CN109988417B - Patch type vacuum tire puncture-proof sealing layer material and preparation method thereof - Google Patents
Patch type vacuum tire puncture-proof sealing layer material and preparation method thereof Download PDFInfo
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- CN109988417B CN109988417B CN201910267599.8A CN201910267599A CN109988417B CN 109988417 B CN109988417 B CN 109988417B CN 201910267599 A CN201910267599 A CN 201910267599A CN 109988417 B CN109988417 B CN 109988417B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/69—Polymers of conjugated dienes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/14—Polyurethanes having carbon-to-carbon unsaturated bonds
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sealing Material Composition (AREA)
- Tires In General (AREA)
Abstract
The invention discloses a puncture-proof sealing layer material for a patch type vacuum tire, which comprises the following components in parts by weight: 30-40 parts of polybutadiene polyurethane, 15-20 parts of liquid butyl rubber, 11-34 parts of liquid polyisobutylene, 8-12 parts of a tackifier and 13-17 parts of carbon black. The sealing layer is endowed with excellent air tightness by utilizing the characteristics of excellent gas barrier properties of polybutadiene, polyisobutylene and butyl rubber; high molecular weight polybutadiene polyurethane is compounded with liquid polyisobutylene and liquid butyl rubber, and the mixture is vulcanized by a kneading process to endow the material with excellent viscoelasticity. The sealing layer can automatically block the puncture along with the large deformation of the inserted and pulled foreign matters. The glass transition temperature of the material is between-70 ℃ and-60 ℃, and embrittlement and flowing phenomena do not occur within the range of-40 ℃ to 100 ℃. Excellent holding viscosity and mechanical strength can prevent the film from being peeled off and falling off during high-speed operation. The material can be adhered to the inner side of the tire without auxiliary heating and spraying equipment, and has high-efficiency constructability and excellent functionality, and great economic advantages.
Description
Technical Field
The invention relates to the technical field of rubber composite materials, in particular to a patch type sealing layer material for preventing puncture of a vacuum tire and a preparation method thereof.
Background
When the traditional tire is punctured by a sharp foreign matter, the inner tube is easy to puncture to cause tire burst, thereby causing serious traffic accidents. In order to solve the problem of instant pressure loss of the tire caused by puncture of the inner tube, the sealing layer is adopted in the industry to replace the inner tube. The basic design principle of the sealing layer is that rubber with excellent air tightness, a tackifier, carbon black and other components are blended to prepare the composite material with excellent viscoelasticity, adhesiveness and mechanical property.
U.S. Pat. No. 3,3935893 discloses in 1976 a carbon black reinforced sealant material based on high and low molecular weight butyl rubber in combination with controlled viscoelasticity and adhesion. The formula system creates a basic idea for designing the puncture-proof sealing layer and promotes the development of butyl rubber and halogenated butyl rubber. The application of the United states patent [ US3952787] discloses a method for preparing a sealing layer material based on matching and blending ethylene propylene diene monomer, styrene butadiene rubber, natural rubber and carbon black, the formula of the method is simple, but the adhesion and the performance of automatically repairing pores after puncture by sharp foreign matters are reduced. In order to improve the adhesion and mechanical properties, U.S. Pat. No. 5,430,6895 discloses formulations of chlorinated butyl rubber emulsions, brominated butyl rubber emulsions, polyisobutylene emulsions, polyisoprene emulsions with antioxidants, titanium dioxide, carbon black or clay. The above typical sealing layer materials need auxiliary equipment to heat and spray the heated sealing layer materials on the inner surface of the tire, and the addition of complex equipment and procedures is not beneficial to improving the production efficiency and reducing the comprehensive cost. Chinese patent application No. CN201510967616 discloses a sealant composition for puncture resistant tires, a way to design a composite sheet of an adhesive sealant layer and an air tight inner sealant layer that circumvents the problems of secondary spray equipment. But the proposal still does not fundamentally take into account the excellent adhesiveness, air tightness, mechanical property, self-repairing function and simple and easy-to-operate constructability.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a patch type vacuum tire puncture-proof sealing layer material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a patch type vacuum tire puncture-proof sealing layer material comprises the following components in parts by weight:
30-40 parts of polybutadiene polyurethane;
15-20 parts of liquid butyl rubber;
11-34 parts of liquid polyisobutylene;
8-12 parts of a tackifier;
13-17 parts of carbon black.
