CN110862623A - Graphene-containing aircraft tire sealing layer rubber material and preparation method thereof - Google Patents
Graphene-containing aircraft tire sealing layer rubber material and preparation method thereof Download PDFInfo
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- 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
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L23/28—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds
- C08L23/283—Iso-olefin halogenated homopolymers or copolymers
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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- 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
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- 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
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses an aviation tire sealing layer rubber material containing graphene and a preparation method thereof, wherein the rubber material comprises the following raw materials in parts by weight: 50-100 parts of halogenated butyl rubber, 0-50 parts of synthetic rubber, 40-80 parts of carbon black filler, 1-10 parts of graphene, 10-30 parts of flaky mineral, 0.5-3 parts of acid acceptor, 4-20 parts of processing aid, 0-5 parts of anti-aging agent, 2-5 parts of tackifying resin, 1.5-5 parts of vulcanizing agent and 1-2.5 parts of vulcanization accelerator. The aviation tire sealing layer adhesive with good physical properties, good air tightness, thermal aging resistance and aging and cracking resistance is designed by adding the graphene, the flaky minerals and other material varieties and reasonable formula proportion; the rubber material has simple components, easily obtained raw materials and convenient manufacture and implementation. The sealing layer is applied to the aircraft tire, so that the permeability of inflation gas of the aircraft tire can be greatly reduced, the pressure maintaining performance of the aircraft tire is improved, the safety of the aircraft tire is improved, and the service life of the aircraft tire is prolonged.
Description
Technical Field
The invention belongs to the field of tire processing, and particularly relates to an aviation tire sealing layer rubber material containing graphene and a preparation method thereof.
Background
At present, most aviation tire sealing layer rubber compounds mainly use halogenated butyl rubber and partial natural rubber and styrene-butadiene rubber materials, and fillers mainly use N330, N326 and N660 carbon black. The rubber material generally has a series of problems of easy aging, low heat resistance, weak pressure retention, short service life and the like, and influences the use of the aircraft tire.
Halogenated (brominated or chlorinated) butyl rubber is rubber with better stability, has the characteristics of excellent ozone resistance, weather aging resistance, temperature resistance, good air tightness and the like, can improve the air permeability resistance of rubber materials by increasing the using amount of the halogenated (brominated or chlorinated) butyl rubber, has certain difference in pressure maintaining performance of tires or aircrafts with high pressure maintaining performance by only increasing the using amount of the halogenated butyl rubber, and needs to be improved by a filling agent.
Disclosure of Invention
The invention provides an aviation tire sealing layer rubber material containing graphene and a preparation method thereof, aiming at the situations, the rubber material is convenient to manufacture and implement, has good physical properties, good air tightness, heat aging resistance and aging cracking resistance, is applied to an aviation tire as a sealing layer, can greatly reduce the permeability of inflation gas of the aviation tire, maintains the pressure stability of the tire, improves the safety of the aviation tire and prolongs the service life of the aviation tire.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the graphene-containing aircraft tire sealing layer rubber material comprises the following raw materials in parts by weight:
50-100 parts of halogenated butyl rubber, 0-50 parts of synthetic rubber, 40-80 parts of carbon black filler, 1-10 parts of graphene, 10-30 parts of flaky mineral, 0.5-3 parts of acid acceptor, 4-20 parts of processing aid, 0-5 parts of anti-aging agent, 2-5 parts of tackifying resin, 1.5-5 parts of vulcanizing agent and 1-2.5 parts of vulcanization accelerator.
Further, the graphene is graphene oxide with a sheet structure, and is a two-dimensional carbon material formed by stacking 10 layers of carbon atoms which are periodically and closely stacked in a hexagonal honeycomb structure in different stacking modes, the thermal conductivity is 850W/(m × k), and the average particle size is 10-30 μm.
Further, the flaky mineral is talcum powder or flaky clay with a flaky structure, and the flaky mineral is singly used or used by combining the talcum powder and the flaky clay; the average diameter of the lamella is 300-500nm (TEM), the average thickness of the lamella is 20-50nm (TEM), and the specific surface area is 30-50m2/g。
Graphene is a nano filler with a lamellar structure which is subjected to lamellar stripping after oxidation, and has excellent mechanical, heat conduction and electric conductivity, and better gas barrier property than carbon black. The flaky mineral fillers such as the flaky argil and the flaky talcum powder also have a lamellar structure and better gas barrier property, but the mineral fillers can reduce the electric conductivity and the heat conductivity of the rubber material and reduce the antistatic capability of the tire. If the dosage of halogenated butyl rubber is increased in the aircraft tire sealing layer rubber and graphene and flaky mineral filler are added in the filler, the air permeability resistance of the sealing layer rubber is greatly improved without reducing the antistatic capacity of the sealing layer rubber.
