CN105218882A - Improve rubber combination and the application of vulcanized rubber stability - Google Patents
Improve rubber combination and the application of vulcanized rubber stability Download PDFInfo
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- CN105218882A CN105218882A CN201510770721.5A CN201510770721A CN105218882A CN 105218882 A CN105218882 A CN 105218882A CN 201510770721 A CN201510770721 A CN 201510770721A CN 105218882 A CN105218882 A CN 105218882A
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Abstract
Both economical and the rubber combination of vulcanized rubber stability, the rubber components containing 100 weight parts, the carbon black of 5-100 weight part, the anti-recovery agent of 1-20 weight part can be improved.Wherein, anti-recovery agent contains two hydration hexa-methylene 1,6-bisthiosulfate disodium salt and fatty acid zinc salts.Described rubber combination ensures sizing material mechanical property stable in over cure situation, improves the anti-reversion behaviour of rubber, improves the dynamic property of sizing material simultaneously.
Description
Technical field
The present invention relates to field of rubber technology, specifically a kind of rubber combination improving vulcanized rubber stability, and use the tire tread of this rubber combination.
Background technology
Natural rubber (NR) is as a kind of conventional rubber, there is good elasticity and mechanical property, but the thermostability of polysulfide crosslink bond is poor in its cross-linked rubber, in sulfidation, along with heated time extends, the initial polysulfide crosslink bond part formed can rupture, and causes the cross-linking density of sizing material to reduce, the physicals of sizing material declines, and the use properties of rubber item reduces.Along with the fast development of rubber industry, researchist studies how to eliminate or reduce the revert phenomenon of rubber in sulfidation and use procedure always, can keep again mechanical property and the use properties of rubber item simultaneously, extends the work-ing life of goods.
Consider from reversion mechanism, the measure improving NR anti-reversion behaviour is mainly by adding sulfur carrier compound or offset-type vulcanization system to make up the loss of cross-link bond, such as add two hydration hexa-methylenes 1,6-bisthiosulfate disodium salt (DuralinkHTS), its chemical formula is as follows:
About Monsanto Chemicals develops DuralinkHTS at first in the 1980s, is used for improving the stability of polysulfide crosslink bond, improves the anti-reversion behaviour of sizing material.Containing sulphur atom and carbon atom in DuralinkHTS molecular structure, during rubber vulcanization, HTS inserts a hexa-methylene disulfide group group in the macromolecular polysulfide crosslink bond of sizing material, embed soft in cross-link bond structure and there is the alkyl of thermostability, the generation of this composite crosslinking key can make the cross-linked rubber aging resistance of resistance to anaerobism improve, improve the thermostability of cross-link bond in sizing material, improve the antireversion of sizing material, extend the work-ing life of rubber item.But in Vulcanization Process of Rubber, HTS because of one end of its S-S key be the form of inorganic inferior sulfate radical, so its activity is low when vulcanization reaction, and the vulcanization crosslinking between rubber macromolecule reacts slow, HTS is caused to play the efficiency of anti-recovery in actual applications not high, play effect comparatively slow, thus the reversion performance of tire can be affected.
Summary of the invention
The object of the invention is to overcome the limitation of above-mentioned prior art existence and deficiency, there is provided a kind of both economical and the rubber combination of raising vulcanized rubber stability of HTS can be given full play to, ensure sizing material mechanical property stable in over cure situation, improve the anti-reversion behaviour of rubber, improve the dynamic property of sizing material simultaneously.
The object of the present invention is to provide a kind of rubber combination improving vulcanized rubber stability, comprise following component:
The rubber components of 100 weight parts, the carbon black of 5-100 weight part, the anti-recovery agent of 1-20 weight part.Wherein, anti-recovery agent contains two hydration hexa-methylene 1,6-bisthiosulfate disodium salt (HTS) and fatty acid zinc salts.
According to rubber combination of the present invention, rubber components can be natural rubber (NR), polyisobutylene rubber (IR), polybutadiene rubber (BR), Styrene Butadiene Copolymer rubber (SBR), ethylene-propylene-diene terpolymer (EPDM), these rubber can be used alone, or use their any mixture.
The kind of carbon black is not particularly limited, and example comprises: HAF, [SAF, SAF or their combination.
With the rubber components of 100 weight parts for benchmark, the consumption of carbon black between 5-100 weight part, preferably between 10-80 weight part.
