CN112625321A - Preparation method of low-hysteresis-loss rubber composition and tire - Google Patents
Preparation method of low-hysteresis-loss rubber composition and tire Download PDFInfo
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- CN112625321A CN112625321A CN202011364299.0A CN202011364299A CN112625321A CN 112625321 A CN112625321 A CN 112625321A CN 202011364299 A CN202011364299 A CN 202011364299A CN 112625321 A CN112625321 A CN 112625321A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 105
- 239000005060 rubber Substances 0.000 title claims abstract description 101
- 239000000203 mixture Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 61
- 230000000996 additive effect Effects 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 229920003244 diene elastomer Polymers 0.000 claims abstract description 11
- 239000007822 coupling agent Substances 0.000 claims abstract description 10
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 10
- JFBIRMIEJBPDTQ-UHFFFAOYSA-N 3,6-dipyridin-2-yl-1,2,4,5-tetrazine Chemical group N1=CC=CC=C1C1=NN=C(C=2N=CC=CC=2)N=N1 JFBIRMIEJBPDTQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 57
- 239000006229 carbon black Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 16
- 229920002857 polybutadiene Polymers 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 229920000346 polystyrene-polyisoprene block-polystyrene Polymers 0.000 claims description 3
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims description 3
- 229920000026 Si 363 Polymers 0.000 claims description 2
- 239000011324 bead Substances 0.000 claims description 2
- 230000007704 transition Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 24
- 238000005096 rolling process Methods 0.000 abstract description 14
- 238000004073 vulcanization Methods 0.000 abstract description 7
- 235000019241 carbon black Nutrition 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 19
- 238000012360 testing method Methods 0.000 description 19
- 230000004048 modification Effects 0.000 description 16
- 238000012986 modification Methods 0.000 description 16
- 238000004898 kneading Methods 0.000 description 15
- 230000000694 effects Effects 0.000 description 11
- CONKBQPVFMXDOV-QHCPKHFHSA-N 6-[(5S)-5-[[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]methyl]-2-oxo-1,3-oxazolidin-3-yl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C[C@H]1CN(C(O1)=O)C1=CC2=C(NC(O2)=O)C=C1 CONKBQPVFMXDOV-QHCPKHFHSA-N 0.000 description 10
- 238000009472 formulation Methods 0.000 description 10
- 239000003921 oil Substances 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- 241001441571 Hiodontidae Species 0.000 description 5
- 239000004594 Masterbatch (MB) Substances 0.000 description 5
- 239000000945 filler Substances 0.000 description 5
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 4
- 239000005062 Polybutadiene Substances 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000000806 elastomer Substances 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 230000020169 heat generation Effects 0.000 description 3
- 235000019808 microcrystalline wax Nutrition 0.000 description 3
- 239000004200 microcrystalline wax Substances 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 244000043261 Hevea brasiliensis Species 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000010692 aromatic oil Substances 0.000 description 2
- 229920005549 butyl rubber Polymers 0.000 description 2
- 229920003193 cis-1,4-polybutadiene polymer Polymers 0.000 description 2
- 229920003211 cis-1,4-polyisoprene Polymers 0.000 description 2
- ZRALSGWEFCBTJO-UHFFFAOYSA-N guanidine group Chemical group NC(=N)N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920003052 natural elastomer Polymers 0.000 description 2
- 229920001194 natural rubber Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229920003051 synthetic elastomer Polymers 0.000 description 2
- 239000005061 synthetic rubber Substances 0.000 description 2
- CBXRMKZFYQISIV-UHFFFAOYSA-N 1-n,1-n,1-n',1-n',2-n,2-n,2-n',2-n'-octamethylethene-1,1,2,2-tetramine Chemical compound CN(C)C(N(C)C)=C(N(C)C)N(C)C CBXRMKZFYQISIV-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 229920002943 EPDM rubber Polymers 0.000 description 1
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- 239000007987 MES buffer Substances 0.000 description 1
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 240000005373 Panax quinquefolius Species 0.000 description 1
- 238000007551 Shore hardness test Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 229920005557 bromobutyl Polymers 0.000 description 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical class C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 1
- 229920005556 chlorobutyl Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012990 dithiocarbamate Substances 0.000 description 1
- 150000004659 dithiocarbamates Chemical class 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 150000002357 guanidines Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- RLAWWYSOJDYHDC-BZSNNMDCSA-N lisinopril Chemical compound C([C@H](N[C@@H](CCCCN)C(=O)N1[C@@H](CCC1)C(O)=O)C(O)=O)CC1=CC=CC=C1 RLAWWYSOJDYHDC-BZSNNMDCSA-N 0.000 description 1