Preferably, the polybutadiene polyurethane is synthesized by hydroxyl-terminated polybutadiene (HTPB) and diisocyanate monomer, the HTPB has an average molecular weight of 2500-5000g/mol and a hydroxyl value of 0.48-0.52mmol/g, and the diisocyanate is one of Toluene Diisocyanate (TDI), diphenylmethane-4-4' -diisocyanate (MDI), 1, 6-Hexamethylene Diisocyanate (HDI), isophorone diisocyanate (IPDI) and dicyclohexylmethane diisocyanate (HMDI).
Preferably, the liquid butyl rubber has an unsaturation of 2.5 to 4.0 mol%, an average molecular weight of 30000 and 60000 g/mol.
Preferably, the liquid polyisobutene has an average molecular weight of 400-2500 g/mol.
Preferably, the tackifier is a mixture of terpene resin, super tackifying resin, rosin glyceride and pentaerythritol ester in a mass ratio of 3:1 to phenolic resin, and the phenolic resin is one of rosin modified phenolic resin, tert-butyl phenolic tackifying resin, octyl phenolic tackifying resin and brominated methyl alkyl phenolic resin.
Preferably, the fineness of the carbon black is not less than 200 meshes.
Meanwhile, the invention also provides a preparation method of the patch type vacuum tire puncture-proof sealing layer material, which comprises the following steps:
(1) and (2) putting a quantitative HTPB into a vertical polyurethane reaction kettle to remove water for 1-2 hours, then putting a quantitative diisocyanate monomer according to a set R value (the amount ratio of isocyanate groups to active hydrogen substances), adding a catalyst to react for 1-3 hours after the reaction is carried out for 1 hour, and adding a quantitative parachlorophenol end-capping reagent to continue the reaction for 0.5-1 hour to obtain the polybutadiene polyurethane.
(2) And (2) putting the polybutadiene polyurethane obtained in the step (1), quantitative liquid butyl rubber, liquid polyisobutylene, a tackifier and carbon black into a vacuum kneading machine for mixing, dispersing and vulcanizing, then extruding by a screw rod and forcibly feeding into an adhesive tape machine, and obtaining the surface mount type sealing layer material after calendering, double-sided sticking of release paper, slitting and rolling.
Preferably, in the step (1), the temperature of the reaction kettle in the water removal stage is 100-120 ℃, the stirring speed is 50-70 r/min, and the vacuum degree is-0.1 to-0.08 MPa. In the reaction stage, the temperature of the reaction kettle is 70-80 ℃, the stirring speed is 50-70 r/min, and nitrogen with the purity of more than or equal to 99.0% is introduced.
Preferably, in the step (1), the R value is 1.2-1.6. A large number of experiments prove that the polybutadiene polyurethane obtained by controlling the R value within the range can be used for preparing a sealing layer material with excellent mechanical strength, adhesion and air tightness.
Preferably, in the step (1), the catalyst is one or a mixture of two of dibutyltin dilaurate, tetramethylbutanediamine, triethylenediamine and stannous octoate, and the adding amount is 0.001-0.003% of the amount of the active hydrogen substance.
Preferably, in the step (2), the temperature of the vacuum kneader is 70-100 ℃, the vacuum degree is-0.095-0.08 MPa, the rotating speed is 25-35 r/min, and the kneading and stirring time is 20-40 min.
Preferably, the glass transition temperature of the material of the puncture-proof sealing layer of the patch type vacuum tire is-70-60 ℃, and the test is carried out by referring to the method specified in ASTM D7028-2007 standard.
Preferably, the patch type vacuum tire puncture-proof sealing layer material is kept at-40 ℃ for 24 hours without embrittlement phenomenon, and the test is carried out by referring to the method specified in GB/T16978-1997 standard.