Preferably, the sizing material comprises the following components in parts by weight:
50 parts of halogenated butyl rubber, 20 parts of natural rubber, 30 parts of styrene butadiene rubber, 66030 parts of carbon black, N32625 parts of carbon black, 5 parts of graphene, 10 parts of flake mineral, 2 parts of active magnesium oxide, 5 parts of naphthenic oil, 1 part of stearic acid, 806 parts of zinc oxide, 2 parts of an anti-aging agent TMQ, 2 parts of anti-aging agent 6PPD, 2042 parts of tackifying resin, 603 parts of sulfur IS-603, 1.5 parts of a promoter CZ, 0.8 part of a promoter DM and 0.3 part of a promoter TMTD.
Preferably, the sizing material comprises the following components in parts by weight:
70 parts of halogenated butyl rubber, 10 parts of natural rubber, 20 parts of styrene butadiene rubber, 66050 parts of carbon black, 3 parts of graphene, 15 parts of flake mineral, 3 parts of active magnesium oxide, 8 parts of naphthenic oil, 3 parts of stearic acid, zinc oxide-804 parts, 1.5 parts of antioxidant TMQ, 1.5 parts of antioxidant 6PPD, 2043 parts of tackifying resin, 601 parts of sulfur IS-601, 0.5 part of accelerator CZ, 1 part of accelerator DM and 0.5 part of accelerator TMTD.
Preferably, the sizing material comprises the following components in parts by weight:
80 parts of halogenated butyl rubber, 20 parts of natural rubber, 66050 parts of carbon black, 10 parts of graphene, 20 parts of flake mineral, 4 parts of active magnesium oxide, 8 parts of naphthenic oil, 3 parts of stearic acid, 805 parts of zinc oxide, 1.5 parts of an anti-aging agent TMQ, 1.5 parts of anti-aging agent 6PPD, 2044 parts of tackifying resin, 601 parts of sulfur IS-601, 0.6 part of accelerator CZ, 1.2 parts of accelerator DM and 0.2 part of accelerator TMTD.
Preferably, the sizing material comprises the following components in parts by weight:
100 parts of halogenated butyl rubber, 5 parts of carbon black N66040, 5 parts of graphene, 30 parts of flake mineral, 2 parts of active magnesium oxide, 10 parts of naphthenic oil, 5 parts of stearic acid, zinc oxide-803.75 parts, 1 part of anti-aging agent TMQ, 1 part of anti-aging agent 6PPD, 2045 parts of tackifying resin, 600.5 parts of sulfur IS-5, 1.5 parts of accelerator DM and 1 part of accelerator TMTD.
The halogenated butyl rubber is brominated butyl rubber or chlorinated butyl rubber, the air permeability resistance of the halogenated butyl rubber and the chlorinated butyl rubber is basically the same, the vulcanization speed of the chlorinated butyl rubber is slower than that of the brominated butyl rubber, the chlorinated butyl rubber and the brominated butyl rubber can obtain proper sulfur speed only by adjusting the vulcanization accelerator, and the required rubber material performance can be obtained without adjusting other components. Either or both of the brominated butyl rubber and the chlorinated butyl rubber may be used alone.
The synthetic rubber of the invention refers to natural rubber and styrene butadiene rubber, and can be used singly or in combination.
The carbon black filler of the present invention is one of general carbon black, quick-pressing carbon black, semi-reinforcing carbon black, and the like, and may be used in combination of a plurality of types. The carbon black is easy to be mixed and processed during processing, and the vulcanized rubber has good elasticity, low heat generation and good dynamic performance.
The acid acceptor of the invention is active magnesium oxide.
The processing aid is one or more of a homogenizing agent (aromatic hydrocarbon resin mixture), hole cyan, coumarone resin, aromatic oil, pine tar, naphthenic oil and the like; the homogenizing agent comprises 40MSF, 145A, RH-100, etc.
