CN115948004B - Self-healing brominated butyl rubber/natural rubber blending modification system and preparation method thereof - Google Patents
Self-healing brominated butyl rubber/natural rubber blending modification system and preparation method thereof Download PDFInfo
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- 229920005557 bromobutyl Polymers 0.000 title claims abstract description 40
- 244000043261 Hevea brasiliensis Species 0.000 title claims abstract description 39
- 229920003052 natural elastomer Polymers 0.000 title claims abstract description 39
- 229920001194 natural rubber Polymers 0.000 title claims abstract description 39
- 238000002156 mixing Methods 0.000 title claims abstract description 31
- 238000012986 modification Methods 0.000 title claims abstract description 17
- 230000004048 modification Effects 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 34
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 11
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 claims abstract description 10
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 claims abstract description 10
- DDRPCXLAQZKBJP-UHFFFAOYSA-N furfurylamine Chemical compound NCC1=CC=CO1 DDRPCXLAQZKBJP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920003192 poly(bis maleimide) Polymers 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 15
- 238000004090 dissolution Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 15
- 229920001971 elastomer Polymers 0.000 description 14
- 230000035876 healing Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 229920005549 butyl rubber Polymers 0.000 description 7
- -1 nitrogen organic compound Chemical class 0.000 description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical class N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 4
- 239000003517 fume Substances 0.000 description 4
- 239000002135 nanosheet Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000013003 healing agent Substances 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000008113 selfheal Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- 229920002367 Polyisobutene Polymers 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 125000001246 bromo group Chemical group Br* 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920005555 halobutyl Polymers 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a self-healing brominated butyl rubber/natural rubber blending modification system and a preparation method thereof. The system comprises brominated butyl rubber, natural rubber, maleic anhydride, furfuryl amine, bismaleimide and benzimidazole. Mixing natural rubber and maleic anhydride, and then heating, refluxing and dissolving the mixture by taking excessive tetrahydrofuran as a solvent; adding furfuryl amine and then adding bismaleimide; dissolving brominated butyl rubber in tetrahydrofuran, and adding benzimidazole; mixing the two mixtures, drying, and putting into a flat vulcanizing machine for molding to obtain the self-healing brominated butyl rubber/natural rubber blending modification system. The obtained brominated butyl rubber has excellent mechanical strength and self-healing effect after being vulcanized. The brominated butyl rubber has the advantages of high self-healing efficiency, good mechanical property, simple and convenient processing, low cost and the like, and is suitable for the application of tires, sealing elements and the like.
Description
Technical Field
The invention relates to a novel self-healing brominated butyl rubber/natural rubber blending modification system and a preparation method thereof, belonging to the technical field of rubber modification.
Background
The butyl rubber is formed by polymerizing and copolymerizing more than 97% of polyisobutene and less than 3% of polyisoprene through cations, and the highly saturated alkane-like structure endows the butyl rubber with extremely strong solvent resistance, aging resistance and other performances, and symmetrical side methyl enables the butyl rubber to keep excellent air tightness while not crystallizing, so that the butyl rubber is widely applied to the fields of inner tubes of tires, sealing rings and the like.
The self-healing method of the polymer material comprises two types of external-assistance healing and intrinsic healing. External healing refers to the repair of damaged areas by supplementing the material with substances or energy, such as by adding healing agents (unreacted reactants and catalysts) to the material, either externally or internally, after the material is damaged, the reactants begin to react after being wounded, which means essentially requires the consumption of substances, and the self-healing properties of the material are lost after multiple damages. The latter is the use of reversible covalent bonds and supramolecular interactions (ionic bonds, hydrogen bonds, coordination bonds, pi-pi interactions, van der waals forces, etc.), the reassembly, bonding, and the process involves only energy transfer, only under supplied energy (heat, light, etc.) even spontaneously at the site of damage. The first way is relatively easy to be put into practice, and has been applied to road materials such as asphalt, but the healing agent (i.e. unreacted reactant and catalyst) is gradually consumed after being damaged many times, and the material will lose self-healing properties accordingly, which greatly limits its development prospect. Reversible covalent intrinsic healing is generally thermally reversible, requiring temperature regulation, i.e., heat supply. The supermolecule type intrinsic healing does not need to consume a healing agent and a matrix material, and does not need external energy. This self-healing approach is growing with the advent of supramolecular chemistry and systematic research and is the main form and direction of development of self-healing material research. However, the existing intrinsic healing materials have the problems that the existing intrinsic healing materials are difficult to overcome, such as insufficient mechanical properties for use, insufficient self-healing properties and the like.
