CN116656022B - Solid tire tread rubber and preparation method thereof - Google Patents
Solid tire tread rubber and preparation method thereof Download PDFInfo
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- CN116656022B CN116656022B CN202310625213.2A CN202310625213A CN116656022B CN 116656022 B CN116656022 B CN 116656022B CN 202310625213 A CN202310625213 A CN 202310625213A CN 116656022 B CN116656022 B CN 116656022B
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- flake graphite
- crystalline flake
- tread rubber
- silicon carbide
- rubber
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 84
- 239000005060 rubber Substances 0.000 title claims abstract description 84
- 239000007787 solid Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000010439 graphite Substances 0.000 claims abstract description 75
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 75
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 36
- 239000006229 carbon black Substances 0.000 claims abstract description 24
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 24
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 16
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 244000043261 Hevea brasiliensis Species 0.000 claims abstract description 12
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 12
- 229920003052 natural elastomer Polymers 0.000 claims abstract description 12
- 229920001194 natural rubber Polymers 0.000 claims abstract description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 9
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 9
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008117 stearic acid Substances 0.000 claims abstract description 9
- 239000011787 zinc oxide Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 10
- 238000012360 testing method Methods 0.000 description 29
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 12
- IANQTJSKSUMEQM-UHFFFAOYSA-N benzofuran Natural products C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 9
- 239000002699 waste material Substances 0.000 description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 230000003068 static effect Effects 0.000 description 6
- 238000005299 abrasion Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000003963 antioxidant agent Substances 0.000 description 5
- 230000003078 antioxidant effect Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 229920002725 thermoplastic elastomer Polymers 0.000 description 3
- 239000004636 vulcanized rubber Substances 0.000 description 3
- OUBMGJOQLXMSNT-UHFFFAOYSA-N N-isopropyl-N'-phenyl-p-phenylenediamine Chemical compound C1=CC(NC(C)C)=CC=C1NC1=CC=CC=C1 OUBMGJOQLXMSNT-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 239000003093 cationic surfactant Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000012492 regenerant Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000010920 waste tyre Substances 0.000 description 2
- ZRMMVODKVLXCBB-UHFFFAOYSA-N 1-n-cyclohexyl-4-n-phenylbenzene-1,4-diamine Chemical compound C1CCCCC1NC(C=C1)=CC=C1NC1=CC=CC=C1 ZRMMVODKVLXCBB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000499 benzofuranyl group Chemical group O1C(=CC2=C1C=CC=C2)* 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010057 rubber processing Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C08L17/00—Compositions of reclaimed rubber
-
- 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
-
- 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
- C08L2201/00—Properties
- C08L2201/04—Antistatic
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention discloses a tread rubber for a solid tire and a preparation method thereof. The tread rubber comprises: 45-60 parts of natural rubber reclaimed rubber, 0.5-1.0 part of zinc oxide, 0.1-0.3 part of stearic acid, 0.1-1.0 part of anti-aging agent, 0.5-2 parts of plasticizer, 5-15 parts of carbon black and 3-5 parts of modified crystalline flake graphite. Adding flake graphite and silicon carbide whisker into alkali liquor, heating, adding hexadecyl trimethyl ammonium chloride for multiple times under stirring, and after the reaction, carrying out suction filtration and drying to obtain a solid; and adding the solid into a sodium dodecyl benzene sulfonate solution for ultrasonic treatment, filtering and drying to obtain the modified crystalline flake graphite. According to the invention, the flake graphite and the silicon carbide whisker are combined together through hydrogen bonds, so that the antistatic capacity and the thermal conductivity of the tread rubber can be improved, the strength of the tread rubber can be improved, the consumption of carbon black can be reduced, and the wear resistance of the tread rubber can be improved.
Description
Technical Field
The invention relates to the technical field of rubber processing, in particular to solid tire tread rubber and a preparation method thereof.
Background
The earliest tires were solid tires. Solid tires remain a major part of engineering vehicles because of their excellent wear and puncture resistance. The tyre body of the solid tyre is solid, does not need a cord as a framework and does not need to be inflated, so that an inner tube or an airtight layer is not needed, and the tyre body is mainly used for high-load vehicles or machines running at a low speed and also used for fixed-position machines at present.