- 239000010690 paraffinic oil Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000010074 rubber mixing Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- QAZLUNIWYYOJPC-UHFFFAOYSA-M sulfenamide Chemical group [Cl-].COC1=C(C)C=[N+]2C3=NC4=CC=C(OC)C=C4N3SCC2=C1C QAZLUNIWYYOJPC-UHFFFAOYSA-M 0.000 description 1
- 150000003557 thiazoles Chemical class 0.000 description 1
- 150000003585 thioureas Chemical class 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000012991 xanthate 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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
- B60C1/0016—Compositions of the tread
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
- B60C1/0025—Compositions of the sidewalls
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
- B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
- B60C1/0041—Compositions of the carcass layers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L15/00—Compositions of rubber derivatives
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (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)
- Tires In General (AREA)
Abstract
The application discloses a preparation method of a low-hysteresis-loss rubber composition and a tire, wherein the preparation method sequentially comprises the following steps: s1, carrying out thermal reaction treatment on the diene rubber and the low hysteresis loss additive in advance, wherein the temperature of the thermal reaction treatment is 130-160 ℃, and the time of the thermal reaction treatment is 100-300 seconds; s2, adding inorganic reinforcing filler and coupling agent for mixing, and then carrying out vulcanization treatment to obtain a rubber composition product, wherein the low hysteresis loss additive is 3, 6-bis (2-pyridyl) -1,2,4, 5-tetrazine, and 0.2-0.9 part of the low hysteresis loss additive, 30-140 parts of the inorganic reinforcing filler and 1-14 parts of the coupling agent are added to 100 parts of the diene rubber in parts by mass. The rubber composition of the present invention is used for manufacturing a tire; when a tire comprising the above rubber composition is used, the tire has low rolling resistance, excellent tear resistance and good processability.
Description
Technical Field
The invention relates to automobile tires, in particular to a preparation method of a low-hysteresis loss rubber composition and a tire.
Background
With the development of the automobile industry, passenger cars have become indispensable vehicles in people's lives. The tire is a very important part on the automobile, and is the only part of the automobile contacting with the ground, various performances of the automobile, such as driving and braking performance, fuel economy performance, riding comfort performance, operation stability performance, damage resistance performance, safety performance and the like, are completely realized by the interaction between the tire and the ground, and the quality of the tire performance is very important for the automobile.
However, the used materials of the prior art tires have poor low hysteresis loss performance and poor tear resistance, and do not have good processability.
Therefore, the problem to be solved by the present invention is to provide a low hysteresis loss rubber composition for manufacturing a tire, which has good low hysteresis loss performance, good tear resistance, good processability, low heat generation and low rolling resistance, and a preparation method thereof.
Disclosure of Invention
The invention aims to provide a preparation method of a low-hysteresis-loss rubber composition and a tire, wherein a low-hysteresis-loss additive with a lower dosage is added into the rubber composition, so that the hysteresis loss and the heat buildup performance of the rubber composition can be effectively improved, and the rolling resistance of the tire is reduced; meanwhile, the dispersion of the filler is improved, so that the tear strength of the rubber composition is improved, and the influence on the processing performance of the rubber composition is small.
In order to achieve the above object, the present invention provides the following technical solutions.
The embodiment of the application discloses a preparation method of a low-hysteresis-loss rubber composition, which sequentially comprises the following steps:
s1, carrying out thermal reaction treatment on the diene rubber and the low hysteresis loss additive in advance, wherein the temperature of the thermal reaction treatment is 130-160 ℃, and the time of the thermal reaction treatment is 100-300 seconds;
s2 adding inorganic reinforcing filler and coupling agent for mixing and vulcanizing to obtain rubber composition product,
the low hysteresis loss additive is 3, 6-bis (2-pyridyl) -1,2,4, 5-tetrazine, and 0.2-0.9 part of the low hysteresis loss additive, 30-140 parts of inorganic reinforcing filler and 1-14 parts of the coupling agent are added into 100 parts of the diene rubber in parts by weight.