Preferably, the puncture-proof sealing layer material of the patch type vacuum tire is kept at 100 ℃ for 24 hours without a flow phenomenon, and the test is carried out by referring to a method specified in GB/T16978-1997 standard.
Preferably, the puncture-proof sealing layer material of the patch type vacuum tire can be directly adhered to the inner side of the vacuum tire without auxiliary heating equipment or spraying equipment.
Compared with the prior art, the invention has the beneficial effects that:
the sealing layer is endowed with excellent air tightness by utilizing the characteristics of excellent gas barrier properties of polybutadiene, polyisobutylene and butyl rubber; the high molecular weight polybutadiene polyurethane is compounded with liquid polyisobutylene and liquid butyl rubber, a viscoelastic rubber composite material is obtained through blending and vulcanization, and the mechanical strength is improved by adopting carbon black, so that the sealing layer is greatly deformed when being punctured by a sharp foreign matter, and the puncturing risk is greatly reduced; the tackifier promotes the compatibility and the dispersibility between each rubber component and carbon black in the formula, obviously improves the adhesion of the material, and can not only block a puncture when a sharp foreign body is pulled, but also prevent the tire from being torn and falling off when the tire runs at high speed. The viscoelastic rubber composite material can be processed into a patch type sealing layer by universal rubber processing equipment. The sealing layer can be adhered to the inner side of the tire without auxiliary heating and spraying equipment in a tire factory, and the size can be cut according to actual needs after the tire is used, so that the functionality is kept within the range of-40 to 100 ℃, and the simple and efficient constructability of the patch type sealing layer material has great economic advantages.
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Detailed description of the preferred embodiment
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The raw materials used in the experiments in the embodiments and the comparative examples of the present invention are as follows, but the present invention is not limited to the following raw materials, and the effects of the patch type vacuum tire puncture-proof sealing layer material in the present application are further specifically described only by taking the following raw materials as specific examples:
polybutadiene type polyurethane: synthesized by type I HTPB of the astronomical chemical industry and MDI-80/20 (Tantawa), and the R value is 1.5.
Liquid butyl rubber: kalene 1300, available from Royal Elastomers.
Liquid polybutadiene: PB2400, purchased from Dalbergia korea.
Tackifier: super tackifying resin KORESIN (BASF), brominated methyl alkyl phenol formaldehyde SP1055 (Shenectady).
Carbon black: n330, available from cabot.
The test method of each performance index in the examples and comparative examples of the present invention is specifically shown in table 1:
table 1 test method for each performance index
| Test items | Unit of | Reference standard |
| Peel strength | kN/m | GB/T 2792-1998 |
| Initial tack | kN/m | GB/T 4852-2002 |
| Viscosity retention property | h | GB/T 4851-1998 |
| Tensile strength | MPa | GB/T 528-2009 |
| Elongation at break | ％ | GB/T 528-2009 |
Airtightness: the method comprises the steps of completely puncturing 10 JIS N100 round nails into a tire longitudinal groove with initial tire pressure of 250kPa, pulling out the round nails within 2 seconds, standing the tire for 1 minute, observing the air leakage condition of each nail hole, counting the number of the nail holes without air leakage as an air tightness value, and using the number as a parameter for evaluating the anti-puncturing capacity of the sealing layer.
The invention is provided with examples 1-12 and comparative examples 1-6, and the components and the weight parts of the components of the specific examples 1-12 and comparative examples 1-6 are shown in the following table 2:
TABLE 2 Components and contents of examples 1 to 12 and comparative examples 1 to 6
The preparation method of the puncture-proof sealing layer material for the patch type vacuum tire in the embodiments 1 to 12 includes the following steps:
(1) putting the quantitative HTPB into a vertical polyurethane reaction kettle to remove water for 1 hour; and adding a certain amount of MDI (diphenylmethane diisocyanate) according to the set R value of 1.5, reacting for 1 hour, adding a catalyst dibutyltin dilaurate with the amount of active hydrogen substances of 0.001 percent for reaction for 2 hours, adding a certain amount of p-chlorophenol end-capping agent, and continuing to react for 0.5 hour to obtain the polybutadiene polyurethane.