The patent CN202111133764 discloses a production process capable of automatically repairing a butyl rubber inner tube, wherein a carbon/nitrogen organic compound is added in a final refining process of the production process of the butyl rubber inner tube, and the carbon/nitrogen organic compound and a bromine group interact to enable a system to have ionic interaction, so that the sheared brominated butyl rubber can self-heal, a completely cut sample can keep the original characteristic after the self-healing process is applied, the self-repairing capability of the butyl rubber inner tube is improved, and the repairing speed is accelerated.
The invention discloses a high-strength self-healing rubber material and a preparation method thereof, wherein a polyethylene polymer grafted modified boron nitride nano sheet with a pyridine structure in a side chain is obtained by carrying out free radical polymerization on a boron nitride nano sheet and a pyridine vinyl monomer, and the polyethylene polymer grafted modified boron nitride nano sheet can form dynamic ionic crosslinking bonds when the polyethylene polymer grafted modified boron nitride nano sheet is uniformly dispersed in a halogenated butyl rubber matrix by a mechanical blending method, so that the finally obtained rubber material has high tensile strength and high self-healing performance, and the preparation method has simple process and is easy to realize large scale.
Patent CN202210743399 discloses a conductive self-healing rubber support and a crack repairing method thereof, wherein the rubber support body comprises a rubber support and a rigid support which are connected with each other, and the rubber support is made of conductive self-healing rubber material; the electrode is connected with an external power supply and is used for changing the structure of the rubber support piece under the condition of electrifying so as to enable cracks in the rubber support body to self-heal; the method solves the problem that the normal use of the support in the service cycle of the building structure and the bridge structure and the durability of the support can not be guaranteed to always meet the original design requirement in the prior art.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: provides the self-healing brominated butyl rubber with high healing efficiency and high mechanical strength.
In order to solve the problems, the invention provides a self-healing brominated butyl rubber/natural rubber blending modification system which is characterized by comprising, by mass, 100 parts of brominated butyl rubber (BIIR), 5-20 parts of Natural Rubber (NR), 1-4 parts of Maleic Anhydride (MA), 0.5-2.0 parts of furfuryl amine (FFA), 1-4 parts of Bismaleimide (BM) and 10 parts of benzimidazole.
Preferably, the brominated butyl rubber has a Mooney viscosity of 32+ -4 at 125 ℃ and a mass content of bromine of 2.0+ -0.2%.
The invention also provides a preparation method of the self-healing brominated butyl rubber/natural rubber blending modification system, which comprises the following steps:
step 1): mixing natural rubber and maleic anhydride in a Hark torque rheometer, cutting into pieces, placing into excessive acetone for magnetic stirring, filtering, and placing into a vacuum oven for drying to obtain maleic anhydride grafted natural rubber (NR-MA); heating, refluxing and dissolving maleic anhydride grafted natural rubber by taking excessive Tetrahydrofuran (THF) as a solvent; adding furfuryl amine after dissolution, and reacting; cooling after the reaction is finished, adding bismaleimide, and stirring for reaction;
step 2): cutting brominated butyl rubber into pieces, putting the pieces into tetrahydrofuran, stirring and dissolving the pieces, and adding benzimidazole after dissolving;
step 3): and (3) adding the mixture obtained in the step (1) into the mixture obtained in the step (2), stirring and mixing, drying, and putting into a flat vulcanizing machine for molding after drying to obtain the self-healing brominated butyl rubber/natural rubber blending modification system.
Preferably, in the step 1), the temperature of the haak torque rheometer is 150 ℃ and the rotating speed is 50rpm; the temperature of the vacuum oven is 40 ℃; the temperature of dissolution by heating reflux was 80 ℃. Preferably, in the step 2), the temperature of stirring and dissolving is 60 ℃.
Preferably, in the step 3), the drying temperature is not more than 40 ℃; the technological parameters of the flat vulcanizing machine are as follows: the temperature is 80-130 ℃, the pressure is 10MPa, and the time is 30min.