The anti-aging agent is N- (1, 3-dimethylbutyl) N/-phenyl p-phenylenediamine (6PPD) and 2,2, 4-trimethyl-1, 2-dihydroquinoline polymer (TMQ). The protective system adopts the antioxidant TMQ, the protective wax and the antioxidant 6PPD, has excellent antioxidant, ozone resistance and flex resistance, has better protective effect on weather aging, has passivation effect on variable-valence metals, and can protect the rubber shock pad which needs to be used for a long time.
The tackifying resin of the invention is octyl phenolic resin, tert-butyl phenolic resin, such as 203, 204 resin and the like.
The vulcanizing agents are zinc oxide and sulfur, and the sulfur can be common sulfur and insoluble sulfur or oil-extended sulfur. The using amount of the zinc oxide is 1-8 parts, and the zinc oxide is preferably zinc oxide-80 of pre-dispersed masterbatch for the zinc oxide; the usage amount of the sulfur is 0-3 parts.
The vulcanization accelerator provided by the invention is dibenzothiazyl Disulfide (DM), 2-mercaptobenzothiazole (M) and thiuram disulfide (TMTD), and can be used singly or in combination in an amount of 1-3 parts.
The preparation method of the graphene-containing aircraft tire sealing layer rubber material adopts an internal mixer two-stage mixing method, and comprises the following steps:
firstly, mixing halogenated butyl rubber, carbon black, graphene, a flaky mineral material and other materials to obtain a master batch;
and secondly, putting the master batch into the internal mixer again, adding a vulcanizing agent and an accelerant at a lower temperature, and mixing to obtain the final rubber.
Compared with the prior formula technology, the aviation tire sealing layer rubber material containing graphene is characterized in that one or more aviation tire sealing layer rubbers with good physical properties, good air tightness, thermal aging resistance and aging cracking resistance are designed by adding graphene, flaky mineral fillers and other material varieties and reasonable formula proportion and through mutual matching of the components; the rubber material has simple components, easily obtained raw materials and convenient manufacture and implementation. The sealing layer is applied to the aircraft tire, the permeability of inflation gas of the aircraft tire can be greatly reduced, the pressure stability of the tire is maintained, the air tightness and the pressure maintaining performance of the aircraft tire are thoroughly improved, the safety of the tire is improved, and the service life of the aircraft tire is prolonged.
Detailed Description
The graphene-containing aircraft tire sealing layer rubber material comprises the following raw materials in parts by weight:
50-100 parts of halogenated butyl rubber, 0-50 parts of synthetic rubber, 40-80 parts of carbon black filler, 1-10 parts of graphene, 10-30 parts of flaky mineral, 0.5-3 parts of acid acceptor, 4-20 parts of processing aid, 0-5 parts of anti-aging agent, 2-5 parts of tackifying resin, 1.5-5 parts of vulcanizing agent and 1-2.5 parts of vulcanization accelerator.
The preparation method of the graphene-containing aircraft tire sealing layer rubber material adopts an internal mixer two-stage mixing method, and comprises the following steps:
firstly, mixing halogenated butyl rubber, carbon black, graphene, a flaky mineral material and other materials to obtain a master batch;
and secondly, putting the master batch into the internal mixer again, adding a vulcanizing agent and an accelerant at a lower temperature, and mixing to obtain the final rubber.
The invention is further illustrated by the following examples, which are not intended to be limiting.
Example 1:
the graphene-containing aircraft tire sealing layer rubber material comprises the following raw materials in parts by weight:
50 parts of halogenated butyl rubber, 20 parts of natural rubber, 30 parts of styrene butadiene rubber, 66030 parts of carbon black, N32625 parts of carbon black, 5 parts of graphene, 10 parts of flake mineral, 2 parts of active magnesium oxide, 5 parts of naphthenic oil, 1 part of stearic acid, 806 parts of zinc oxide, 2 parts of an anti-aging agent TMQ, 2 parts of anti-aging agent 6PPD, 2042 parts of tackifying resin, 603 parts of sulfur IS-603, 1.5 parts of a promoter CZ, 0.8 part of a promoter DM and 0.3 part of a promoter TMTD.