(2) And (2) putting the polybutadiene polyurethane obtained in the step (1), quantitative liquid butyl rubber, liquid polyisobutylene, a tackifier and carbon black into a vacuum kneading machine for mixing, dispersing and vulcanizing, extruding and forcibly feeding into an adhesive tape machine by a screw after kneading and stirring, and obtaining the surface mount type sealing layer material after calendering, double-sided release paper pasting, slitting and rolling.
In the step (1), the temperature of the reaction kettle in the water removal stage is 110 ℃, the stirring speed is 60 r/min, and the vacuum degree is-0.09 MPa; in the reaction stage, the temperature of the reaction kettle is 78 ℃, the stirring speed is 60 r/min, and nitrogen with the purity of 99.9 percent is introduced.
In the step (2), the temperature of the vacuum kneader is 80 ℃, the vacuum degree is-0.09 MPa, the rotating speed is 30 r/min, and the kneading and stirring time is 30 min.
The performance of the polypropylene composite materials of examples 1 to 12 and comparative examples 1 to 6 was tested according to the method shown in table 1, and the specific evaluation results are shown in table 3:
TABLE 3 evaluation results of the performance of the sealing layer materials in examples 1 to 12 and comparative examples 1 to 6
Strictly speaking, the air tightness value of 10 has practical value, because the safety can be ensured only when the automobile is pricked in the high-speed running process and no instant pressure loss or even tire burst occurs. As can be seen from the comprehensive performance evaluation in Table 3, the polybutadiene polyurethane and liquid butyl rubber are vulcanized and crosslinked to endow viscoelasticity, the liquid polyisobutylene and the tackifier endow adhesion to the material, the carbon black plays a role in improving the mechanical strength, and the viscoelasticity, the adhesion and the mechanical property influence the final air tightness, so that the qualified air tightness can be ensured only by controlling each component within a special range.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The patch type vacuum tire puncture-proof sealing layer material is characterized by comprising the following components in parts by weight: 30-40 parts of polybutadiene polyurethane, 15-20 parts of liquid butyl rubber, 11-34 parts of liquid polyisobutylene, 8-12 parts of a tackifier and 13-17 parts of carbon black; the preparation method of the patch type vacuum tire puncture-proof sealing layer material comprises two steps, (1) the synthesis of polybutadiene polyurethane, namely, putting quantitative hydroxyl-terminated polybutadiene HTPB into a vertical polyurethane reaction kettle for dewatering, then putting quantitative diisocyanate monomer according to a set molar ratio of isocyanate group to active hydrogen, namely, R value, adding a catalyst for reacting for a certain time, and then adding quantitative parachlorophenol for end sealing, (2) the preparation of the patch type vacuum tire puncture-proof sealing layer material, namely, putting polybutadiene polyurethane, quantitative liquid butyl rubber, liquid polyisobutylene, a tackifier and carbon black into a vacuum kneading machine for mixing, dispersing and vulcanizing, then extruding by a screw rod and forcibly feeding into an adhesive tape machine for calendaring, double-sided sticking of release paper, slitting and rolling; the glass transition temperature of the puncture-proof sealing layer material of the patch type vacuum tire is-70-60 ℃ tested according to the method specified by ASTM D7028-2007 standard, the glass transition temperature is kept for 24 hours at-40 ℃ without embrittlement phenomenon according to the method specified by GB/T16978-.
2. The patch type vacuum tire puncture-proof sealing layer material according to claim 1, wherein the HTPB has an average molecular weight of 2500-5000g/mol and a hydroxyl value of 0.48-0.52mmol/g, and the diisocyanate is one of Toluene Diisocyanate (TDI), diphenylmethane-4-4' -diisocyanate (MDI), 1, 6-Hexamethylene Diisocyanate (HDI), isophorone diisocyanate (IPDI), and dicyclohexylmethane diisocyanate (HMDI).
