CN116144120A - Preparation method of self-sealing sizing material, self-sealing sizing material and application thereof - Google Patents
Preparation method of self-sealing sizing material, self-sealing sizing material and application thereof Download PDFInfo
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- CN116144120A CN116144120A CN202310041203.4A CN202310041203A CN116144120A CN 116144120 A CN116144120 A CN 116144120A CN 202310041203 A CN202310041203 A CN 202310041203A CN 116144120 A CN116144120 A CN 116144120A
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- 239000000463 material Substances 0.000 title claims abstract description 112
- 238000007789 sealing Methods 0.000 title claims abstract description 79
- 238000004513 sizing Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 229920001971 elastomer Polymers 0.000 claims abstract description 107
- 239000005060 rubber Substances 0.000 claims abstract description 107
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- 239000002904 solvent Substances 0.000 claims abstract description 40
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- 239000003292 glue Substances 0.000 claims abstract description 33
- 150000001875 compounds Chemical class 0.000 claims abstract description 31
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- 238000003756 stirring Methods 0.000 claims description 40
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- 239000003795 chemical substances by application Substances 0.000 claims description 21
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- -1 alkyl peroxide Chemical class 0.000 claims description 18
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 16
- 239000003921 oil Substances 0.000 claims description 16
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- 229920005549 butyl rubber Polymers 0.000 claims description 11
- RIIPKNZLLQVCRR-UHFFFAOYSA-N formaldehyde;2-(2,4,4-trimethylpentan-2-yl)phenol Chemical compound O=C.CC(C)(C)CC(C)(C)C1=CC=CC=C1O RIIPKNZLLQVCRR-UHFFFAOYSA-N 0.000 claims description 11
- 238000004132 cross linking Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- DZCCLNYLUGNUKQ-UHFFFAOYSA-N n-(4-nitrosophenyl)hydroxylamine Chemical compound ONC1=CC=C(N=O)C=C1 DZCCLNYLUGNUKQ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011787 zinc oxide Substances 0.000 claims description 9
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 8
- 239000012936 vulcanization activator Substances 0.000 claims description 8
- MKZXROSCOHNKDX-UHFFFAOYSA-N 1,4-dinitrosobenzene Chemical compound O=NC1=CC=C(N=O)C=C1 MKZXROSCOHNKDX-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- 150000001451 organic peroxides Chemical class 0.000 claims description 6
- 239000003208 petroleum Substances 0.000 claims description 6
- LZDOYVMSNJBLIM-UHFFFAOYSA-N 4-tert-butylphenol;formaldehyde Chemical compound O=C.CC(C)(C)C1=CC=C(O)C=C1 LZDOYVMSNJBLIM-UHFFFAOYSA-N 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 5
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 5
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims description 4
- UHBGYFCCKRAEHA-UHFFFAOYSA-N P-toluamide Chemical compound CC1=CC=C(C(N)=O)C=C1 UHBGYFCCKRAEHA-UHFFFAOYSA-N 0.000 claims description 4
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 claims description 3
- 239000005062 Polybutadiene Substances 0.000 claims description 3
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 229920005557 bromobutyl Polymers 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 229920005556 chlorobutyl Polymers 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910000464 lead oxide Inorganic materials 0.000 claims description 3
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 3
- 229920002857 polybutadiene Polymers 0.000 claims description 3
- 229920001195 polyisoprene Polymers 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- OKISUZLXOYGIFP-UHFFFAOYSA-N 4,4'-dichlorobenzophenone Chemical compound C1=CC(Cl)=CC=C1C(=O)C1=CC=C(Cl)C=C1 OKISUZLXOYGIFP-UHFFFAOYSA-N 0.000 claims description 2
- 239000010692 aromatic oil Substances 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 39
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- RINWGRJHXCCLOV-UHFFFAOYSA-N BPO Chemical compound BPO RINWGRJHXCCLOV-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
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- 239000011343 solid material Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XYLFFOSVQCBSDT-UHFFFAOYSA-N 1,2-dinitrosobenzene Chemical compound O=NC1=CC=CC=C1N=O XYLFFOSVQCBSDT-UHFFFAOYSA-N 0.000 description 1
- JSTCPNFNKICNNO-UHFFFAOYSA-N 4-nitrosophenol Chemical compound OC1=CC=C(N=O)C=C1 JSTCPNFNKICNNO-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 229920003244 diene elastomer Polymers 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Classifications
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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
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
-
- 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
Abstract
The invention belongs to the field of rubber, and relates to a preparation method of self-sealing rubber material, self-sealing rubber material and application thereof, wherein the preparation method comprises the steps of dissolving materials which are easily dissolved in rubber solution, such as synthetic rubber, tackifying resin and liquid plasticizer, in a solvent to prepare a glue solution; crushing and dispersing materials insoluble in rubber solution, such as filler and vulcanizing system components, in a solvent to prepare slurry; uniformly mixing the glue solution and the slurry to prepare a mixed solution; and (5) removing the solvent from the mixed solution to obtain the self-sealing rubber compound. The invention adopts a wet continuous mixing process to prepare the self-sealing sizing material, and optimizes and improves the formula of the self-sealing sizing material; compared with the traditional process for directly producing wet master batch by wet mixing, the method has the advantages that the method can directly produce the self-sealing rubber material which is vulcanized, reduces the post-mixing processing and vulcanization process of the rubber material, perfectly solves the problems of uniform dispersion and mixing of large rubber molecules and a large number of plasticizer small molecules, and has more excellent rubber material performance.