Preferably, in the above-mentioned method for producing a low hysteresis loss rubber composition, the diene rubber includes one or more of polybutadiene rubber, styrene-butadiene copolymer rubber, styrene-isoprene-styrene triblock copolymer rubber, and styrene-butadiene-styrene triblock copolymer rubber.
Preferably, in the above method for preparing a low hysteresis loss rubber composition, the styrene-butadiene copolymer rubber comprises one or more of unmodified solution-polymerized styrene-butadiene rubber, unmodified emulsion-polymerized styrene-butadiene rubber, terminal-modified solution-polymerized styrene-butadiene rubber, terminal-modified emulsion-polymerized styrene-butadiene rubber, main chain-modified solution-polymerized styrene-butadiene rubber and main chain-modified emulsion-polymerized styrene-butadiene rubber.
Preferably, in the above-mentioned method for producing a low hysteresis loss rubber composition, the low hysteresis loss additive is used in an amount of preferably 0.3 to 08 parts, more preferably 0.3 to 0.6 part.
Preferably, in the above method for preparing a low hysteresis loss rubber composition, the inorganic reinforcing filler is white carbon and/or carbon black, and the specific surface area of the white carbon is 60 to 250m2Per g, preferably from 90 to 180m2(ii)/g, the specific surface area of the carbon black is 20 to 160m2Per g, preferably from 40 to 140m2/g。
Preferably, in the preparation method of the low hysteresis loss rubber composition, the white carbon black is used in an amount of 20-120 parts, and the carbon black is used in an amount of 0-80 parts.
Preferably, in the above method for preparing a low hysteresis loss rubber composition, the temperature of the thermal reaction treatment is 140-150 ℃ and the time of the thermal reaction treatment is 150 to 200 seconds.
Preferably, in the above method for preparing a low hysteresis loss rubber composition, the coupling agent is a silane coupling agent, and includes silane coupling agents Si69, Si75, NXT, Si747, and Si 363.
Correspondingly, the rubber composition product obtained by the method is applied to a tire crown or a tire tread or an underlying tread or a tread base or a shoulder cushion rubber or a tire body or a tire side wall or a crown strip or a bead or a transition layer.
When the tire containing the rubber composition is used, the tire has low rolling resistance, excellent tear resistance and good processability.
Detailed Description
Technical solutions in the embodiments of the present invention will be described in detail below, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The present invention relates to a rubber composition for a tire comprising at least one diene rubber, 0.2 to 0.9 part by mass of a low hysteresis loss additive 3, 6-bis (2-pyridyl) -1,2,4, 5-tetrazine, 30 to 140 parts by mass of an inorganic reinforcing filler and 1 to 14 parts by mass of a coupling agent, relative to 100 parts by mass of a rubber component;
the chemical formula of 3, 6-bis (2-pyridyl) -1,2,4, 5-tetrazine is as follows:
the invention also relates to a tire comprising a crown component comprising at least one diene rubber, 100 parts by mass relative to the rubber component, 0.2 to 0.9 part by mass of a low hysteresis loss additive, 30 to 140 parts by mass of an inorganic reinforcing filler and 1 to 14 parts by mass of a coupling agent; (ii) a
The rubber composition contains a low hysteresis loss additive 3, 6-bis (2-pyridyl) -1,2,4, 5-tetrazine. In one embodiment, the low hysteresis loss additive is used in an amount of 0.3 parts by mass. In one embodiment, the low hysteresis loss additive is used in an amount of 0.45 parts by mass.
In one embodiment, the rubber composition contains 50 to 120 parts by mass of white carbon black per 100 parts by mass of the rubber. In one embodiment, the rubber composition contains 60 to 90 parts by mass of white carbon black per 100 parts by mass of the rubber.
The rubber composition can be used for rubbers or elastomers containing unsaturated bonds. Rubber compositions refer to rubber that has been blended or mixed with various ingredients and materials. "diene rubber" or "rubber or elastomer containing unsaturated double bonds" includes natural rubber and other various synthetic rubbers, wherein specific examples of the synthetic rubber include cis-butadiene rubber (cis-1, 4-polybutadiene), polyisoprene (cis-1, 4-polypentadiene), butyl rubber (including ordinary butyl rubber, chlorinated butyl rubber and brominated butyl rubber), styrene-butadiene rubber (butadiene-styrene copolymer), ethylene-propylene rubber (ethylene-propylene-diene monomer copolymer), styrene-isoprene-styrene triblock copolymer rubber and styrene-butadiene-styrene triblock copolymer rubber. Preferred rubbers or elastomers are styrene butadiene rubber and butadiene rubber.