The brominated butyl rubber disclosed by the invention realizes high-degree self-healing after being treated for a period of time at a certain temperature. Compared with the prior art, the brominated butyl rubber has the advantages of high healing efficiency and high mechanical strength, improves the solution mixing preparation process, has the characteristics of simple and quick preparation process, good mixing quality and contribution to industrialized production, and has wide market application prospect. The self-healing brominated butyl rubber prepared by the invention can be well matched with the existing commercial rubber preparation and processing technology, and is suitable for the application fields of tires, sealing elements and the like.
Detailed Description
In order to make the present invention more comprehensible, preferred embodiments accompanied with the present invention are described in detail below.
The various materials used in examples 1-3 were all commercially available and commonly used materials. The self-healing efficiency test method of the self-healing brominated butyl rubber/natural rubber blending modification system prepared in examples 1-3 was the percentage of the tensile strength of the healed rubber and the tensile strength of the original rubber.
The mechanical strength of the self-healing rubber is tested according to GB/T528-2009, the stretching rate is 500mm/min, and the measuring instrument for 20mm gauge length of the extensometer is SUN500 type universal electronic testing machine, GALDABINI company of Italy.
Example 1
(1) 5g of natural rubber and 1g of maleic anhydride are mixed in a Hark torque rheometer in proportion for about 5min at a temperature of 150 ℃ and a rotational speed of 50rpm. And taking out, cutting into pieces, putting into excessive acetone, magnetically stirring for more than 1h, filtering, putting into a vacuum oven, drying for more than 24h at 40 ℃ to obtain the maleic anhydride grafted natural rubber (NR-MA). The maleic anhydride grafted natural rubber was placed in a flask and dissolved in excess Tetrahydrofuran (THF) as solvent under reflux at 80 ℃ for 72h. After dissolution 0.5g of furfuryl amine was added in proportion and the reaction stirred for 5h at 80 ℃. After cooling, the mixture was left overnight, 1g of bismaleimide was added in proportion, and the mixture was stirred at 80℃for reaction for 1 hour.
(2) 100g of brominated butyl rubber is cut into pieces and put into tetrahydrofuran of a flask to be stirred and dissolved at 60 ℃ for 72 hours, and 10g of benzimidazole is added proportionally after the dissolution.
(3) Adding the mixture in (1) into (2), stirring and mixing for 24 hours, volatilizing the solvent in a fume hood and a vacuum oven, and drying at a temperature of not more than 40 ℃. Drying and molding in a flat vulcanizing machine at 80 deg.c and 10MPa for 30min to obtain self-healing brominated butyl rubber/natural rubber blending modified system.
Example 2
(1) 20g of natural rubber and 4g of maleic anhydride are mixed in a Hark torque rheometer in proportion for about 5min at a temperature of 150℃and a rotational speed of 50rpm. And taking out, cutting into pieces, putting into excessive acetone, magnetically stirring for more than 1h, filtering, putting into a vacuum oven, drying for more than 24h at 40 ℃ to obtain the maleic anhydride grafted natural rubber (NR-MA). The maleic anhydride grafted natural rubber was placed in a flask and dissolved in excess Tetrahydrofuran (THF) as solvent under reflux at 80 ℃ for 72h. After dissolution 2g of furfuryl amine was added in proportion and the reaction stirred for 5h at 80 ℃. After cooling, the mixture was left overnight, 4g of bismaleimide was added in proportion, and the mixture was stirred at 80℃for 1 hour.
(2) 100g of brominated butyl rubber is cut into pieces and put into tetrahydrofuran of a flask to be stirred and dissolved at 60 ℃ for 72 hours, and 10g of benzimidazole is added proportionally after the dissolution.
(3) Adding the mixture in (1) into (2), stirring and mixing for 24 hours, volatilizing the solvent in a fume hood and a vacuum oven, and drying at a temperature of not more than 40 ℃. Drying and molding in a flat vulcanizing machine at 160 deg.c and 10MPa for 10min to obtain self-healing brominated butyl rubber/natural rubber blending modified system.