Description
Technical Field
The invention belongs to the field of rubber, and relates to a special sizing material used for a self-sealing tire, in particular to a preparation method of the self-sealing sizing material, the self-sealing sizing material and application thereof; the self-sealing rubber material is processed by adopting a wet continuous mixing process, and is used for self-sealing tire rubber material, in particular to a rubber material layer for delaying air leakage after puncture for self-sealing tires.
Background
With the rapid rise and expansion of the electric automobile market in recent years, new requirements of electric automobiles on assembled tires are also getting more and more attention from automobile and tire companies. An electric automobile needs to be provided with a large number of battery packs in order to achieve high endurance mileage, so that the automobile weight is larger than that of a fuel oil automobile, and meanwhile, the large number of battery packs are arranged at the bottom of the automobile and even occupy the positions of tires of a trunk. Accordingly, in order to meet the demand for weight reduction and the installation position of the battery pack, electric vehicles are further required to have a spare tire-free design, and the spare tire-free design of the vehicle increases the demand for a safety tire. The traditional civil safety tire is a run-flat tire, but the defects of high tire noise, poor comfort level and the like of the run-flat tire in recent years are gradually amplified by electric automobiles, and automobile manufacturers and tire manufacturers have to search for new electric tire alternatives. The self-sealing tire avoids the defects of poor comfort level, large tire noise and the like of the run-flat tire, and the self-sealing special tire for the electric automobile, which is put forward by a tire company, meets the requirements of no spare tire, energy conservation and noise reduction of the electric automobile.
The self-sealing compound has good creep fluidity and is also greatly different from the solid form of the conventional rubber in appearance, which requires the technicians to add a small amount of filler and a large amount of plasticizing material when designing the self-sealing compound formula, wherein the main components of the self-sealing compound formula are high-molecular-weight rubber and low-molecular-weight plasticizing material. Because the self-sealing rubber material contains a large amount of plasticizing materials, the molecular weight difference between the plasticizing components and the macromolecules of the rubber polymer is large, the macromolecular rubber polymer is a massive solid, the mixing equipment is required to provide enough mechanical shearing action to crush the solid rubber blocks to a smaller size during dry mixing, other material components except the rubber are contacted with the crushed rubber macromolecules and dispersed, the small molecular plasticizing components can play a lubricating role during dry mixing, and the shearing stress during the mixing of the rubber material is reduced, so that the particle size of the rubber blocks cannot be further reduced after the rubber blocks are crushed to a certain degree, and the rubber macromolecules are still in an agglomerated state and cannot be contacted with other components except the rubber. Therefore, when an internal mixer, an open mill and a kneader are used for dry mixing, rubber and plasticizer can still gather on a large scale, and macromolecular rubber polymers are difficult to be mixed and dispersed uniformly with micromolecular plasticizing materials, so that the traditional internal mixer, the open mill and the kneader cannot meet the processing requirements of self-sealing sizing materials, high-rotation-speed high-shear mixing equipment with higher rotation speed, more complex equipment structure and stronger shear force can be provided is needed, and the high-rotation-speed high-shear mixing equipment with complex design is needed for crushing and dispersing the macromolecular rubber polymers, so that the high-rotation-speed high-shear mixing equipment has the defects of high development difficulty, high manufacturing cost, long installation period, small equipment processing capacity, poor equipment universality and the like.
The wet mixing is a mixing technology which is emerging in recent years, the mixing mechanism of the wet mixing is very different from that of the traditional dry mixing (including internal mixer, open mill, kneader and extruder mixing), and the invention improves the traditional wet mixing process according to the formula characteristics of self-sealing sizing materials and the characteristics of the wet mixing process, and develops a wet continuous mixing process for the first time, so as to solve the problem of difficult dry mixing of the self-sealing sizing materials.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a preparation method of self-sealing sizing material, the self-sealing sizing material and application thereof, wherein a wet continuous mixing process is adopted to prepare the self-sealing sizing material, and the formula of the self-sealing sizing material is optimized and improved to meet the matching of the self-sealing sizing material and the wet continuous process; the wet continuous mixing process can directly produce the self-sealing rubber material which is vulcanized, and compared with the traditional process for directly producing wet master batch by wet mixing, the wet continuous mixing process reduces the post-mixing processing and vulcanization process of the rubber material. The preparation method can perfectly solve the problems of uniform dispersion and mixing of rubber macromolecules and a large number of plasticizer micromolecules, saves development and investment of high-rotation-speed high-shear equipment in a dry process, has higher material dispersion level than that in a dry mixing process, and has more excellent sizing material performance.