In one aspect, the rubber is preferably a rubber of at least two dienes. For example, a combination of two or more rubbers such as cis-1, 4-polyisoprene rubber (including synthetic cis-1, 4-polyisoprene), styrene-butadiene rubber (butadiene-styrene copolymer), cis-butadiene rubber (cis-1, 4-polybutadiene) is preferable.
In one aspect of the present invention, the styrene-butadiene rubber may be an emulsion-polymerized butadiene-styrene copolymer, which may contain 5 to 40 mass% of styrene, and may be a styrene-butadiene rubber having a higher styrene content.
The rubber composition may contain a plasticizer or a processing oil. May be added during rubber mixing or may be included in the rubber. The processing oil used comprises both extender oil in the rubber or elastomer and processing oil added during mixing of the rubber compound. The processing oil includes various oils known in the art, including aromatic oil, environmentally friendly aromatic oil, naphthenic oil, paraffinic oil, MES, TDAE, various oils of vegetable system, and the like.
The rubber composition may contain 20 to 120 parts by mass of white carbon black. In one embodiment, 60 to 90 parts by mass of white carbon black may be used.
The white carbon black used for the rubber composition includes fumed silica, precipitated silica and the like. In one embodiment precipitated silica is used.
Carbon black may be used as a filler reinforcing material. In one embodiment, the carbon black is used in an amount of less than 50 parts by mass. In one embodiment, the amount of carbon black used is less than 15 parts by mass. In one embodiment, no carbon black is filled. Typical carbon blacks are N110, N121, N134, N220, N231, N234, N242, N293, N299, N315, N326, N330, N332, N339, N343, N347, N351, N358, N375, N539, N550, N582, N630, N642, N650, N683, N754, N762, N765, N774, N787, N907, N908, N990, N991. These carbon blacks are characterized by iodine absorption values of 5 to 150g/kg and DBP absorption values of 30 to 150cm3/100 g.
The rubber composition may contain 1 to 30 parts by mass of a processing aid. The antioxidant is generally used in an amount of 1 to 6 parts by mass. The amount of stearic acid used is generally 0 to 5 parts by mass. The amount of zinc oxide used is generally 1 to 9 parts by mass. The amount of the microcrystalline wax used is generally 0.5 to 5 parts by mass.
The rubber composition contains a vulcanization accelerator to control the vulcanization speed and temperature and improve the processing and use performance of the rubber composition. In one embodiment, two vulcanization accelerators are used, a primary accelerator and a secondary accelerator. Wherein the amount of the main accelerator is generally 0.5 to 4.5 parts by mass, and the amount of the auxiliary accelerator is relatively small and is generally 0.1 to 3 parts by mass. The accelerators which can be used in the present invention are thiazoles, thiurams, sulfenamides, dithiocarbamates, xanthates, guanidines, thioureas and the like. In one embodiment, the primary accelerator is a sulfenamide and the secondary accelerator is a guanidine.
The mixing of the rubber composition can be accomplished by methods commonly used in the art.
The vulcanization temperature of the rubber composition of the present invention is carried out at 100 to 200 ℃. In one embodiment, the vulcanization is carried out at a temperature of 130 to 180 ℃. Conventional vulcanization processes can be used, for example in oil bath heated or electrically heated molds.
The rubber compositions of the invention were tested according to the following standards and methods:
1) mooney viscosity: referring to ASTM D1646-2007, the test conditions were ML (1+4)100 ℃. The larger the index, the higher the Mooney viscosity.
2) Mooney scorching: referring to ASTM D1646-2007, the test temperature was 130 degrees Celsius. The larger the index, the longer the scorch time.
3) Hardness: shore hardness test, according to ASTM D2240-2010. The higher the index the higher the hardness.
4) MA 100: the 100% tensile modulus was measured by reference to ASTM D412-2006, and the modulus was taken at a tensile rate of 100%. The larger the index, the higher the tensile modulus.
5) Tensile strength and elongation at break: referring to ASTM D412-2006, the samples were dumbbell-shaped, testing speed 500mm/min, and testing ambient temperature 23 + -2 deg.C. The larger the index, the higher the tensile strength.