Since the solid tire has no cord and skeleton, the rubber consumption of the solid tire is large, which also increases the cost of the solid tire; in order to reduce the production cost, the tread rubber can replace part of raw rubber by natural rubber made of waste rubber, but compared with the natural rubber, the strength and the wear resistance of the reclaimed rubber are still poor, so that the bearing capacity of the solid tire made of the reclaimed rubber is low and the wear resistance is poor. And the surface of the tire can generate electrostatic phenomenon to accumulate a large amount of static charges after being ground for a long time, when the static charges accumulate too much, the static charges can change oxygen in the air into ozone with higher activity, so that the oxidation damage of the surface of the tread rubber is accelerated, and the wear resistance of the tread rubber is reduced. The patent with application number 201910454958.0 discloses a noise-reducing and vibration-reducing solid tire and a preparation method thereof, wherein the wear resistance and the tensile property of tread rubber are improved by adding glass fiber, silicon carbide fiber and acrylate emulsion. The patent with application number 202111610525.3 discloses a durable solid tire and a preparation method thereof, wherein the calcium carbonate whisker with good antistatic function is added, and the static charge generated in the friction process can be timely dispersed by means of a three-dimensional network constructed by the calcium carbonate whisker in tread rubber, so that the formation of ozone is reduced, and the wear resistance of the tire is improved. Compared with calcium carbonate whisker, the crystalline flake graphite has good performances of high temperature resistance, electric conduction, heat conduction, lubrication, plasticity, acid and alkali resistance and the like, and if the crystalline flake graphite is used in tread rubber, the antistatic performance of the tread rubber can be improved, and the heat conduction performance, the acid and alkali resistance and the like of the tread rubber can also be improved. However, the flake graphite is easy to agglomerate and poor in dispersibility, the wear resistance of the tread rubber cannot be improved, a large amount of carbon black is needed to be added to improve the wear resistance, the addition amount of the carbon black is too large, and a deep black trace is left when the solid tire rubs with the ground in the use process, so that the environment is damaged. So the report of using the flake graphite for tread rubber is less at present. Therefore, how to use the flake graphite in the tread rubber for static resistance, heat resistance, abrasion resistance and strength improvement and reduce the dosage of carbon black is a technical problem to be solved.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a solid tire tread rubber and a preparation method thereof. According to the invention, the flake graphite and the silicon carbide whisker are combined together through hydrogen bonds, so that the antistatic capacity and the thermal conductivity of the tread rubber can be improved, the strength of the tread rubber can be improved, the consumption of carbon black can be reduced, and the wear resistance of the tread rubber can be improved.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a solid tire tread rubber, which comprises the following raw materials in parts by weight:
45-60 parts of natural rubber reclaimed rubber, 0.5-1.0 part of zinc oxide, 0.1-0.3 part of stearic acid, 0.1-1.0 part of anti-aging agent, 0.5-2 parts of plasticizer, 5-15 parts of carbon black and 3-5 parts of modified crystalline flake graphite;
the modified crystalline flake graphite comprises crystalline flake graphite and silicon carbide whiskers, and the mass ratio of the crystalline flake graphite to the silicon carbide whiskers is 10: (0.5-1).
The antioxidant is at least one selected from antioxidant 4010, antioxidant 4010NA, antioxidant AW, antioxidant 3100, antioxidant RD and antioxidant A.
The plasticizer is coumarone.
Preferably, the modified flake graphite is prepared by the following method:
(1) Adding flake graphite and silicon carbide whisker into alkali liquor, heating, adding hexadecyl trimethyl ammonium chloride for multiple times under stirring, and after the reaction, carrying out suction filtration and drying to obtain a solid;
(2) And adding the solid into a sodium dodecyl benzene sulfonate solution for ultrasonic treatment, filtering and drying to obtain the modified crystalline flake graphite.
Preferably, in the step (1), the alkali liquor is sodium hydroxide solution or potassium hydroxide solution, and the concentration of the alkali liquor is 0.1-0.3 moL/L; the mass ratio of the total mass of the crystalline flake graphite and the silicon carbide crystal to the alkali liquor and the hexadecyl trimethyl ammonium chloride is 1:10:0.1.
preferably, in the step (1), the heating temperature is 40-60 ℃, and the heating time is 10-30 min.