With the rubber components of 100 weight parts for benchmark, the consumption of anti-recovery agent is 1-20 weight part, preferred 2-10 weight part.
Anti-recovery agent in rubber combination of the present invention contains two hydration hexa-methylene 1,6-bisthiosulfate disodium salt (HTS) and fatty acid zinc salts.The general formula of described fatty acid zinc salt is
r is selected from C
5-20the alkyl of straight or branched, C
5-20the thiazolinyl of straight or branched, C
7 ~ 12aryl radical.One or more preferably in n-caprylic acid zinc, isocaprylic acid zinc, n-capric acid zinc, zinc laurate, TETRADECONIC ACID zinc, zinc palmitate, zinc oleate, Zinic stearas, Zinc dibenzoate, toluylic acid zinc, phenylpropionic acid zinc of fatty acid zinc.In anti-recovery agent, the mass percentage of HTS is 40 ~ 95%, is preferably 60 ~ 90%; The mass percentage of fatty acid zinc is 5 ~ 60%, is preferably 10 ~ 40%.
The zinc oxide of 1.0 ~ 6.0 weight parts, the stearic acid of 1.0 ~ 4.0 weight parts, the anti-aging agent of 1.5 ~ 5.0 weight parts, the sulphur of 2.0 ~ 6.0 weight parts, the promotor of 0.5 ~ 2.0 weight part can also be contained in rubber combination of the present invention.
Promotor can select sulfenamide type accelerators, as CZ, NOBS, NS, DZ, OTOS etc.
Except above-mentioned fundamental component, rubber combination of the present invention can also contain multiple tire typical additives, such as vulcanizing agent, polytype oil, process oil, wax, antiaging agent and softening agent etc.
Said components is mixed to generate the rubber combination that can be used for thereafter sulfuration by the ordinary method by the art.
Present invention also offers a kind of tire tread, this tire tread is prepared by above-mentioned rubber combination.
The anti-recovery agent adopted in the present invention contains HTS and fatty acid zinc salt, fatty acid zinc salt can promote the fracture of S-S key in HTS molecular structure in vulcanization reaction process, improve the reactive behavior of HTS, HTS can be made more effectively to participate in the vulcanization reaction process of rubber, improve the cross-linking density of rubber combination, the C-S key of Heat of Formation good stability simultaneously, improves the thermostability of cross-link bond.HTS and fatty acid zinc salt with the use of, make the mechanical property that its rubber combination can keep good, there is good anti-reversion behaviour simultaneously.
Accompanying drawing explanation
Fig. 1 becomes with sulphur the reversion performance that instrument measures comparative example 1,2 and embodiment 1 ~ 3 rubber, can find out that the rubber compounding torque not adding any anti-recovery agent through 30min obviously declines, after adding HTS, the torque of rubber compounding slightly improves, and adopts its torque downtrending of rubber compounding of the present invention significantly better than the rubber compounding only adding HTS.
Embodiment
In order to make those skilled in the art understand technical scheme of the present invention better, below in conjunction with specific embodiment, the present invention is described in further detail.It is pointed out that all similar replacements and change apparent to those skilled in the art, they are all deemed to be included in the present invention.
In embodiment 1 ~ 3 in anti-recovery agent HTS and fatty acid zinc component and content as shown in table 1.
The composition of table 1, embodiment 1 ~ 3 anti-recovery agent
Table 2. rubber compounding (each material content unit: weight part)
| Starting material | Comparative example 1 | Comparative example 2 | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Natural rubber | 100.0 | 100.00 | 100.0 | 100.0 | 100.0 |
| Carbon black N330 | 45.0 | 45.00 | 45.0 | 45.0 | 45.0 |
| Zinc oxide | 4.5 | 4.5 | 4.5 | 4.5 | 4.5 |
| Stearic acid | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 |
| Anti-aging agent 6PPD | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Sulphur | 2.0 | 2.0 | 2.0 | 2.0 | 2.0 |
| Accelerator NS | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 |
| HTS | - | 2.0 | - | - | - |
| Anti-recovery agent | - | - | 3.0 | 2.74 | 2.49 |
Component in embodiment rubber combination and source as follows:
Natural rubber, SMR20, Malaysian product;
Carbon black N330, Degussa;
Zinc oxide, Dalian zinc oxide factory;
Stearic acid, safe Ke's brown;
Anti-aging agent 6PPD, commercially available;
Sulphur, commercially available;
Accelerator NS, commercially available;
HTS, Flexsys;
Zinic stearas, Chemical Reagent Co., Ltd., Sinopharm Group;
Zinc laurate, Chemical Reagent Co., Ltd., Sinopharm Group;
Zinc dibenzoate, Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment plant and instrument:
1.6LBR1600 Banbury mixer, U.S. Farrel Products;
The mill of XK-160 type, Qingdao Xin Chengyiming machine works product;
XLB-D600 × 600 type vulcanizing press, Zhejiang Huzhou Hong Qiao machine works product;
3365 type puller systems, Instron Corporation of U.S. product;
Without rotor rheometer, U.S. Ai Erfa Products.