Example 3
(1) 10g of natural rubber and 2.5g of maleic anhydride are mixed in a Hark torque rheometer in proportion for about 5min at a temperature of 150℃and a rotational speed of 50rpm. And taking out, cutting into pieces, putting into excessive acetone, magnetically stirring for more than 1h, filtering, putting into a vacuum oven, drying for more than 24h at 40 ℃ to obtain the maleic anhydride grafted natural rubber (NR-MA). The maleic anhydride grafted natural rubber was placed in a flask and dissolved in excess Tetrahydrofuran (THF) as solvent under reflux at 80 ℃ for 72h. After dissolution 1.25g of furfuryl amine was added in proportion and the reaction stirred for 5h at 80 ℃. After cooling, the mixture was left overnight, and then 2.5g of bismaleimide was added in proportion and reacted at 80℃with stirring for 1 hour.
(2) 100g of brominated butyl rubber is cut into pieces and put into tetrahydrofuran of a flask to be stirred and dissolved at 60 ℃ for 72 hours, and 10g of benzimidazole is added proportionally after the dissolution.
(3) Adding the mixture in (1) into (2), stirring and mixing for 24 hours, volatilizing the solvent in a fume hood and a vacuum oven, and drying at a temperature of not more than 40 ℃. Drying and molding in a flat vulcanizing machine at 130 ℃ under 10MPa for 20min to obtain the self-healing brominated butyl rubber/natural rubber blending modified system.
Comparative example
(1) 100g of brominated butyl rubber is cut into pieces and put into tetrahydrofuran of a flask to be stirred and dissolved at 60 ℃ for 72 hours, and 10g of benzimidazole is added proportionally after the dissolution. (2) The mixture of (1) is dried by volatilizing the solvent in a fume hood and vacuum oven at a temperature of no more than 40 ℃. Drying and molding in a flat vulcanizing machine at 100 ℃ under 10MPa for 10min to obtain the brominated butyl rubber with the self-healing effect.
The samples of examples 1-3 and comparative examples were subjected to self-healing efficiency and mechanical strength tests, and the test results are shown in Table 1.
TABLE 1
| Material Properties | Example 1 | Example 2 | Example 3 | Comparative example |
| Self-healing efficiency (%) | 83％ | 75％ | 88％ | 92％ |
| Tensile Strength (MPa) | 2.45 | 2.83 | 2.95 | 2.12 |
Claims (5)
1. The self-healing brominated butyl rubber/natural rubber blending modification system is characterized by comprising, by mass, 100 parts of brominated butyl rubber, 5-20 parts of natural rubber, 1-4 parts of maleic anhydride, 0.5-2.0 parts of furfuryl amine, 1-4 parts of bismaleimide and 10 parts of benzimidazole;
the preparation method of the self-healing brominated butyl rubber/natural rubber blending modification system comprises the following steps:
step 1): mixing natural rubber and maleic anhydride in a Hark torque rheometer, cutting into pieces, placing into excessive acetone for magnetic stirring, filtering, placing into a vacuum oven for drying to obtain maleic anhydride grafted natural rubber; heating, refluxing and dissolving maleic anhydride grafted natural rubber by taking excessive tetrahydrofuran as a solvent; adding furfuryl amine after dissolution, and reacting; cooling after the reaction is finished, adding bismaleimide, and stirring for reaction;
step 2): cutting brominated butyl rubber into pieces, putting the pieces into tetrahydrofuran, stirring and dissolving the pieces, and adding benzimidazole after dissolving;
step 3): and (3) adding the mixture obtained in the step (1) into the mixture obtained in the step (2), stirring and mixing, drying, and putting into a flat vulcanizing machine for molding after drying to obtain the self-healing brominated butyl rubber/natural rubber blending modification system.
2. The self-healing brominated butyl rubber/natural rubber blending modification system of claim 1, wherein the brominated butyl rubber has a mooney viscosity of 32±4 at 125 ℃ and a mass content of bromine of 2.0±0.2%.
3. The self-healing brominated butyl rubber/natural rubber blending modification system of claim 1, wherein in step 1), the temperature of the haak torque rheometer is 150 ℃ and the rotation speed is 50rpm; the temperature of the vacuum oven is 40 ℃; the temperature of dissolution by heating reflux was 80 ℃.
4. The self-healing brominated butyl rubber/natural rubber blending modification system of claim 1, wherein in step 2), the temperature of stirring dissolution is 60 ℃.
5. The self-healing brominated butyl rubber/natural rubber blending modification system of claim 1, wherein in step 3), the drying temperature is not more than 40 ℃; the technological parameters of the flat vulcanizing machine are as follows: the temperature is 80-130 ℃, the pressure is 10MPa, and the time is 30min.
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