Preferably, in the step (2), the mass ratio of the solid to the sodium dodecyl benzene sulfonate solution is 1: (5-10); the concentration of the sodium dodecyl benzene sulfonate solution is 25g/L; the ultrasonic treatment time is 10-30 min.
The sodium dodecyl benzene sulfonate solution is obtained by dissolving sodium dodecyl benzene sulfonate in water.
In a second aspect of the present invention, there is provided a method for producing a tread rubber for a solid tire, the method comprising:
mixing the waste rubber powder with zinc oxide, stearic acid, an anti-aging agent and a plasticizer for primary banburying, adding carbon black and modified crystalline flake graphite for secondary banburying, blanking, then opening, discharging and cooling to obtain the tread rubber.
Preferably, the temperature of the primary banburying is 120-130 ℃ and the time is 10-13 min; the temperature of the secondary banburying is 100-110 ℃ and the time is 3-7 min.
Preferably, the temperature of the open mill is 100-110 ℃ and the time is 10-15 min.
The invention has the beneficial effects that:
(1) According to the invention, the flake graphite and the silicon carbide whisker are combined together through the hydrogen bond, the antistatic capacity and the heat conductivity of the tread rubber are improved by utilizing the flake graphite, the strength of the tread rubber is improved by utilizing the silicon carbide whisker, the wear resistance of the tread rubber is improved after the flake graphite-silicon carbide whisker is combined through the hydrogen bond, and the consumption of carbon black is reduced.
(2) The tread rubber prepared by the invention can reduce the dosage of carbon black, reduce black marks generated by friction between the solid tire and the ground in the use process, and reduce the damage to the environment. Meanwhile, the dosage of the silicon carbide whisker is not high, and the dosage of the carbon black is reduced, so that the cost of the tread rubber is not increased.
(3) The preparation method is simple, and the tread rubber can be obtained only by secondary banburying and primary scouring.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the present application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background art, the crystalline flake graphite has good performances of high temperature resistance, electric conduction, heat conduction, lubrication, plasticity, acid and alkali resistance and the like, and can not only improve the antistatic performance of the tread rubber, but also improve the heat conduction performance, acid and alkali resistance and the like of the tread rubber if used in the tread rubber. But the flake graphite is easy to agglomerate and has poor dispersibility, and the wear resistance of the tread rubber cannot be improved.
Based on the above, the invention aims to provide a solid tire tread rubber and a preparation method thereof. According to the invention, the silicon carbide whisker is used for modifying the crystalline flake graphite, and the crystalline flake graphite is added into the tread rubber as a filler, so that the tread rubber has the characteristics of static resistance, heat conduction and the like, the wear resistance of the tread rubber is improved, and the consumption of carbon black is reduced. Unlike calcium carbonate whiskers used for improving wear resistance, silicon carbide whiskers generally have a reinforcing component added to a plastic matrix, a metal matrix or a ceramic matrix to play a good role in reinforcing and toughening. Both silicon carbide whiskers and crystalline flake graphite have the problem of difficult stable and uniform dispersion, and crystalline flake graphite and silicon carbide whiskers are respectively added into tread rubber, so that the abrasion resistance is not remarkably improved, and a large amount of carbon black is required to be added. According to the invention, through research, the treatment of alkali liquor and hexadecyl trimethyl ammonium chloride is utilized, the crystalline flake graphite and the silicon carbide whisker can be combined together through hydrogen bonds, and the hexadecyl trimethyl ammonium chloride is acid and alkali resistant, so that the crystalline flake graphite and the silicon carbide whisker can be helped to form hydrogen bonds in an alkaline environment. The stable and uniform dispersion of the crystalline flake graphite-silicon carbide whisker can be improved by using sodium dodecyl benzene sulfonate for treatment. However, since cetyl trimethyl ammonium chloride is a cationic surfactant and sodium dodecyl benzene sulfonate is an anionic surfactant, precipitation is generated when the cetyl trimethyl ammonium chloride and the sodium dodecyl benzene sulfonate are mixed, so that the effect of the sodium dodecyl benzene sulfonate is lost, and the invention discovers that after hydrogen bonds are formed, the obtained solid is dried, the excessive cetyl trimethyl ammonium chloride is removed, and then the solid is added into sodium dodecyl benzene sulfonate for ultrasonic treatment, so that the effect of the cationic surfactant and the anionic surfactant are complementary, so that crystalline flake graphite and silicon carbide whisker can be combined together, and crystalline flake graphite-silicon carbide whisker can be stably and uniformly dispersed in tread rubber. As can be seen from test example 1, the addition of cetyltrimethylammonium chloride to the medium alkali solution for treating the crystalline flake graphite and the silicon carbide whisker to obtain crystalline flake graphite-silicon carbide whisker, and the sodium dodecyl benzene sulfonate for treating the crystalline flake graphite-silicon carbide whisker can reduce the carbon black dosage and remarkably improve the wear resistance. The flake graphite can also improve the electrical conductivity, the flake graphite and the silicon carbide whisker can improve the thermal conductivity of the tread rubber, and under the condition of reducing the carbon black consumption, the tread rubber can not rub with the ground to generate a dark black print in the use process, thereby protecting the surrounding environment.