The standard method that embodiment uses:
Rubber test sizing material batching, mixing and vulcanizing equipment and schedule of operation GB/T6038-2006;
The preparation of rubber physical test method sample and adjustment universal program GB/T2914-2006;
Rubber measures vulcanization characteristics GB/T16584-1996 with without rotor vulkameter;
The mensuration GB/T528-2009 of vulcanized rubber or thermoplastic elastomer tensile stress-strain performance.
Vulcanized rubber or thermoplastic elastomer penetration hardness test method (Shore durometer method) GBT531.1-2008
The preparation of sample
Be filled with natural rubber compound (100 parts of NR of carbon black, 45 parts of N330 carbon blacks, 2 parts of stearic acid, 4.5 parts of zinc oxide, 2 parts of 6PPD, 1 part of accelerator NS, 2 parts of sulphur) middle interpolation anti-recovery agent, with 1.6 liters of Banbury Banbury mixeies, by rubber, carbon black, anti-recovery agent and other compound except sulphur and vulcanization accelerator 5 minutes, to obtain master batch, then use opening rubber mixing machine in master batch, mix vulcanization accelerator and sulphur, thus acquisition rubber combination, the sulfuration 10 minutes at the temperature of 160 DEG C of often kind of rubber combination obtained like this, thus acquisition vulcanized rubber.
Processing characteristics
The mooney viscosity method of testing specified according to GB/T1232.1-2000, the mooney viscosity of working sample at 100 DEG C.The mooney viscosity ML (1+4) 100 DEG C of comparative example 1 and 3 is set to 100, and processing characteristics is with the exponential representation in equation below, and index is less, and Mooney viscosity value is less, and processing characteristics is better.
Mooney viscosity index=(Mooney point of each composition)/(Mooney point of comparative example 1 and 3) × 100
Reversion resistance
The MDR2000 type of alpha company of the U.S. is used to become the curability of instrument test glue stuff compounding without rotor sulphur, the following formulae discovery of reversion percentage according to GB/T16584-1996
To revert rate=(torque capacity-final torque)/(torque capacity-minimum torque) × 100
Anti-reversion behaviour represents with the rate of reverting, and rate of reverting is less, and anti-recovery effect is better.
Table 3 reverts rate
| To revert rate | |
| Comparative example 1 | 20％ |
| Comparative example 2 | 10％ |
| Embodiment 1 | 8％ |
| Embodiment 3 | 8％ |
| Embodiment 3 | 7％ |
As can be seen from the rate of reverting of table 1, after adding HTS in comparative example 2, the rate of reverting decreases, and the rate of reverting adopting rubber compounding provided by the invention to obtain is lower than comparative example 2, the reactive behavior that improve HTS after adding fatty acid zinc is described, more abundant with the vulcanization reaction of rubber, thus there is better anti-reversion behaviour.
Table 4 mechanical property (160 DEG C × 20min)
| Comparative example 1 | Comparative example 2 | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| 10% stretches surely | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
| 100% stretches surely | 3.8 | 3.5 | 3.6 | 3.6 | 3.8 |
| 300% stretches surely | 16.8 | 16.0 | 15.7 | 15.9 | 16.8 |
| Tensile strength | 28.0 | 28.2 | 27.5 | 27.8 | 27.0 |
| Elongation at break | 456 | 469 | 469 | 477 | 443 |
| Hardness | 68 | 68 | 68 | 68 | 68 |
Sulfur vulcanization mechanical property (175 DEG C × 60min) crossed by table 5
| Comparative example 1 | Comparative example 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| 10% stretches surely | 0.6 | 0.7 | 0.7 | 0.7 | 0.7 |
| 100% stretches surely | 2.8 | 2.9 | 3.2 | 3.1 | 3.4 |
| 300% stretches surely | 12.6 | 13.7 | 14.2 | 14.5 | 15.5 |
| Tensile strength | 23.8 | 24.7 | 24.5 | 25.2 | 24.6 |
| Elongation at break | 441 | 422 | 426 | 437 | 412 |
| Hardness | 62 | 65 | 65 | 65 | 66 |
Comparison sheet 5 and table 4 can be found out, under over cure condition, composition mechanical property conservation rate of the present invention is better than HTS.