3. The patch type vacuum tire puncture-proof sealing layer material as claimed in claim 1, wherein the liquid butyl rubber has an unsaturation degree of 2.5-4.0 mol%, and an average molecular weight of 30000 and 60000 g/mol.
4. The patch-type vacuum tire puncture-proof sealing layer material as claimed in claim 1, wherein the liquid polyisobutylene has an average molecular weight of 400-.
5. The patch type vacuum tire puncture-proof sealing layer material as claimed in claim 1, wherein the tackifier is a mixture of terpene resin, super tackifying resin, rosin glyceride and pentaerythritol ester in a mass ratio of 3:1 with phenolic resin, and the phenolic resin is one of rosin modified phenolic resin, tert butyl phenolic tackifying resin, octyl phenolic tackifying resin and methyl alkyl brominated phenolic resin.
6. The patch type vacuum tire puncture-proof sealing layer material as claimed in claim 1, wherein the fineness of the carbon black is not less than 200 meshes.
7. The material for the puncture-proof sealing layer of the patch-type vacuum tire as claimed in claim 1, wherein in the step (1), the temperature of the reaction kettle in the water removal stage is 100-; and in the reaction stage, the temperature of the reaction kettle is 70-80 ℃, the stirring speed is 50-70 r/min, nitrogen with the purity of more than or equal to 99.0% is introduced, the reaction is carried out for 1 hour before the catalyst is added, and the reaction is carried out for 1-3 hours after the catalyst is added.
8. The patch type vacuum tire puncture-proof sealing layer material according to claim 1, wherein in the step (1), the R value is 1.2-1.6.
9. The patch type vacuum tire puncture-proof sealing layer material according to claim 1, wherein in the step (1), the catalyst is one or a mixture of two of dibutyltin dilaurate, tetramethylbutanediamine, triethylenediamine and stannous octoate, and the input amount is 0.001-0.003% of the amount of the active hydrogen substance.
10. The material for the puncture-proof sealing layer of the patch-type vacuum tire as claimed in claim 1, wherein in the step (2), the temperature of the vacuum kneader is 70-100 ℃, the vacuum degree is-0.095-0.08 MPa, the rotation speed is 25-35 r/min, and the kneading and stirring time is 20-40 min.
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| CN110527060A (en) * | 2019-08-16 | 2019-12-03 | 青岛喜乐途新材料科技有限公司 | A kind of polyurethaneurea compositions and its polyurethane urea coating preparation method |
| CN110527280A (en) * | 2019-09-27 | 2019-12-03 | 南京瑞兴科技有限公司 | A kind of roofing extruded sheet envelope painting material |
| CN113930171A (en) * | 2021-11-24 | 2022-01-14 | 广东盈通新材料有限公司 | Hot melt adhesive film for transfer printing silica gel and preparation method thereof |
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| EP0063280A2 (en) * | 1981-04-17 | 1982-10-27 | The Firestone Tire & Rubber Company | A curable storage-stable and solventless single component sealant composition for pneumatic tires |
| CN1092783A (en) * | 1994-01-11 | 1994-09-28 | 青岛化工学院 | The manufacture method of polyurethane elastomer glue stock |
| CN103496302A (en) * | 2013-10-11 | 2014-01-08 | 杭州顺源轮胎制造有限公司 | Preparation method of safe anti-puncturing tyre |
| CN105419024A (en) * | 2015-12-22 | 2016-03-23 | 三角轮胎股份有限公司 | Sealing layer composition for anti-pricking tire |
| WO2018093962A1 (en) * | 2016-11-17 | 2018-05-24 | Bridgestone Americas Tire Operations, Llc | Pneumatic tire having a sealant layer and air barrier layer |
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2019
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| US4352704A (en) * | 1979-03-16 | 1982-10-05 | Dunlop Limited | Method of making porous tread |
| EP0063280A2 (en) * | 1981-04-17 | 1982-10-27 | The Firestone Tire & Rubber Company | A curable storage-stable and solventless single component sealant composition for pneumatic tires |
| CN1092783A (en) * | 1994-01-11 | 1994-09-28 | 青岛化工学院 | The manufacture method of polyurethane elastomer glue stock |
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