low in pollution, and is beneficial to energy conservation and emission reduction.
Detailed Description
The present invention will be described in further detail below in conjunction with specific embodiments for the purpose of facilitating understanding by those skilled in the art, but it will be understood by those skilled in the art that the embodiments described below are some, but not all, embodiments of the present invention and are intended to be illustrative of the present invention and should not be construed as limiting the scope of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were not manufacturer-identified and the conventional products obtained were purchased commercially. Wherein, the true density of the hollow glass beads is 0.37-0.5g/cm 3 The compressive strength is above 50MPa, and the average particle diameter is 30-70 μm.
Example 1
A low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 20 parts of polypropylene resin, 40 parts of ethylene propylene diene monomer, 30 parts of hollow glass beads, 5 parts of calcium carbonate, 0.4 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber, 5703 parts of KH and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
adding 30 parts by weight of hollow glass beads and 3 parts by weight of KH570 into an ethanol water solution with a volume concentration of 5% for stirring reaction, reacting at 90 ℃ for 0.5h, after the reaction is finished, filtering and flushing by using absolute ethanol, and then heating and drying for 6h to obtain the modified hollow glass beads.
Uniformly mixing 40 parts by weight of ethylene propylene diene monomer, 20 parts by weight of polypropylene resin, 5 parts by weight of calcium carbonate, 0.4 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 80 ℃ for 30min, adding the mixed raw materials and the modified hollow glass beads into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 150 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
Example 2
A low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 25 parts of polypropylene resin, 35 parts of ethylene propylene diene monomer, 40 parts of hollow glass microsphere, 10 parts of calcium carbonate, 0.3 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber, 5704 parts of KH and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
adding 40 parts by weight of hollow glass beads and 4 parts by weight of KH570 into an ethanol water solution with the volume concentration of 7% for stirring reaction, reacting for 2 hours at 75 ℃, after the reaction is finished, filtering and washing by using absolute ethanol, and then heating and drying for 10 hours to obtain the modified hollow glass beads.
Uniformly mixing 35 parts by weight of ethylene propylene diene monomer, 25 parts by weight of polypropylene resin, 10 parts by weight of calcium carbonate, 0.3 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 70 ℃ for 30min, adding the mixed raw materials and the modified hollow glass beads into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 180 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
Example 3
A low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 15 parts of polypropylene resin, 30 parts of ethylene propylene diene monomer, 40 parts of hollow glass beads, 5 parts of calcium carbonate, 0.4 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber, 5704 parts of KH and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
adding 40 parts by weight of hollow glass beads and 4 parts by weight of KH570 into an ethanol water solution with the volume concentration of 8% for stirring reaction, reacting for 2 hours at 60 ℃, after the reaction is finished, filtering and washing by using absolute ethanol, and then heating and drying for 15 hours to obtain the modified hollow glass beads.
Uniformly mixing 30 parts by weight of ethylene propylene diene monomer, 15 parts by weight of polypropylene resin, 5 parts by weight of calcium carbonate, 0.4 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 80 ℃ for 30min, adding the mixed raw materials and the modified hollow glass beads into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 230 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
TABLE 1 specific amounts of raw materials for examples 1-3
| Example 1 | Example 2 | Example 3 | |
| Polypropylene resin (weight portions) | 20 | 25 | 15 |
| Ethylene propylene diene monomer (weight portions) | 40 | 35 | 30 |
| Mineral filler (weight portion) | 5 | 10 | 5 |
| Crosslinking agent (weight portions) | 0.4 | 0.3 | 0.4 |
| Ultraviolet absorber (weight portion) | 0.2 | 0.2 | 0.2 |
| Antioxidant (weight portions) | 0.2 | 0.2 | 0.2 |
| Hollow glass bead (weight portion) | 30 | 40 | 40 |
| Coupling agent (weight portions) | 3 | 4 | 4 |
Comparative example 1
Unlike example 1, the following is: the dosage of the hollow glass beads and the coupling agent is zero. The other raw material components are used in the same amounts and the preparation method as in example 1:
a low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 20 parts of polypropylene resin, 40 parts of ethylene propylene diene monomer, 5 parts of calcium carbonate, 0.4 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
uniformly mixing 40 parts by weight of ethylene propylene diene monomer, 20 parts by weight of polypropylene resin, 5 parts by weight of calcium carbonate, 0.4 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 80 ℃ for 30min, adding the mixed raw materials into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 150 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
Comparative example 2
Unlike example 2, the following is: the dosage of the hollow glass beads and the coupling agent is zero. The other raw material components are used in the same amounts and the preparation method as in example 2:
a low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 25 parts of polypropylene resin, 35 parts of ethylene propylene diene monomer, 10 parts of calcium carbonate, 0.3 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
uniformly mixing 35 parts by weight of ethylene propylene diene monomer, 25 parts by weight of polypropylene resin, 10 parts by weight of calcium carbonate, 0.3 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 70 ℃ for 30min, adding the mixed raw materials into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 180 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
Comparative example 3
Unlike example 3, the following is: the dosage of the hollow glass beads and the coupling agent is zero. The other raw material components are used in the same amounts and the preparation method as in example 3:
a low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 15 parts of polypropylene resin, 30 parts of ethylene propylene diene monomer, 5 parts of calcium carbonate, 0.4 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
uniformly mixing 30 parts by weight of ethylene propylene diene monomer, 15 parts by weight of polypropylene resin, 5 parts by weight of calcium carbonate, 0.4 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 80 ℃ for 30min, adding the mixed raw materials into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 230 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
Comparative example 4
Unlike example 1, the following is: before the hollow glass beads are mixed with other raw materials, no coupling agent is used for modification. The other raw material components are used in the same amounts and the preparation method as in example 1:
a low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 20 parts of polypropylene resin, 40 parts of ethylene propylene diene monomer, 30 parts of hollow glass microsphere, 5 parts of calcium carbonate, 0.4 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
uniformly mixing 40 parts by weight of ethylene propylene diene monomer, 20 parts by weight of polypropylene resin, 5 parts by weight of calcium carbonate, 0.4 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 80 ℃ for 30min, adding the mixed raw materials and the hollow glass beads into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 150 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
Comparative example 5
Unlike example 2, the following is: before the hollow glass beads are mixed with other raw materials, no coupling agent is used for modification. The other raw material components are used in the same amounts and the preparation method as in example 2:
a low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 25 parts of polypropylene resin, 35 parts of ethylene propylene diene monomer, 40 parts of hollow glass microsphere, 10 parts of calcium carbonate, 0.3 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
uniformly mixing 35 parts by weight of ethylene propylene diene monomer, 25 parts by weight of polypropylene resin, 10 parts by weight of calcium carbonate, 0.3 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 70 ℃ for 30min, adding the mixed raw materials and the hollow glass beads into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 180 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
Comparative example 6
Unlike example 3, the following is: before the hollow glass beads are mixed with other raw materials, no coupling agent is used for modification. The other raw material components are used in the same amounts and the preparation method as in example 3:
a low-density thermoplastic dynamic vulcanized rubber material comprises the following raw materials in parts by weight: 15 parts of polypropylene resin, 30 parts of ethylene propylene diene monomer, 40 parts of hollow glass microsphere, 5 parts of calcium carbonate, 0.4 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber and 0.2 part of antioxidant.
The preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
uniformly mixing 30 parts by weight of ethylene propylene diene monomer, 15 parts by weight of polypropylene resin, 5 parts by weight of calcium carbonate, 0.4 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 80 ℃ for 30min, adding the mixed raw materials and the hollow glass beads into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 230 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
The low-density thermoplastic dynamic vulcanized rubber materials prepared in examples 1 to 3 and comparative examples 1 to 6 were subjected to performance tests, and the test results are shown in Table 2:
TABLE 2 Low Density thermoplastic dynamic vulcanizate Performance test results
As can be seen from the comparison between examples 1-3 and comparative examples 1-3 in Table 2, the density of the low-density thermoplastic dynamic vulcanized rubber material is effectively reduced, the hardness is slightly reduced, but the compression set resistance is improved, and the sealing performance of the low-density thermoplastic dynamic vulcanized rubber material for sealing elements is ensured.
As can be seen from the comparison between examples 1-3 and comparative examples 4-6 in table 2, although the hollow glass beads were also used in comparative examples 4-6, the hollow glass beads were not subjected to surface modification by the coupling agent, which resulted in poor intermolecular binding force between the hollow glass beads and the low-density thermoplastic dynamic vulcanized rubber material substrate, which resulted in two problems: 1. in the compression deformation process of rubber, the hollow glass beads in the microstructure of the material and the low-density thermoplastic dynamic vulcanized rubber material base material can slide, so that the rubber is permanently deformed, namely, the compression permanent deformation rate is higher; 2. the hollow glass beads will tend to agglomerate rather than uniformly disperse between the low density thermoplastic dynamic vulcanizate substrates, resulting in a rubber hardness that is relatively high.
The foregoing is merely a specific embodiment of the application to enable one skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (2)
1. The preparation method of the low-density thermoplastic dynamic vulcanized rubber material is characterized by comprising the following raw materials in parts by weight: 15 parts of polypropylene resin, 30 parts of ethylene propylene diene monomer, 40 parts of hollow glass beads, 5 parts of calcium carbonate, 0.4 part of peroxide cross-linking agent, 0.2 part of ultraviolet light absorber, 570.4 parts of KH and 0.2 part of antioxidant;
the true density of the hollow glass beads is 0.37-0.5g/cm 3 The compressive strength is more than 50MPa, and the average grain diameter is 30-70 mu m;
the preparation method of the low-density thermoplastic dynamic vulcanized rubber material comprises the following steps:
adding 40 parts by weight of hollow glass beads and 4 parts by weight of KH570 into an ethanol water solution with the volume concentration of 8%, stirring for reaction, reacting at 60 ℃ for 2 hours, after the reaction is finished, filtering and flushing by using absolute ethanol, and then heating and drying for 15 hours to obtain modified hollow glass beads;
uniformly mixing 30 parts by weight of ethylene propylene diene monomer, 15 parts by weight of polypropylene resin, 5 parts by weight of calcium carbonate, 0.4 part by weight of peroxide cross-linking agent, 0.2 part by weight of ultraviolet light absorber and 0.2 part by weight of antioxidant to obtain a mixed raw material; mixing the mixed raw materials at 80 ℃ for 30min, adding the mixed raw materials and the modified hollow glass beads into a double-screw extruder for extrusion granulation, wherein the extrusion granulation temperature is 230 ℃, and naturally cooling to obtain the low-density thermoplastic dynamic vulcanized rubber material.
2. Use of the low density thermoplastic dynamic vulcanizate prepared by the process of claim 1 as a sealing material.
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| CN109749460A (en) * | 2018-12-26 | 2019-05-14 | 浙江清优材料科技有限公司 | A kind of resistance to compression gets higher hardness foam silicone rubber material and preparation method thereof |
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| CN103980621A (en) * | 2014-05-23 | 2014-08-13 | 苏州特威塑胶有限公司 | High-performance dynamic vulcanization thermoplastic elastomer and preparation method thereof |
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| CN109749460A (en) * | 2018-12-26 | 2019-05-14 | 浙江清优材料科技有限公司 | A kind of resistance to compression gets higher hardness foam silicone rubber material and preparation method thereof |
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