By rubber combination of the present invention, the rubber combination for tire tread that antireversion can be higher can be obtained and use the pneumatic tyre of this rubber combination.
Claims (10)
1. improve a rubber combination for vulcanized rubber stability, it is characterized in that, comprising: the rubber components of 100 weight parts, the carbon black of 5-100 weight part, the anti-recovery agent of 1-20 weight part;
Wherein, described anti-recovery agent contains two hydration hexa-methylene 1,6-bisthiosulfate disodium salt and fatty acid zinc salts.
2. rubber combination as claimed in claim 1, it is characterized in that, described rubber components be selected from natural rubber, polyisobutylene rubber, polybutadiene rubber, Styrene Butadiene Copolymer rubber, ethylene-propylene-diene terpolymer one or more.
3. rubber combination as claimed in claim 1, is characterized in that, the preferred 10-80 weight part of consumption of described carbon black.
4. rubber combination as claimed in claim 1, is characterized in that, the preferred 2-10 weight part of consumption of described anti-recovery agent.
5. rubber combination as claimed in claim 1, it is characterized in that, in described anti-recovery agent, the mass percentage of two hydration hexa-methylene 1,6-bisthiosulfate disodium salts is 40 ~ 95%, and the mass percentage of fatty acid zinc is 560%.
6. rubber combination as claimed in claim 1, it is characterized in that, in described anti-recovery agent, the mass percentage of two hydration hexa-methylene 1,6-bisthiosulfate disodium salts is preferably 60 ~ 90%, and the mass percentage of fatty acid zinc is preferably 10 ~ 40%.
7. rubber combination as claimed in claim 1, it is characterized in that, the general formula of described fatty acid zinc salt is
r is selected from C
5-20the alkyl of straight or branched, C
5-20the thiazolinyl of straight or branched, C
7 ~ 12aryl radical.
8. rubber combination as claimed in claim 7, it is characterized in that, described fatty acid zinc salt be selected from n-caprylic acid zinc, isocaprylic acid zinc, n-capric acid zinc, zinc laurate, TETRADECONIC ACID zinc, zinc palmitate, zinc oleate, Zinic stearas, Zinc dibenzoate, toluylic acid zinc, phenylpropionic acid zinc one or more.
9. rubber combination as claimed in claim 1, it is characterized in that, also comprise the zinc oxide of 1.0 ~ 6.0 weight parts, the stearic acid of 1.0 ~ 4.0 weight parts, the anti-aging agent of 1.5 ~ 5.0 weight parts, the sulphur of 2.0 ~ 6.0 weight parts, the promotor of 0.5 ~ 2.0 weight part.
10. a tire tread, comprises the rubber combination described in any one of claim 1 ~ 9.