6) Tear strength: referring to ASTM D624-2007, a right-angle shaped test specimen is adopted, the test speed is 500mm/min, and the test environment temperature is 23 +/-2 ℃. The larger the index the higher the tear strength.
7) Hysteresis loss factor: metravib DMA test is adopted, the temperature is 25 ℃, the frequency is 10Hz, the dynamic deformation is 0.07-50 percent, and the plane shearing mode is adopted. The smaller the index, the smaller the hysteresis loss
The raw materials used in the production examples and examples are as follows,
RC 2557S: mono-mountain petrochemical non-modified solution polymerized styrene-butadiene rubber
LG 2550: non-modified solution-polymerized styrene-butadiene rubber of LG Corp Korea
NS616 and NS 612: modified solution-polymerized styrene-butadiene rubber available from Nippon Ruizhong Co., Ltd
SOL 5251H: modified solution polymerized styrene-butadiene rubber from Korea brocade lake company
BR 9000: qilu petrochemical Co Ltd
Natural rubber: no. 20 Biao national corporation
Low hysteresis loss additives: 3, 6-bis (2-pyridyl) -1,2,4, 5-tetrazine, tsukamur chemical co HD165 MP: stannless silicon-forming Co Ltd
N234, N375: carbon black of cabot
Si 69: nanjing eosin chemical group Co., Ltd
6 PPD: shandong Shanshun chemical engineering Co., Ltd
Microcrystalline wax: antilux 111, Rhine chemical Germany
Vivatec 700: han Sheng, Germany, Ltd
Stearic acid: sichuan Tianyu oleochemical Co., Ltd
Zinc oxide: dalian Zinc oxide Co Ltd
DPG: shandong Shanshun chemical engineering Co., Ltd
And (3) CBS: shandong Shanshun chemical engineering Co., Ltd
Sulfur: shandong Shanshun chemical engineering Co., Ltd
Production example 1
In production example 1, the low hysteresis loss additive was applied by kneading it with a solution-polymerized styrene-butadiene rubber in advance to prepare a master batch for a modified rubber, wherein the low hysteresis loss additive was used in an amount of 0.3 part by mass and 0.45 part by mass in the preparation of the modified rubber at a kneading modification temperature of 150 ℃ for a kneading modification time of 120 seconds
TABLE 1 formulation of low hysteresis loss additive modified solution polymerized styrene butadiene rubber
Example 1
The modified rubbers of production examples 1-1, 1-2, 1-3, and 1-4 described above were applied to a rubber composition formulation to evaluate the effect of the low hysteresis loss additive on the modification of solution-polymerized styrene-butadiene rubber in a white carbon black filler system.
TABLE 2 example of application of low hysteresis loss additive modified solution polymerized styrene butadiene rubber
TABLE 3 application Effect of Low hysteresis loss additives modified solution polymerized styrene butadiene rubber
The test results of the rubber compositions are expressed in terms of indices,
the calculation formula is as follows: test items (example comparative examples 1 to 1) × 100.
The hysteresis loss factor of a DMA deformation scan is commonly used in the tire industry to characterize the rolling resistance and heat build-up of a tire, with lower rolling resistance and lower heat build-up for smaller hysteresis loss factors. From example 1, it was found that the hysteresis loss factors of deformation scans of examples 1-1, 1-2, 1-3, 1-4 using the modified rubbers of production examples 1-1, 1-2, 1-3, and 1-4 were all significantly improved as compared with the conventional solution-polymerized styrene-butadiene rubbers of comparative examples 1-1 and 1-2. The modified rubber examples 1-1 in which 0.3 parts by mass of the low hysteresis loss additive was used was improved in hysteresis loss factor by 25% or more as compared with comparative examples 1-1, and the modified rubber examples 1-4 in which 0.45 parts by mass of the low hysteresis loss additive was also improved in hysteresis loss factor by 30% as compared with comparative examples 1-2, thereby effectively reducing the rolling resistance of the tire. In addition, the tear strengths of examples 1-1, 1-2, 1-3, and 1-4 were greatly improved by 20-50% as compared with comparative examples 1-1 and 1-2. Meanwhile, the Mooney viscosities of examples 1-1, 1-2, 1-3 and 1-4 were increased only by a small amount as compared with those of comparative examples 1-1 and 1-2. Therefore, the solution-polymerized styrene-butadiene rubber modified with 0.3 to 0.45 parts by mass of the low hysteresis loss additive can well achieve a balance of low rolling resistance, tear resistance, and good processability.