The preparation method of the graphene-containing aircraft tire sealing layer rubber material adopts an internal mixer two-stage mixing method, and comprises the following steps:
step 1, master batch mixing: setting the rotating speed of an internal mixer to be 50rpm, adding halogenated butyl rubber, carbon black, graphene and a flaky mineral material into the internal mixer, mixing for 60 seconds, adding operating oil, mixing to 120 seconds, adding stearic acid, a processing aid and a magnesium oxide aid, mixing to 170 seconds, extracting a bolt, pressing the bolt to 240 seconds, discharging to obtain a master batch, and controlling the rubber discharge temperature to be below 130 ℃;
step 2, final mixing: setting the rotating speed of an internal mixer to be 30rpm, adding master batch into the internal mixer, mixing for 30s, adding zinc oxide, sulfur and an accelerator, mixing to 70s, extracting suppository, then pressing the suppository to 120s, discharging to obtain final rubber, and controlling the rubber discharging temperature to be below 105 ℃.
The process is carried out by adopting GK250 internal mixer, or other internal mixers, and determining the amount of the mixed rubber according to the volume of an internal mixing chamber of the internal mixer.
Example 2:
the graphene-containing aircraft tire sealing layer rubber material comprises the following raw materials in parts by weight:
70 parts of halogenated butyl rubber, 10 parts of natural rubber, 20 parts of styrene butadiene rubber, 66050 parts of carbon black, 3 parts of graphene, 15 parts of flake mineral, 3 parts of active magnesium oxide, 8 parts of naphthenic oil, 3 parts of stearic acid, zinc oxide-804 parts, 1.5 parts of antioxidant TMQ, 1.5 parts of antioxidant 6PPD, 2043 parts of tackifying resin, 601 parts of sulfur IS-601, 0.5 part of accelerator CZ, 1 part of accelerator DM and 0.5 part of accelerator TMTD.
The rest is the same as example 1.
Example 3:
the graphene-containing aircraft tire sealing layer rubber material comprises the following raw materials in parts by weight:
80 parts of halogenated butyl rubber, 20 parts of natural rubber, 66050 parts of carbon black, 10 parts of graphene, 20 parts of flake mineral, 4 parts of active magnesium oxide, 8 parts of naphthenic oil, 3 parts of stearic acid, 805 parts of zinc oxide, 1.5 parts of an anti-aging agent TMQ, 1.5 parts of anti-aging agent 6PPD, 2044 parts of tackifying resin, 601 parts of sulfur IS-601, 0.6 part of accelerator CZ, 1.2 parts of accelerator DM and 0.2 part of accelerator TMTD.
The rest is the same as example 1.
Example 4:
the graphene-containing aircraft tire sealing layer rubber material comprises the following raw materials in parts by weight:
100 parts of halogenated butyl rubber, 5 parts of carbon black N66040, 5 parts of graphene, 30 parts of flake mineral, 2 parts of active magnesium oxide, 10 parts of naphthenic oil, 5 parts of stearic acid, zinc oxide-803.75 parts, 1 part of anti-aging agent TMQ, 1 part of anti-aging agent 6PPD, 2045 parts of tackifying resin, 600.5 parts of sulfur IS-5, 1.5 parts of accelerator DM and 1 part of accelerator TMTD.
The rest is the same as example 1.
The compounds obtained in examples 1 to 4 and comparative example above were subjected to performance tests, the results of which are listed in table 1. The formulation of the comparative example contained no graphene and no plate-like minerals.
TABLE 1 results of Performance test of examples 1-4 and comparative examples
As can be seen from Table 1, examples 1 to 4 all are superior to comparative examples in air-tightness, heat resistance and ozone aging cracking resistance.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. The graphene-containing aircraft tire sealing layer rubber material is characterized by comprising the following raw materials in parts by weight:
50-100 parts of halogenated butyl rubber, 0-50 parts of synthetic rubber, 40-80 parts of carbon black filler, 1-10 parts of graphene, 10-30 parts of flaky mineral, 0.5-3 parts of acid acceptor, 4-20 parts of processing aid, 0-5 parts of anti-aging agent, 2-5 parts of tackifying resin, 1.5-5 parts of vulcanizing agent and 1-2.5 parts of vulcanization accelerator.
2. The graphene-containing aircraft tire sealant layer compound according to claim 1, wherein the graphene is graphene oxide having a sheet structure, and is a two-dimensional carbon material consisting of 10 layers of carbon atoms stacked in different stacking manners, wherein the carbon atoms are periodically and closely packed in a hexagonal honeycomb structure, and the average particle size is 10-30 μm.