Test example 1
The test is divided into 7 groups, wherein each group comprises 500g of natural rubber reclaimed rubber, 5g of zinc oxide, 1g of stearic acid, 0g of anti-aging agent 4011 g, 10g of plasticizer, 60g of carbon black and 44g of modified crystalline flake graphite. The modified crystalline flake graphite in each group is prepared by the following method:
test 1 group: and crystalline flake graphite and silicon carbide whiskers are not added.
Test 2 group: 40g of crystalline flake graphite and 4g of silicon carbide whisker are mixed to obtain modified crystalline flake graphite.
Test 3 group: 40g of crystalline flake graphite and 4g of silicon carbide whisker are dispersed in 220g of sodium dodecyl benzene sulfonate solution, and the modified crystalline flake graphite is obtained by ultrasonic treatment for 20min, wherein the ultrasonic power is 300W and the frequency is 40 KHz.
Test 4 groups: 40g of crystalline flake graphite and 4g of silicon carbide whisker are added into 0.2moL/L sodium hydroxide solution, and the mixture is heated at 50 ℃ for reaction for 20min, and then the modified crystalline flake graphite is obtained after suction filtration and drying.
Test 5 group: 40g of crystalline flake graphite and 4g of silicon carbide whisker are added into 0.2moL/L sodium hydroxide solution, and the mixture is heated at 50 ℃ for reaction for 20min, and then is filtered and dried to obtain solid. And dispersing the solid into 220g of sodium dodecyl benzene sulfonate solution, and carrying out ultrasonic treatment for 20min, wherein the ultrasonic power is 300W and the frequency is 40KHz, so as to obtain the modified crystalline flake graphite.
Test 6 groups: 40g of crystalline flake graphite and 4g of silicon carbide whisker are added into 0.2moL/L sodium hydroxide solution, heated at 50 ℃ and added with 4.4g of cetyltrimethylammonium chloride for four times under stirring, and after reacting for 20min, the crystalline flake graphite is obtained after suction filtration and drying.
Test 7 groups: 40g of crystalline flake graphite and 4g of silicon carbide whisker are added into 0.2moL/L sodium hydroxide solution, heated at 50 ℃ and added with 4.4g of cetyltrimethylammonium chloride for four times under stirring, and after reacting for 20min, the solid is obtained after suction filtration and drying. And dispersing the solid into 220g of sodium dodecyl benzene sulfonate solution, and carrying out ultrasonic treatment for 20min, wherein the ultrasonic power is 300W and the frequency is 40KHz, so as to obtain the modified crystalline flake graphite.
The modified crystalline flake graphite and other raw materials of the test group are respectively recorded as test 1 group to test 7 group, each group is respectively mixed by an open mill, the temperature of the open mill is 120 ℃, the open mill time is 30min, and then the mixture is injected into a die (silicone oil-coated release agent is coated in the die), the die temperature is 130 ℃, and the heat preservation is carried out for 30min. After cooling, the samples were taken out and pressed to test the mechanical strength and abrasion resistance (5 samples per group, averaged). The results obtained are shown in Table 1.
Tensile strength: the tensile strength of the tread rubber was tested according to GB/T528-2009 determination of tensile stress Strain Properties of vulcanized rubber or thermoplastic rubber.