Production example 2
In production example 2, the low hysteresis loss additive was applied by kneading it with a modified solution-polymerized styrene-butadiene rubber in advance to prepare a further modified rubber master batch, wherein the amount of the low hysteresis loss additive used in the preparation of the modified rubber was 0.3 part by mass, the kneading modification temperature was 150 ℃ and the kneading modification time was 120 seconds.
TABLE 4 formulation of low hysteresis loss additives for modifying modified solution-polymerized styrene-butadiene rubber
Example 2
The modified rubbers of production examples 2-1, 2-2 and 2-3 described above were applied to a rubber composition formulation to evaluate the effect of the low hysteresis loss additive on the modification of a modified solution-polymerized styrene-butadiene rubber in a white carbon black filler system.
TABLE 5 example of application of Low hysteresis loss additives to modified solution-polymerized styrene-butadiene rubber
TABLE 6 application Effect of Low hysteresis loss additives to modified solution-polymerized styrene-butadiene rubber
The test results of the rubber compositions are expressed in terms of indices,
the calculation formula is as follows: test item (example comparative example 2-1) × 100.
From example 2, it can be seen that the effect of significantly reducing hysteresis loss can be achieved by further modifying the solution-polymerized styrene-butadiene rubber with the low hysteresis loss additive. The hysteresis loss factors of deformation scans of examples 2-1, 2-2, and 2-3 were all significantly reduced by 15-30% as compared with comparative examples 2-1, 2-2, and 2-3. Meanwhile, the Mooney viscosities of examples 2-1, 2-2 and 2-3 were increased by only a small amount of about 6 to 10% as compared with those of comparative examples 2-1, 2-2 and 2-3. Therefore, the modified solution-polymerized styrene-butadiene rubber modified with 0.3 parts by mass of the low hysteresis loss additive can well achieve a balance of low rolling resistance and good processability.
Production example 3
In production example 3, the low hysteresis loss additive was used by kneading it with solution-polymerized styrene-butadiene rubber RC2557S in advance to prepare a master batch for a modified rubber, wherein the amount of the low hysteresis loss additive used in the preparation of the modified rubber was 0.4 part by mass, the kneading modification temperature was 150 ℃ and the kneading modification time was 120 seconds.
TABLE 7 formulation of low hysteresis loss additive modified solution polymerized styrene butadiene rubber
| Production example 3-1 | |
| RC2557S | 137.5 |
| Low hysteresis loss additives | 0.4 |
Example 3
The modified rubber of production example 3-1 was used in a rubber composition formulation to evaluate the effect of the low hysteresis loss additive on the modification of solution-polymerized styrene-butadiene rubber in a mixed filler system of white carbon black and carbon black.
TABLE 8 example of application of Low hysteresis loss additive modified solution polymerized styrene butadiene rubber
TABLE 9 application effect of low-hysteresis loss additive modified solution polymerized styrene-butadiene rubber in white carbon black and carbon black mixed system
The test results of the rubber compositions are expressed in terms of indices,
the calculation formula is as follows: test item (example comparative example 3-1) × 100.
From example 3, it can be seen that in the mixed system of white carbon black and carbon black, the hysteresis loss factors of deformation scanning of examples 3-2 and 3-3 are greatly reduced by 15% compared with those of comparative examples 3-2 and 3-3. Meanwhile, the Mooney viscosities of examples 3-2 and 3-3 were reduced by a small amount of about 3 to 5% as compared with those of comparative examples 3-2 and 3-3. Therefore, in a mixed system of white carbon black and carbon black, the solution polymerized styrene-butadiene rubber modified by 0.4 part by mass of the low hysteresis loss additive can well realize the balance of low rolling resistance and good processability.
Production example 4
In production example 4, the low hysteresis loss additive was used by kneading it with solution-polymerized styrene-butadiene rubber RC2557S in advance to prepare a master batch for modified rubber, wherein the amount of the low hysteresis loss additive used in the preparation of modified rubber was 0.4 to 1.0 part by mass, the kneading modification temperature was 150 ℃ and the kneading modification time was 120 seconds.