The technical scheme of the invention is as follows:
the invention provides a preparation method of self-sealing rubber material, which adopts a wet continuous mixing process to solve the problem that rubber and a large number of small molecular polymers are difficult to polymerize and disperse in the dry mixing process of a self-sealing formula, so that the rubber material has better material dispersibility. According to the characteristic that the self-sealing rubber can be vulcanized and then coated, the self-sealing rubber can be vulcanized in the wet continuous mixing process.
The wet continuous mixing process adopted in the preparation of the self-sealing sizing material is different from the conventional wet mixing process. In the rubber industry, a part of sizing material mixed by a mixture (namely various materials in a formula) is called a masterbatch or a masterbatch, the masterbatch is mixed for multiple times, the rest of the compounding agent in the formula is continuously added, and the sizing material entering the next working procedure is obtained, and the final rubber is generally obtained through two or more sections of mixing. The sizing material obtained by conventional wet mixing is wet mixing master batch, namely, only a part of master batch composed of compounding agents in the formula is processed, and the wet mixing master batch is also required to be added with the rest compounding agents under one or more sections of dry mixing process, so that the final dry final rubber is prepared.
The wet continuous mixing process is used for preparing wet final rubber, namely the rubber material obtained by the wet process is added with the full-composition mixture in the formula, the inventor prefers the types of the compounding agents in the formula, and the wet mixing process is optimized, so that all the compounding agents can be uniformly mixed in the wet process. The wet continuous mixing process saves the dry mixing process after the traditional wet mixing process.
The invention provides a preparation method of self-sealing sizing material, which comprises the following steps:
(1) Preparing glue solution: dissolving synthetic rubber, tackifying resin and liquid plasticizer in alkane solvent, controlling the dissolving temperature at 40-80 ℃, stirring at 10-200 rpm, and dissolving for 10-100 h to obtain glue solution;
in the step of preparing the glue solution, the lower the dissolution temperature is, the lower the stirring rate is, and the longer the dissolution time is; and vice versa. For example, a dissolution temperature of 40℃and a stirring rate of 40rpm may be selected, and the dissolution time is 100 hours; or the dissolution temperature is 60 ℃, the stirring speed is 100rpm, and the dissolution time is 50 hours; or the dissolution temperature is 80 ℃, the stirring speed is 200rpm, and the dissolution time is 10 hours; etc.
(2) Preparing slurry: crushing the components of a filler and a vulcanizing system, controlling the rotating speed at 1000-2000 rpm, controlling the temperature at 30-80 ℃, controlling the particle size range at 1-100 mu m, adding crushed materials into an alkane solvent, controlling the concentration of the materials at 10-30%, mixing and dispersing by stirring, controlling the rotating speed at 15-150 rpm and the mixing time period at 10-30 min, and preparing the slurry;
(3) Preparing a mixed solution: fully mixing the glue solution and the slurry under the stirring action, wherein the stirring rotation speed is 10-200 rpm, the material temperature is 20-60 ℃, and the mixing time is 30-240 min, so as to prepare a mixed solution;
(4) And (3) preparation of rubber compound: and (3) removing the solvent from the mixed solution, and heating and crosslinking the mixed solution for 10-240 min at 70-180 ℃ to obtain self-sealing rubber compound, namely the self-sealing rubber compound.
By adopting the preparation method provided by the invention, the wet final rubber prepared by the wet continuous mixing process is vulcanized rubber, namely, the wet final rubber completes the mixing processing process and the vulcanization process of the rubber in the wet continuous mixing process. According to the invention, the design of a vulcanization system in a formula is optimized according to the thermal history of the process after adding the compounding agent of the vulcanization system in the wet process, not only are components of the compounding agent uniformly dispersed in the self-sealing sizing material in the wet continuous mixing process, but also the removal of the solvent and the vulcanization of the sizing material are completed by controlling proper processing temperature and time after the components of the compounding agent are uniformly dispersed.
The synthetic rubber, tackifying resin and liquid plasticizer in the step (1) belong to materials which are easily dissolved in rubber solution, and are dissolved in alkane solvent to prepare glue solution; in the step (2), when materials insoluble in rubber solution, such as filler and vulcanizing system components, are crushed and dispersed in alkane solvent to prepare slurry, in order to accelerate the crushing of the filler and other solid material components, the solid materials are crushed on a crusher, the rotating speed of the crusher is controlled at 1000-2000 rpm, the temperature is 30-80 ℃, the particle size range is controlled at 1-100 mu m, and the crushed materials are added into alkane solvent for mixing and dispersing.
Further, in the step (1), the amount of the synthetic rubber is 100phr, and the synthetic rubber is butyl rubber polymerized by isobutene and a small amount of isoprene; butyl rubber has optimal air tightness and water resistance, and can better prevent gas from penetrating through a rubber molecular gap, wherein the butyl rubber comprises brominated butyl rubber, chlorinated butyl rubber and non-halogenated butyl rubber;
according to the types and the sequence of materials added in the wet continuous mixing process, the temperature, the time and other process parameters of the wet continuous mixing process, the non-halogenated butyl rubber is preferably used as a main polymer for the wet continuous mixing because of higher processing stability. The non-halogenated butyl rubber is used in an amount of 100phr (parts by weight based on 100 parts by weight of rubber polymer, other materials being converted to relative weight). The non-halogenated butyl rubber requires a greater rubber molecular weight to provide stronger physico-mechanical properties, i.e., mooney viscosity (ML1+8@125℃) is controlled between 46 and 56; the degree of unsaturation (mol%) is very dependent on the degree of vulcanization of the final compound and is preferably controlled between 1.5 and 2.0%.