Elongation at break: the elongation at break of the tread rubber was tested according to GB/T528-2009 determination of tensile stress Strain Properties of vulcanized rubber or thermoplastic rubber.
Abrasion resistance: the wear resistance of the tread rubber was tested according to astm d1630-2006 standard test method for wear resistance of rubber.
TABLE 1
| Test item | Tensile strength MPa | Elongation at break% | Wear resistance mm 3 |
| Test 1 group | 25.3 | 459 | 29 |
| Test 2 groups | 26.7 | 483 | 31 |
| Test 3 groups | 28.1 | 499 | 36 |
| Test 4 groups | 27.3 | 487 | 36 |
| Test 5 groups | 29.2 | 503 | 43 |
| Test 6 groups | 27.9 | 481 | 38 |
| Test 7 groups | 31.4 | 521 | 49 |
As can be seen from table 1, the crystalline flake graphite and the silicon carbide whisker are formed into crystalline flake graphite-silicon carbide whisker by hydrogen bonding only through treatment, sodium dodecyl benzene sulfonate is not added, the dispersibility of the crystalline flake graphite-silicon carbide whisker in the tread rubber is poor, and the mechanical property of the tread rubber is difficult to be greatly improved. The crystalline flake graphite and the silicon carbide whisker are not combined through hydrogen bonds only by using sodium dodecyl benzene sulfonate for treatment, and the wear resistance is not greatly improved although the strength and other performances can also be improved. The fact that the flake graphite and the silicon carbide whisker can improve the wear resistance of the tread rubber through hydrogen bonding is shown, and the wear resistance of the tread rubber can be greatly improved after the tread rubber is further treated by sodium dodecyl benzene sulfonate.
In order to enable those skilled in the art to more clearly understand the technical solutions of the present application, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The natural rubber reclaimed rubber can be purchased from commercial products, and can also be prepared according to the method disclosed in the application number CN201910454853.5 for the rubber for the high-bearing solid tire and the preparation method thereof, and the method specifically comprises the following steps:
(1) taking waste tires made of natural rubber, removing steel wires and curtain cloth, and crushing the waste tires at normal temperature to obtain waste rubber powder with fineness of 15 meshes;
(2) stirring waste rubber powder, operating oil and a regenerant (selected from preparation example 1 of the regenerant) in a weight ratio of 4:2:1 for 5min at a temperature of 40 ℃, and then soaking for 1h under the conditions of a pressure of 1.5MPa and a temperature of 140 ℃ to obtain pretreated waste rubber powder;
(3) the waste rubber powder is subjected to microwave activation for 1min under the condition that the microwave frequency is 2450MHz and the radiation power is 675W;
(4) and (3) mixing the waste rubber powder at the temperature of 120 ℃ for 10min to obtain reclaimed rubber.
Coumarone is purchased from Shandong Baihong New Material Co., ltd, under the HK designation.
Carbon black was purchased from Tianjin Hua Yuan chemical technology Co., ltd and is available under the designation N339.
The flake graphite is purchased from a double dragon mineral product processing plant in the Ming county of Lingshou, the fineness of the product is 1250 meshes, and the carbon content is more than or equal to 95 percent.
Silicon carbide whiskers were purchased from Xu Zhoujie innovative materials technologies, inc., diameter: 0.1-1 μm, length: 5-30 μm.
The test materials used in the examples of the present invention are all conventional in the art and are commercially available.
Example 1: preparation of modified flake graphite
4kg of crystalline flake graphite and 0.4kg of silicon carbide whisker are added into 0.2moL/L sodium hydroxide solution, heated at 50 ℃ and added with 0.44kg of cetyltrimethylammonium chloride for four times under stirring, and after reacting for 20min, the solid is obtained after suction filtration and drying. And dispersing the solid into 33kg of sodium dodecyl benzene sulfonate solution, and carrying out ultrasonic treatment for 20min, wherein the ultrasonic power is 300W and the frequency is 40KHz, so as to obtain the modified crystalline flake graphite.