TABLE 10 formulation of low hysteresis loss additive modified solution polymerized styrene butadiene rubber
Example 4
The modified rubbers of production examples 4-1, 4-2, 4-3, and 4-4 were used in rubber composition formulations to evaluate the effect of various amounts of low hysteresis loss additives on the modification of solution-polymerized styrene-butadiene rubber in a white carbon black system.
TABLE 11 example of application of Low hysteresis loss additive modified solution polymerized styrene butadiene rubber
TABLE 12 application effects of low hysteresis loss additives modified solution polymerized styrene butadiene rubber with different addition amounts
The test results of the rubber compositions are expressed in terms of indices,
the calculation formula is as follows: test item (example comparative example 4-1) × 100.
From example 4, it can be seen that increasing the amount of the low hysteresis loss additive, the hysteresis loss factor of the deformation scan of examples 4-1, 4-2, 4-3, 4-4 gradually decreased. The hysteresis loss factor of the solution-polymerized styrene-butadiene rubber modified by using 0.4 to 0.6 mass part of the low hysteresis loss additive is reduced by 20 to 25 percent, and the reduction range of the hysteresis loss factor becomes insignificant after the dosage of the low hysteresis loss additive is continuously increased. In addition, the tear strengths of examples 4-1, 4-2, 4-3, and 4-4 were significantly improved by 26-79% as compared to comparative example 4-1 while keeping the hardness close. Meanwhile, the Mooney viscosities of examples 4-1 and 4-2 were increased only to a small extent as compared with comparative example 4-1 while keeping the hardness close. Therefore, the solution polymerized styrene-butadiene rubber modified by 0.4 to 0.6 mass part of the low-hysteresis loss additive can well realize the balance of low rolling resistance, tear resistance, good processability and high cost performance.
Production example 5
In production example 5, the low hysteresis loss additive was used by kneading it with solution-polymerized styrene-butadiene rubber RC2557S in advance to prepare a master batch for a modified rubber, wherein the amount of the low hysteresis loss additive used in the preparation of the modified rubber was 0.5 part by mass, the kneading modification temperature was 150 ℃ and the kneading modification time was 120 seconds.
TABLE 13 formulation of low hysteresis loss additive modified solution polymerized styrene butadiene rubber
| Production example 5-1 | |
| RC2557S | 137.5 |
| Low hysteresis loss additives | 0.5 |
Example 5
The modified rubber of production example 5-1 was used in a rubber composition formulation to evaluate the effect of the low hysteresis loss additive on the modification of styrene-butadiene rubber in a white carbon black system.
TABLE 14 examples of applications of low hysteresis loss additives modified styrene butadiene rubber
| Comparative example 5-1 | Example 5-1 | |
| RC2557S | 137.5 | |
| Production example 5-1 | 137.5 | |
| HD165MP | 80 | 80 |
| Si69 | 12.8 | 12.8 |
| 6PPD | 2 | 2 |
| Microcrystalline wax | 1.5 | 1.5 |
| Stearic acid | 2 | 2 |
| Zinc oxide | 2 | 2 |
| DPG | 1.2 | 0.6 |
| CBS | 1.8 | 1.8 |
| Sulfur | 1.2 | 1.2 |
TABLE 15 application effects of low hysteresis loss additives modified solution polymerized styrene butadiene rubber with different addition amounts
| Test items | Comparative example 5-1 | Example 5-1 |
| Mooney viscosity | 100 | 110 |
| Hardness of | 100 | 95 |
| MA100 | 100 | 94 |
| Tensile strength | 100 | 110 |
| Elongation at break | 100 | 106 |
| Tear strength | 100 | 120 |
| Hysteresis loss factor | 100 | 75 |
The test results of the rubber compositions are expressed in terms of indices,
the calculation formula is as follows: test item (example comparative example 5-1) × 100.
From example 5, it can be seen that the hysteresis loss factor of the deformation scan of example 5-1 is significantly reduced by 25% after the addition of the low hysteresis loss additive, and further, the tensile strength, elongation at break and tear strength of example 5-1 are significantly improved as compared to comparative example 4-1.