Further, the tackifying resin in the step (1) mainly provides viscosity for the self-sealing sizing material, the using amount of the tackifying resin is 10-40 phr, and the tackifying resin comprises C5 and C9 petroleum tackifying resins of petroleum resins, tert-octyl phenol formaldehyde tackifying resins and p-tert-butyl phenol formaldehyde resins of alkyl phenol formaldehyde tackifying resins, and hydrocarbon mixed resins blended by aromatic hydrocarbon and aliphatic hydrocarbon which are commonly used as rubber homogenizing agents in rubber industry; preferably, the tackifying resin at least comprises an alkyl phenolic tackifying resin, and the softening point is controlled to be 90-150 ℃ according to the tackifying effect; the amount is preferably 15 to 30phr. Because the liquid plasticizer generally has a tackifying effect, the amount of tackifying resin can be reduced by increasing the amount of the liquid plasticizer.
Further, in the step (1), the amount of the liquid plasticizer is 70 to 500phr, and the liquid plasticizer comprises liquid rubber and rubber oil; liquid rubber, i.e., rubber polymers that generally have molecular weights below one hundred thousand and that behave as non-solid at ordinary temperature, including liquid polyisobutylene PIB, liquid polybutadiene LBR, liquid polyisoprene LIR; the rubber oil comprises environment-friendly aromatic hydrocarbon oil TDAE, heavy naphthenic oil HNAP and solvent shallow oil pumping MES.
The liquid plasticizer mainly acts to soften the rubber material, provide plasticity for the rubber material, enable the rubber material to creep and deform, and provide enough deformation when used in a tire, wherein the deformation is used for wrapping foreign matters penetrating through the tire and blocking gaps left after the penetration.
The molecular weight of the liquid rubber is controlled to be Mn < 10000g/mol; in view of compatibility with non-halogenated butyl rubber, polyisobutylene PIB is preferred, and further preferably, PIB weight average molecular weight Mn is controlled to 1000 to 4000g/mol. The rubber oil has small molecular weight and good plasticizing effect, but the excessive rubber oil affects the performance and the ejection problem of the rubber material, and the dosage is controlled to be 0-50 phr. Preferably, the liquid plasticizer comprises at least one component of PIB, the amount of PIB being controlled between 50 and 400 phr.
Further, in the step (2), the amount of the filler is 5-50 phr, and the filler is one or more of carbon black, white carbon black, light calcium carbonate and kaolin; the selection of the filler is carried out according to the processability of the wet continuous mixing process in addition to the performance required by the conventional rubber reinforcement, and carbon black and white carbon black are selected as the filler, wherein the specific surface area of the white carbon black is controlled between 160 and 220m 3 Per gram (BET test method), the specific surface area of the carbon black is controlled between 35 and 85m 3 /g (BET test method). The filler amount is preferably 15 to 40phr. The amount of the filler is in a certain proportion to the amount of the liquid plasticizer, and the amount of the filler rises with the increase of the amount of the liquid plasticizer.
Further, the components of the vulcanization system in step (2) comprise a vulcanizing agent and a vulcanization activator, and the vulcanization system of the present invention comprises at least one vulcanizing agent and at least one vulcanization activator, wherein the vulcanizing agent is used in an amount of 1 to 5phr and the vulcanization activator is used in an amount of 0 to 20phr, preferably 3 to 20phr.
The butyl rubber has low double bond content in molecular chain and lower reaction activity than common diene rubber. The research and test of the invention show that the vulcanizing speed of the common sulfur and accelerator vulcanizing system and the vulcanizing resin system is very low, but the vulcanizing reaction speed of the vulcanizing resin and the non-halogenated butyl rubber is slower when the peroxide is used alone to vulcanize the butyl rubber at high temperature to degrade butyl rubber macromolecules preferably. The vulcanization system used in the non-halogenated butyl rubber of the present invention is a quinone oxime vulcanization system comprising a vulcanizing agent and a vulcanization activator. The vulcanizing agent comprises p-benzoquinone dioxime, p-dibenzoyl benzoquinone dioxime and p-dinitrosobenzene. The vulcanization activator includes zinc oxide, lead oxide, organic peroxide, 2-mercaptobenzothiazole (accelerator M), and dibenzothiazyl Disulfide (DM).
The organic peroxide comprises alkyl peroxide (R-C-O-O-C-R '), acyl peroxide (R-C (O) -O-O- (O) C-R') lipid peroxide (R-C (O) O-O-R '), lipid peroxycarbonate (R-O-C (O) O-O-R'), and the like. The different peroxides have large difference in reactivity, and acyl peroxides with better activity are preferred, such as dibenzoyl peroxide BPO, bis (4-methylbenzamide) MBPO and bis (2, 4-dichlorobenzoyl) DCBP. As previously mentioned, peroxide alone as a vulcanization activator degrades butyl rubber when reacted with non-halogenated butyl rubber, so to achieve non-halogenated butyl rubber cross-linking, peroxide is used with the aforementioned vulcanizing agent and the ratio of the two is controlled, and excess peroxide still degrades non-halogenated butyl rubber. Peroxide is used in an amount of 0 to 10phr (pure).