Example 2
45kg of natural rubber reclaimed rubber (prepared according to the method in application number CN 201910454853.5), 0.5kg of zinc oxide, 0.1kg of stearic acid, 0.2kg of anti-aging agent 4010 and 0.1kg of anti-aging agent A and 1.0kg of coumarone resin are mixed for primary banburying, wherein the temperature of the primary banburying is 120 ℃ and the time is 12min. 7kg of carbon black and 4kg of modified crystalline flake graphite prepared in accordance with the method of example 1 were further added to conduct secondary banburying. The temperature of the secondary banburying is 110 ℃ and the time is 5min. And (3) after blanking, boiling off, wherein the temperature of mixing is 110 ℃, the time is 10min, and cooling the obtained sheet to obtain the tread rubber.
Example 3
50kg of natural rubber reclaimed rubber (prepared according to the method in application number CN 201910454853.5), 0.75kg of zinc oxide, 0.2kg of stearic acid, 0.3kg of anti-aging agent 4010NA and 0.2kg of anti-aging agent A and 1.5kg of coumarone resin are mixed for primary banburying, wherein the temperature of the primary banburying is 120 ℃ and the time is 13min. 7kg of carbon black and 4kg of modified crystalline flake graphite prepared in accordance with the method of example 1 were further added to conduct secondary banburying. The temperature of the secondary banburying is 110 ℃ and the time is 6min. And (3) after blanking, boiling off, wherein the temperature of mixing is 110 ℃, the time is 10min, and cooling the obtained sheet to obtain the tread rubber.
Example 4
60kg of natural rubber reclaimed rubber (prepared according to the method in application number CN 201910454853.5), 1.0kg of zinc oxide, 0.3kg of stearic acid, 0.5kg of anti-aging agent 4010 and 0.3kg of anti-aging agent RD, and 1.6kg of coumarone resin are mixed for primary banburying, wherein the temperature of the primary banburying is 130 ℃ and the time is 10min. 8kg of carbon black and 4.4kg of modified crystalline flake graphite prepared in accordance with the method of example 1 were further added to conduct secondary banburying. The temperature of the secondary banburying is 110 ℃ and the time is 7min. And (3) after blanking, boiling off, wherein the temperature of mixing is 110 ℃, the time is 10min, and cooling the obtained sheet to obtain the tread rubber.
Comparative example 1
The difference from example 3 is that: no modified crystalline flake graphite is added.
Comparative example 2
The difference from example 3 is that:
the modified crystalline flake graphite is obtained by dispersing 4kg of crystalline flake graphite into 30kg of sodium dodecyl benzene sulfonate solution and performing ultrasonic treatment for 20 min.
Comparative example 3
The difference from example 3 is that:
and the modified silicon carbide whisker is used for replacing the modified crystalline flake graphite without adding crystalline flake graphite. 0.4kg of silicon carbide whisker is added into 3kg of sodium dodecyl benzene sulfonate solution, and the modified silicon carbide whisker is obtained after ultrasonic treatment for 20 min.
Comparative example 4
The difference from example 3 is that:
the silicon carbide whiskers were replaced with calcium carbonate whiskers.
Test example 2
The tread rubbers prepared in examples 2 to 4 and comparative examples 1 to 4 were prepared as in test example 1, and the remaining samples were prepared to have a specification of 100mm×100mm×20mm, except that the test standards had a sample specification specified clearly. The tensile strength, abrasion resistance, thermal conductivity and antistatic property of the above samples were tested, and the results are shown in Table 2.
The tensile strength and the wear resistance were measured in the same manner as in test example 1;
the thermal conductivity is measured by a quasi-steady state method specific heat conductivity tester, the thermal conductivity is characterized by the thermal conductivity, and the higher the thermal conductivity is, the better the thermal conductivity is;
antistatic test antistatic properties are characterized by resistance as measured according to standard GB/T11210-2014 "determination of resistance of antistatic and conductive articles of vulcanized rubber or thermoplastic rubber": the test environment temperature is (23+/-2) DEG C, the relative humidity is (50+/-5)%, and the smaller the resistance is, the better the antistatic property is.