3. The graphene-containing aircraft tire sealant layer compound according to claim 1, wherein the flake mineral is talc or flake clay having a flake structure, used alone or in combination; the average diameter of the lamella is 300-500nm (TEM), the average thickness of the lamella is 20-50nm (TEM), and the specific surface area is 30-50m2/g。
4. The graphene-containing aircraft tire sealing layer rubber compound according to claim 1, wherein the rubber compound raw material comprises the following components in parts by weight:
50 parts of halogenated butyl rubber, 20 parts of natural rubber, 30 parts of styrene butadiene rubber, 66030 parts of carbon black, N32625 parts of carbon black, 5 parts of graphene, 10 parts of flake mineral, 2 parts of active magnesium oxide, 5 parts of naphthenic oil, 1 part of stearic acid, 806 parts of zinc oxide, 2 parts of an anti-aging agent TMQ, 2 parts of anti-aging agent 6PPD, 2042 parts of tackifying resin, 603 parts of sulfur IS-603, 1.5 parts of a promoter CZ, 0.8 part of a promoter DM and 0.3 part of a promoter TMTD.
5. The graphene-containing aircraft tire sealing layer rubber compound according to claim 1, wherein the rubber compound raw material comprises the following components in parts by weight:
70 parts of halogenated butyl rubber, 10 parts of natural rubber, 20 parts of styrene butadiene rubber, 66050 parts of carbon black, 3 parts of graphene, 15 parts of flake mineral, 3 parts of active magnesium oxide, 8 parts of naphthenic oil, 3 parts of stearic acid, zinc oxide-804 parts, 1.5 parts of antioxidant TMQ, 1.5 parts of antioxidant 6PPD, 2043 parts of tackifying resin, 601 parts of sulfur IS-601, 0.5 part of accelerator CZ, 1 part of accelerator DM and 0.5 part of accelerator TMTD.
6. The graphene-containing aircraft tire sealing layer rubber compound according to claim 1, wherein the rubber compound raw material comprises the following components in parts by weight:
80 parts of halogenated butyl rubber, 20 parts of natural rubber, 66050 parts of carbon black, 10 parts of graphene, 20 parts of flake mineral, 4 parts of active magnesium oxide, 8 parts of naphthenic oil, 3 parts of stearic acid, 805 parts of zinc oxide, 1.5 parts of an anti-aging agent TMQ, 1.5 parts of anti-aging agent 6PPD, 2044 parts of tackifying resin, 601 parts of sulfur IS-601, 0.6 part of accelerator CZ, 1.2 parts of accelerator DM and 0.2 part of accelerator TMTD.
7. The graphene-containing aircraft tire sealing layer rubber compound according to claim 1, wherein the rubber compound raw material comprises the following components in parts by weight:
100 parts of halogenated butyl rubber, 5 parts of carbon black N66040, 5 parts of graphene, 30 parts of flake mineral, 2 parts of active magnesium oxide, 10 parts of naphthenic oil, 5 parts of stearic acid, zinc oxide-803.75 parts, 1 part of anti-aging agent TMQ, 1 part of anti-aging agent 6PPD, 2045 parts of tackifying resin, 600.5 parts of sulfur IS-5, 1.5 parts of accelerator DM and 1 part of accelerator TMTD.
8. The preparation method of the graphene-containing aircraft tire sealing layer rubber compound as claimed in any one of claims 1 to 7, wherein the preparation method adopts an internal mixer two-stage mixing method, and comprises the following steps:
step 1, master batch mixing: setting the rotating speed of an internal mixer to be 50rpm, adding halogenated butyl rubber, carbon black, graphene and a flaky mineral material into the internal mixer, mixing for 60 seconds, adding operating oil, mixing to 120 seconds, adding stearic acid, a processing aid and a magnesium oxide aid, mixing to 170 seconds, extracting a bolt, pressing the bolt to 240 seconds, discharging to obtain a master batch, and controlling the rubber discharge temperature to be below 130 ℃;
step 2, final mixing: setting the rotating speed of an internal mixer to be 30rpm, adding master batch into the internal mixer, mixing for 30s, adding zinc oxide, sulfur and an accelerator, mixing to 70s, extracting suppository, then pressing the suppository to 120s, discharging to obtain final rubber, and controlling the rubber discharging temperature to be below 105 ℃.
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Application publication date: 20200306 |