Further, the mixed solution obtained in the step (4) needs to be conveyed to an extruder for solvent removal and heating crosslinking, the process temperature is between 10min and 4h, the temperature is between 70 and 180 ℃, the recovery and the cyclic utilization are carried out after the solvent is removed, the process temperature and the time are set to be the results of coordinating the solvent removal and the vulcanization of the sizing material, and the preferable temperature is between 100 and 160 ℃ and the time is between 10min and 2h.
The invention also provides a self-sealing sizing material which is prepared by adopting the preparation method.
The invention also protects the application of the self-sealing sizing material in the self-sealing tire.
Furthermore, the self-sealing rubber material is used for preparing a rubber material layer for delaying air leakage after puncture for the self-sealing tire.
The invention has the beneficial effects that:
according to the preparation method of the self-sealing rubber material, when wet continuous mixing is carried out, components such as plasticizer and the like which are dissolved in a solvent and rubber macromolecules are dissolved in a solution to complete dispersion work, namely a glue solution preparation process, components which are insoluble in the rubber solvent, such as filler and a vulcanization system component are uniformly dispersed in the solvent under the stirring action after special crushing treatment, namely a glue solution preparation process, the glue solution and the glue solution are mixed to form a mixed solution, all the components are uniformly distributed under the stirring action, and the solvent is removed from the mixed solution at a certain temperature to obtain the rubber compound. Compared with the traditional wet mixing process for directly producing wet master batch, the wet continuous mixing process maintains the continuity of the processing of the rubber material, can directly complete the vulcanization of the rubber material, and reduces the post-mixing processing and vulcanization process of the rubber material; and the problems of uniform dispersion and mixing of rubber macromolecules and a large number of plasticizer micromolecules can be perfectly solved, the development and investment of high-rotation-speed high-shear equipment in a dry process are saved, the material dispersion level is higher than that in a dry mixing process, and the sizing material performance is more excellent.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in connection with various embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
For a further understanding of the present invention, the present invention will be further described with reference to examples.
The invention provides a preparation method of self-sealing sizing material, which comprises the following steps:
(1) Preparing glue solution: dissolving synthetic rubber, tackifying resin and liquid plasticizer in alkane solvent, controlling the dissolving temperature at 40-80 ℃, stirring at 10-200 rpm, and dissolving for 10-100 h to obtain glue solution;
(2) Preparing slurry: crushing the components of a filler and a vulcanizing system, controlling the rotating speed at 1000-2000 rpm, controlling the temperature at 30-80 ℃, controlling the particle size range at 1-100 mu m, adding crushed materials into an alkane solvent, controlling the concentration of the materials at 10-30%, mixing and dispersing by stirring, controlling the rotating speed at 15-150 rpm and the mixing time period at 10-30 min, and preparing the slurry;
(3) Preparing a mixed solution: fully mixing the glue solution and the slurry under the stirring action, wherein the stirring rotation speed is 10-200 rpm, the material temperature is 20-60 ℃, and the mixing time is 30-240 min, so as to prepare a mixed solution;
(4) And (3) preparation of rubber compound: and (3) removing the solvent from the mixed solution, heating and crosslinking for 10-240 min at 70-180 ℃ to obtain the self-sealing rubber compound.
The parameters of temperature, stirring speed, rotating speed, time and the like in the preparation step can be any value in the range value; in addition, in the glue solution preparation step of the step (1), the lower the temperature is, the lower the stirring speed is, and the longer the dissolution time is; further, if the amount of the liquid plasticizer to be added is large, the amount of the tackifying resin to be added is small, and the amount of the filler to be added is about 10 times the amount of the liquid plasticizer to be added.