TABLE 2
As can be seen from table 2, the use of flake graphite alone or silicon carbide whiskers alone does not significantly improve the mechanical properties as well as the thermal and electrical conductivity properties of the tread band. The silicon carbide whisker is replaced by the calcium carbonate whisker, the mechanical property and the heat and electric conductivity are not remarkably improved, and the high wear resistance, the high heat conductivity and the high electric conductivity can be realized by increasing the consumption of carbon black or modified crystalline flake graphite. The tread rubber prepared in examples 2-4 has obviously improved mechanical properties and heat and electrical conductivity, can reduce the carbon black consumption and prolong the service life of the tread rubber.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.
Claims (4)
1. The solid tire tread rubber is characterized by comprising the following raw materials in parts by weight:
45-60 parts of natural rubber reclaimed rubber, 0.5-1.0 part of zinc oxide, 0.1-0.3 part of stearic acid, 0.1-1.0 part of an anti-aging agent, 0.5-2 parts of a plasticizer, 5-15 parts of carbon black and 3-5 parts of modified crystalline flake graphite;
the modified crystalline flake graphite comprises crystalline flake graphite and silicon carbide whiskers, and the mass ratio of the crystalline flake graphite to the silicon carbide whiskers is 10: (0.5-1);
the modified crystalline flake graphite is prepared by the following method:
(1) Adding flake graphite and silicon carbide whisker into alkali liquor, heating, adding hexadecyl trimethyl ammonium chloride for multiple times under stirring, and after the reaction, carrying out suction filtration and drying to obtain a solid; the alkali liquor is sodium hydroxide solution or potassium hydroxide solution, and the concentration of the alkali liquor is 0.1-0.3 mol/L; the mass ratio of the total mass of the crystalline flake graphite and the silicon carbide crystal to the alkali liquor and the hexadecyl trimethyl ammonium chloride is 1:10:0.1; the heating temperature is 40-60 ℃, and the heating time is 10-30 min;
(2) Adding the solid into sodium dodecyl benzene sulfonate solution for ultrasonic treatment, filtering and drying to obtain modified crystalline flake graphite; the mass ratio of the solid to the sodium dodecyl benzene sulfonate solution is 1: (5-10); the concentration of the sodium dodecyl benzene sulfonate solution is 25g/L; the ultrasonic treatment time is 10-30 min.
2. The method for preparing the tread rubber for the solid tire according to claim 1, wherein the method for preparing comprises the following steps:
mixing the natural rubber reclaimed rubber with zinc oxide, stearic acid, an anti-aging agent and a plasticizer for primary banburying, adding carbon black and modified crystalline flake graphite for secondary banburying, blanking, then opening, discharging and cooling to obtain the tread rubber.
3. The preparation method according to claim 2, wherein the temperature of the primary internal mixing is 120-130 ℃ and the time is 10-13 min; the temperature of the secondary banburying is 100-110 ℃ and the time is 3-7 min.
4. The preparation method according to claim 2, wherein the temperature of the open mill is 100-110 ℃ and the time is 10-15 min.
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| CN110128723A (en) * | 2019-05-29 | 2019-08-16 | 浙江通超工贸有限公司 | A kind of high-mechanic solid tyre rubber and preparation method thereof |
| WO2023024250A1 (en) * | 2021-08-24 | 2023-03-02 | 青岛科技大学 | High wear-resistant tire tread rubber and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108239306B (en) * | 2017-12-11 | 2020-08-11 | 山东玲珑轮胎股份有限公司 | Tire sidewall rubber composite material and preparation method thereof |
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|---|---|---|---|---|
| KR20000055447A (en) * | 1999-02-06 | 2000-09-05 | 한종웅 | method for forming canbon brick with fire resistance and corrosion resestance |
| CN108587143A (en) * | 2018-03-29 | 2018-09-28 | 深圳市富恒新材料股份有限公司 | A kind of high heat conduction PA6-Surlyn resin composite materials and preparation method thereof |
| CN109824961A (en) * | 2019-03-01 | 2019-05-31 | 江苏锵尼玛新材料股份有限公司 | A kind of cut resistant, creep resistance UHMWPE fiber and preparation method thereof |
| CN110128723A (en) * | 2019-05-29 | 2019-08-16 | 浙江通超工贸有限公司 | A kind of high-mechanic solid tyre rubber and preparation method thereof |
| WO2023024250A1 (en) * | 2021-08-24 | 2023-03-02 | 青岛科技大学 | High wear-resistant tire tread rubber and preparation method therefor |
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