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| CN201510770721.5A CN105218882A (en) | 2015-11-13 | 2015-11-13 | Improve rubber combination and the application of vulcanized rubber stability |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105504384A (en) * | 2016-01-27 | 2016-04-20 | 江苏爱特恩东台新材料科技有限公司 | Zinc oxide special for natural rubber and preparation method of zinc oxide |
| CN106589482A (en) * | 2016-12-24 | 2017-04-26 | 安徽佳通乘用子午线轮胎有限公司 | Rubber improving vulcanization system and preparation method and application of rubber |
| CN107973950A (en) * | 2017-12-11 | 2018-05-01 | 青岛泰凯英轮胎有限公司 | Environment-friendly type downhole well applications engineering tire tread rubber composition and preparation method thereof |
| FR3065004A1 (en) * | 2017-04-10 | 2018-10-12 | Compagnie Generale Des Etablissements Michelin | RUBBER COMPOSITION BASED ON HIGHLY SATURATED DIENE ELASTOMER AND DITHIOSULFATE SALT |
| FR3065005A1 (en) * | 2017-04-10 | 2018-10-12 | Compagnie Generale Des Etablissements Michelin | TIRE TREAD FOR PNEUMATIC TIRES BASED ON A HIGHLY SATURATED DIENE ELASTOMER |
| CN109942909A (en) * | 2019-03-11 | 2019-06-28 | 浦林成山（山东）轮胎有限公司 | A kind of rubber composition and its application |
| CN112029150A (en) * | 2020-09-14 | 2020-12-04 | 江苏麒祥高新材料有限公司 | Anti-reversion accelerator and preparation method and application thereof |
| CN115678118A (en) * | 2021-07-28 | 2023-02-03 | 北京化工大学 | Rubber composition for high-wear-resistance tire, preparation method, vulcanized rubber and application |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105504384A (en) * | 2016-01-27 | 2016-04-20 | 江苏爱特恩东台新材料科技有限公司 | Zinc oxide special for natural rubber and preparation method of zinc oxide |
| CN105504384B (en) * | 2016-01-27 | 2017-06-30 | 盐城科迈特新材料有限公司 | Special zinc oxide of natural rubber and preparation method thereof |
| CN106589482A (en) * | 2016-12-24 | 2017-04-26 | 安徽佳通乘用子午线轮胎有限公司 | Rubber improving vulcanization system and preparation method and application of rubber |
| CN110475677A (en) * | 2017-04-10 | 2019-11-19 | 米其林集团总公司 | Tire tread based on HI SA highly saturated diene elastomer |
| FR3065004A1 (en) * | 2017-04-10 | 2018-10-12 | Compagnie Generale Des Etablissements Michelin | RUBBER COMPOSITION BASED ON HIGHLY SATURATED DIENE ELASTOMER AND DITHIOSULFATE SALT |
| FR3065005A1 (en) * | 2017-04-10 | 2018-10-12 | Compagnie Generale Des Etablissements Michelin | TIRE TREAD FOR PNEUMATIC TIRES BASED ON A HIGHLY SATURATED DIENE ELASTOMER |
| WO2018189455A1 (en) * | 2017-04-10 | 2018-10-18 | Compagnie Generale Des Etablissements Michelin | Tyre tread based on a highly saturated diene elastomer |
| WO2018189456A1 (en) * | 2017-04-10 | 2018-10-18 | Compagnie Generale Des Etablissements Michelin | Rubber composition made from a highly saturated diene elastomer and a dithiosulfate salt |
| CN110475677B (en) * | 2017-04-10 | 2021-09-03 | 米其林集团总公司 | Tire tread based on highly saturated diene elastomer |
| CN110475676A (en) * | 2017-04-10 | 2019-11-19 | 米其林集团总公司 | The rubber composition made of HI SA highly saturated diene elastomer and dithionate |
| CN110475676B (en) * | 2017-04-10 | 2021-10-29 | 米其林集团总公司 | Rubber composition made of highly saturated diene elastomer and dithiosulfate |
| CN107973950A (en) * | 2017-12-11 | 2018-05-01 | 青岛泰凯英轮胎有限公司 | Environment-friendly type downhole well applications engineering tire tread rubber composition and preparation method thereof |
| CN107973950B (en) * | 2017-12-11 | 2020-01-21 | 泰凯英(青岛)专用轮胎技术研究开发有限公司 | Environment-friendly underground engineering tire tread rubber composition and preparation method thereof |
| CN109942909A (en) * | 2019-03-11 | 2019-06-28 | 浦林成山（山东）轮胎有限公司 | A kind of rubber composition and its application |
| CN109942909B (en) * | 2019-03-11 | 2021-03-16 | 浦林成山（山东）轮胎有限公司 | Rubber composition and application thereof |
| CN112029150A (en) * | 2020-09-14 | 2020-12-04 | 江苏麒祥高新材料有限公司 | Anti-reversion accelerator and preparation method and application thereof |
| CN115678118A (en) * | 2021-07-28 | 2023-02-03 | 北京化工大学 | Rubber composition for high-wear-resistance tire, preparation method, vulcanized rubber and application |
| CN115678118B (en) * | 2021-07-28 | 2024-03-26 | 北京化工大学 | Rubber composition for high-wear-resistance tire, preparation method, vulcanized rubber and application |
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Application publication date: 20160106 |