The formula composition of the self-sealing sizing material prepared by the preparation method comprises the following components:
100phr of synthetic rubber;
wherein the synthetic rubber is butyl rubber, which can be any one of brominated butyl rubber, chlorinated butyl rubber and non-halogenated butyl rubber, preferably non-halogenated butyl rubber;
10 to 40phr of tackifying resin;
wherein the amount of the tackifying resin is any value within the range of 10 to 40phr, for example, 10phr, 15phr, 20phr, 30phr, 40phr, etc.; the tackifying resins include petroleum resins such as C5 and C9 petroleum tackifying resins, alkyl phenol formaldehyde tackifying resins such as tert-octyl phenol formaldehyde tackifying resins, p-tert-butyl phenol formaldehyde resins, and hydrocarbon mixed resins blended with aromatic and aliphatic hydrocarbons, preferably alkyl phenol formaldehyde tackifying resins;
70 to 500phr of liquid plasticizer;
wherein the amount of the liquid plasticizer is any value in the range of 70 to 500phr, and may be, for example, 70phr, 80phr, 90phr, 100phr, 150phr, 200phr, 350phr, 400phr, 500phr, etc.; the liquid plasticizer comprises liquid rubber and rubber oil, the rubber oil comprises environment-friendly aromatic hydrocarbon oil TDAE, heavy naphthenic oil HNAP and solvent shallow oil pumping MES, and the liquid rubber comprises liquid polyisobutene PIB, liquid polybutadiene LBR and liquid polyisoprene LIR, preferably PIB;
5 to 50phr filler;
wherein the amount of the filler is any value within the range of 5 to 50phr, for example, 5phr, 15phr, 20phr, 25phr, 30phr, 40phr, 50phr and the like; the filler is one or more of carbon black, white carbon black, light calcium carbonate and kaolin, preferably carbon black and white carbon black;
4 to 25phr of a cure system component;
wherein the cure system components comprise 1 to 5phr of a curing agent and 3 to 20phr of a curing active agent, the curing agent being any value within the range of 1 to 5phr, such as 1phr, 2phr, 3phr, 4phr, 5phr, etc., the curing active agent being any value within the range of 3 to 20phr, such as 3phr, 5phr, 7phr, 9phr, 12phr, 16phr, 20phr, etc.; the vulcanizing system comprises a vulcanizing agent and a vulcanizing active agent, wherein the vulcanizing agent comprises p-benzoquinone dioxime, p-dibenzoyl benzoquinone dioxime and p-dinitrosobenzene, and the vulcanizing active agent comprises zinc oxide, lead oxide, organic peroxide, 2-mercaptobenzothiazole (accelerator M) and dibenzothiazyl Disulfide (DM); the vulcanization activator is preferably an acyl peroxide.
Example 1
Weighing 100phr of non-halogenated butyl rubber X_ButylRB100, 20phr of tert-octyl phenol formaldehyde tackifying resin, 280phr of liquid polyisobutylene PIBGlisopal 1300, 30phr of carbon black N326, 15phr of dibenzoyl peroxide BPO, zinc oxide and p-benzoquinone dioxime according to a formula of the self-sealing rubber compound;
the preparation method of the self-sealing sizing material comprises the following steps:
(1) Preparing glue solution: dissolving non-halogenated butyl rubber X_ButylRB100, tert-octyl phenol formaldehyde tackifying resin and liquid polyisobutene PIBGlisopal 1300 in an alkane solvent, controlling the dissolving temperature at 60 ℃, and dissolving for 60 hours at the stirring speed of 100rpm to prepare a glue solution;
(2) Preparing slurry: crushing carbon black N326, dibenzoyl peroxide BPO, zinc oxide and p-benzoquinone dioxime, controlling the rotation speed at 1500rpm, controlling the temperature at 50 ℃, controlling the particle size range at 50 mu m, adding crushed materials into an alkane solvent, controlling the concentration of the materials at 20%, mixing and dispersing through stirring, controlling the rotation speed at 80rpm and the mixing time at 20min, and preparing slurry;
(3) Preparing a mixed solution: fully mixing the glue solution and the slurry under the stirring action, wherein the stirring rotation speed is 100rpm, the material temperature is 40 ℃, and the mixing time is 130min, so as to prepare a mixed solution;
(4) And (3) preparation of rubber compound: and (3) removing the solvent from the mixed solution, and carrying out heating crosslinking for 120min at 130 ℃ to obtain the self-sealing rubber compound, namely the self-sealing rubber compound prepared in the embodiment.
Example 2
Weighing 100phr of non-halogenated Butyl rubber Butyl268, 15phr of p-tert-butylphenol formaldehyde resin, 400phr of liquid polyisobutylene PIBGLissopal2300, 40phr of white carbon black ZEOSIL1165MP and 6phr of p-dinitrosobenzene according to a formula of the self-sealing sizing material;
the preparation method of the self-sealing sizing material comprises the following steps:
(1) Preparing glue solution: dissolving non-halogenated Butyl rubber Butyl268, p-tert-butylphenol formaldehyde resin and liquid polyisobutene PIBGLissopal2300 in an alkane solvent, controlling the dissolving temperature at 50 ℃, and dissolving for 80 hours at a stirring speed of 80rpm to prepare a glue solution;
(2) Preparing slurry: crushing white carbon black ZEOSIL1165MP and dinitroso benzene, controlling the rotation speed at 1300rpm, the temperature at 40 ℃ and the particle size range at 30 mu m, adding crushed materials into an alkane solvent, controlling the concentration of the materials at 20%, mixing and dispersing by stirring, controlling the rotation speed at 50rpm and the mixing time at 25min, and preparing slurry;
(3) Preparing a mixed solution: fully mixing the glue solution and the slurry under the stirring action, wherein the stirring rotation speed is 60rpm, the material temperature is 30 ℃, and the mixing time is 180min, so as to prepare a mixed solution;
(4) And (3) preparation of rubber compound: and (3) removing the solvent from the mixed solution, and heating and crosslinking the mixed solution for 200min at the temperature of 100 ℃ to obtain the self-sealing rubber material.