As can be seen from the above list, the rolling resistance and heat generation of the tire are lower when the hysteresis loss factor of the present invention is smaller, and the rolling resistance is lower and the heat generation is lower when the hysteresis loss factor is smaller. In addition, the invention has lower Mooney viscosity, namely good processing property, while reducing hysteresis loss, and greatly improves the tearing strength, and can realize the balance of low rolling resistance, tearing resistance and good processing property.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. 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 invention. Thus, the present invention 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 (9)
1. A preparation method of a low hysteresis loss rubber composition is characterized by sequentially comprising the following steps:
s1, carrying out thermal reaction treatment on the diene rubber and the low hysteresis loss additive in advance, wherein the temperature of the thermal reaction treatment is 130-160 ℃, and the time of the thermal reaction treatment is 100-300 seconds;
s2 adding inorganic reinforcing filler and coupling agent for mixing and vulcanizing to obtain rubber composition product,
the low hysteresis loss additive is 3, 6-bis (2-pyridyl) -1,2,4, 5-tetrazine, and 0.2-0.9 part of the low hysteresis loss additive, 30-140 parts of inorganic reinforcing filler and 1-14 parts of the coupling agent are added into 100 parts of the diene rubber in parts by weight.
2. The method of claim 1, wherein the diene rubber comprises one or more of polybutadiene rubber, styrene-butadiene copolymer rubber, styrene-isoprene-styrene triblock copolymer rubber, and styrene-butadiene-styrene triblock copolymer rubber.
3. The method of claim 2, wherein the styrene-butadiene copolymer rubber comprises one or more of unmodified solution-polymerized styrene-butadiene rubber, unmodified emulsion-polymerized styrene-butadiene rubber, terminal-modified solution-polymerized styrene-butadiene rubber, terminal-modified emulsion-polymerized styrene-butadiene rubber, main-chain-modified solution-polymerized styrene-butadiene rubber, and main-chain-modified emulsion-polymerized styrene-butadiene rubber.
4. The method for preparing a low hysteresis loss rubber composition according to claim 1, wherein the amount of the low hysteresis loss additive is preferably 0.3 to 08 parts, more preferably 0.3 to 0.6 part.
5. The method for preparing a low hysteresis loss rubber composition according to claim 1, wherein the inorganic reinforcing filler is white carbon and/or carbon black, and the white carbon has a specific surface area of 60 to 250m2Per g, preferably from 90 to 180m2(ii)/g, the specific surface area of the carbon black is 20 to 160m2Per g, preferably from 40 to 140m2/g。
6. The method for preparing the rubber composition with low hysteresis loss according to claim 5, wherein the amount of the white carbon black is 20 to 120 parts, and the amount of the carbon black is 0 to 80 parts.
7. The method for preparing a rubber composition with low hysteresis loss as defined in claim 1, wherein the temperature of the thermal reaction treatment is 140 ℃ and 150 ℃ and the time of the thermal reaction treatment is 150 to 200 seconds.
8. The method of claim 1, wherein the coupling agent is a silane coupling agent comprising silane coupling agents Si69, Si75, NXT, Si747, Si 363.
9. A tire, characterized in that, the rubber composition product obtained in any of claims 1-8 is applied to the tire crown or tire tread or lower tread or tread base or shoulder cushion rubber or carcass or sidewall or crown band or bead or transition layer.
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| CN113801384A (en) * | 2021-10-12 | 2021-12-17 | 肇庆骏鸿实业有限公司 | Tire bead rubber for preventing bead from being empty and preparation method and application thereof |
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| US20040059060A1 (en) * | 1999-09-16 | 2004-03-25 | Keisuke Chino | Thermo-reversible, crosslinkable elastomer and composition thereof |
| CN110461931A (en) * | 2017-03-10 | 2019-11-15 | 大塚化学株式会社 | Rubber composition and tire |
| CN112778592A (en) * | 2019-11-06 | 2021-05-11 | 大冢材料科技（上海）有限公司 | Low-hysteresis-loss rubber composition for tire |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20040059060A1 (en) * | 1999-09-16 | 2004-03-25 | Keisuke Chino | Thermo-reversible, crosslinkable elastomer and composition thereof |
| CN110461931A (en) * | 2017-03-10 | 2019-11-15 | 大塚化学株式会社 | Rubber composition and tire |
| CN112778592A (en) * | 2019-11-06 | 2021-05-11 | 大冢材料科技（上海）有限公司 | Low-hysteresis-loss rubber composition for tire |
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| CN113801384A (en) * | 2021-10-12 | 2021-12-17 | 肇庆骏鸿实业有限公司 | Tire bead rubber for preventing bead from being empty and preparation method and application thereof |
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