Example 3
Weighing 100phr of non-halogenated butyl rubber X_ButylRB100, 30phr of tert-octyl phenol formaldehyde tackifying resin, 200phr of liquid polyisobutylene PIBGlisopal 1300, 20phr of carbon black N330, 15phr of p-benzoquinone dioxime, zinc oxide and dibenzoyl peroxide BPO according to a formula of the self-sealing rubber compound;
the preparation method of the self-sealing sizing material comprises the following steps:
(1) Preparing glue solution: dissolving non-halogenated butyl rubber X_ButylRB100, tert-octyl phenol formaldehyde tackifying resin and liquid polyisobutene PIBGlisopal 1300 in an alkane solvent at 70 ℃, stirring at 150rpm for 30 hours to obtain a glue solution;
(2) Preparing slurry: crushing carbon black N330, p-benzoquinone dioxime, zinc oxide and dibenzoyl peroxide BPO, controlling the rotation speed at 1800rpm, controlling the temperature at 70 ℃, controlling the particle size range at 80 mu m, adding crushed materials into an alkane solvent, controlling the concentration of the materials at 20%, mixing and dispersing through stirring, controlling the rotation speed at 120rpm and the mixing time at 15min, and preparing slurry;
(3) Preparing a mixed solution: fully mixing the glue solution and the slurry under the stirring action, wherein the stirring rotation speed is 150rpm, the material temperature is 50 ℃, and the mixing time is 80min, so as to prepare a mixed solution;
(4) And (3) preparation of rubber compound: and (3) removing the solvent from the mixed solution, and heating and crosslinking the mixed solution for 60 minutes at 160 ℃ to obtain the self-sealing rubber material.
Example 4
Weighing 100phr of non-halogenated butyl rubber X_ButylRB100, 40phr of tert-octyl phenol formaldehyde tackifying resin, 70phr of liquid polyisobutylene PIBGLissopal1300, 10phr of carbon black N550 and 4phr of p-dinitrosobenzene according to a formula of the self-sealing rubber material;
the preparation method of the self-sealing sizing material comprises the following steps:
(1) Preparing glue solution: dissolving non-halogenated butyl rubber X_ButylRB100, tert-octyl phenol formaldehyde tackifying resin and liquid polyisobutene PIBGlisopal 1300 in an alkane solvent at 80 ℃ and stirring speed of 200rpm for 10 hours to prepare a glue solution;
(2) Preparing slurry: crushing carbon black N550 and p-dinitroso benzene, controlling the rotating speed at 2000rpm, controlling the temperature at 80 ℃, controlling the particle size range at 100 mu m, adding crushed materials into an alkane solvent, controlling the concentration of the materials at 30%, mixing and dispersing by stirring, controlling the rotating speed at 150rpm and the mixing time period at 10min, and preparing slurry;
(3) Preparing a mixed solution: fully mixing the glue solution and the slurry under the stirring action, wherein the stirring rotation speed is 200rpm, the material temperature is 60 ℃, and the mixing time is 30min, so as to prepare a mixed solution;
(4) And (3) preparation of rubber compound: and (3) removing the solvent from the mixed solution, and heating and crosslinking the mixed solution for 10min at 180 ℃ to obtain the self-sealing rubber material.
Example 5
Weighing 100phr of non-halogenated Butyl rubber Butyl268, 10phr of tert-octyl phenol formaldehyde tackifying resin, 450phr of liquid polyisobutylene PIBGLissaopal 2300, 50phr of carbon black N330, 20phr of p-benzoquinone dioxime, zinc oxide and dibenzoyl peroxide BPO according to a formula of the self-sealing sizing material;
the preparation method of the self-sealing sizing material comprises the following steps:
(1) Preparing glue solution: dissolving non-halogenated Butyl rubber Butyl268, tert-octyl phenol formaldehyde tackifying resin and liquid polyisobutene PIBGlisopal 2300 in an alkane solvent, controlling the dissolving temperature at 40 ℃, and dissolving at a stirring speed of 10rpm for 100 hours to prepare a glue solution;
(2) Preparing slurry: crushing carbon black N330, p-benzoquinone dioxime, zinc oxide and dibenzoyl peroxide BPO, controlling the rotation speed at 1000rpm, the temperature at 30 ℃ and the particle size range at 1 mu m, adding crushed materials into an alkane solvent, controlling the concentration of the materials at 10%, mixing and dispersing through stirring, and controlling the rotation speed at 15rpm and the mixing time at 30min to prepare slurry;
(3) Preparing a mixed solution: fully mixing the glue solution and the slurry under the stirring action, wherein the stirring rotation speed is 10rpm, the material temperature is 20 ℃, and the mixing time is 240min, so as to prepare a mixed solution;
(4) And (3) preparation of rubber compound: and (3) removing the solvent from the mixed solution, and heating and crosslinking the mixed solution for 240min at the temperature of 70 ℃ to obtain the self-sealing rubber material.
Of the above formulation materials, the non-halogenated butyl rubber X_ButylRB100 is a commercially available product of ARLANXEO company of Arlunaceae; non-halogenated Butyl rubber Butyl268 is a commercially available product from ExxonMobil corporation; liquid polyisobutylene PIB Glissopal1300 and Glissopal2300 are commercially available from BASF corporation; the white carbon black ZEOSIL1165MP is a commercial product of Solvier company. Other raw materials not illustrated are commercially available products known to those skilled in the art.
The foregoing description is only a preferred embodiment of the present invention and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or that equivalents may be substituted for part of the technical features thereof. Any modification, equivalent replacement, variation, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the self-sealing sizing material is characterized by comprising the following steps of:
(1) Preparing glue solution: dissolving synthetic rubber, tackifying resin and liquid plasticizer in alkane solvent, controlling the dissolving temperature at 40-80 ℃, stirring at 10-200 rpm, and dissolving for 10-100 h to obtain glue solution;
(2) Preparing slurry: crushing the components of a filler and a vulcanizing system, controlling the rotating speed at 1000-2000 rpm, controlling the temperature at 30-80 ℃, controlling the particle size range at 1-100 mu m, adding crushed materials into an alkane solvent, controlling the concentration of the materials at 10-30%, mixing and dispersing by stirring, controlling the rotating speed at 15-150 rpm and the mixing time period at 10-30 min, and preparing the slurry;
(3) Preparing a mixed solution: fully mixing the glue solution and the slurry under the stirring action, wherein the stirring rotation speed is 10-200 rpm, the material temperature is 20-60 ℃, and the mixing time is 30-240 min, so as to prepare a mixed solution;
(4) And (3) preparation of rubber compound: and (3) removing the solvent from the mixed solution, heating and crosslinking for 10-240 min at 70-180 ℃ to obtain the self-sealing rubber compound.
2. The method of preparing a self-sealing compound according to claim 1, wherein in step (1), the amount of synthetic rubber is 100phr, said synthetic rubber being butyl rubber polymerized from isobutylene and a small amount of isoprene;
preferably, the butyl rubber includes brominated butyl rubber, chlorinated butyl rubber, and non-halogenated butyl rubber;
preferably, the butyl rubber is non-halogenated butyl rubber, the Mooney viscosity (ML1+8@125 ℃) of the non-halogenated butyl rubber is controlled between 46 and 56, and the unsaturation (mol%) is controlled between 1.5 and 2.0%.
3. The method of preparing a self-sealing compound according to claim 1, wherein in step (1), the amount of tackifying resin is 10 to 40phr, the tackifying resin comprises C5, C9 petroleum tackifying resins of petroleum resins, tert-octylphenol formaldehyde tackifying resins of alkylphenol tackifying resins, p-tert-butylphenol formaldehyde resins, and hydrocarbon mixed resins blended with aromatic hydrocarbons and aliphatic hydrocarbons;
preferably, the tackifying resin is alkyl phenolic tackifying resin, and the softening point of the tackifying resin is controlled to be 90-150 ℃;
preferably, the tackifying resin is used in an amount of 15 to 30phr.
4. The method of preparing a self-sealing compound according to claim 1, wherein in step (1), the amount of liquid plasticizer is 70 to 500phr, and the liquid plasticizer comprises liquid rubber and rubber oil;
preferably, the rubber oil comprises environment-friendly aromatic oil TDAE, heavy naphthenic oil HNAP and solvent shallow oil pumping MES;
preferably, the liquid rubber comprises liquid polyisobutylene PIB, liquid polybutadiene LBR, liquid polyisoprene LIR;
preferably, the molecular weight of the liquid rubber is controlled to Mn < 10000g/mol;
preferably, the liquid rubber is PIB, and the weight average molecular weight Mn of the PIB is controlled to be 1000-4000 g/mol.
5. The method for preparing self-sealing rubber material according to claim 1, wherein in the step (2), the amount of filler is 5-50 phr, and the filler is one or more of carbon black, white carbon black, light calcium carbonate and kaolin;
preferably, the filler comprises carbon black and white carbon black, and the specific surface area of the white carbon black is controlled to be 160-220 m 3 Per gram, the specific surface area of the carbon black is controlled between 35 and 85m 3 /g。
6. The method of preparing a self-sealing compound according to claim 1, wherein the components of the vulcanization system in step (2) comprise a vulcanizing agent in an amount of 1 to 5phr and a vulcanization active agent in an amount of 0 to 20phr;
preferably, the vulcanizing agent comprises p-benzoquinone dioxime, p-dibenzoyl benzoquinone dioxime, p-dinitrosobenzene;
preferably, the vulcanization activator comprises zinc oxide, lead oxide, organic peroxide, 2-mercaptobenzothiazole, dibenzothiazyl disulfide, preferably organic peroxide;
the organic peroxide is one or more of alkyl peroxide, acyl peroxide, peroxide ester and peroxide carbonate ester; preferably an acyl peroxide;
the acyl peroxide comprises dibenzoyl peroxide BPO, bis (4-methylbenzamide) MBPO and bis (2, 4-dichlorobenzoyl) DCBP.
7. The method of preparing a self-sealing compound according to claim 1, wherein the temperature in step (4) is 100-160 ℃ for 10-120 min.
8. A self-sealing compound, characterized in that it is produced by the preparation method according to any one of claims 1 to 7.
9. Use of the self-sealing compound of claim 8 in a self-sealing tire.
10. Use according to claim 9, characterized in that said self-sealing compound is used as a compound layer for delaying the leakage of air after puncture for self-sealing tyres.
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