CN102863650B - Rubber compound peptizer and preparation method thereof - Google Patents
Rubber compound peptizer and preparation method thereof Download PDFInfo
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- CN102863650B CN102863650B CN201210378433.1A CN201210378433A CN102863650B CN 102863650 B CN102863650 B CN 102863650B CN 201210378433 A CN201210378433 A CN 201210378433A CN 102863650 B CN102863650 B CN 102863650B
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- mercaptobenzothiazole
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Abstract
The invention discloses a rubber compound peptizer. The rubber compound peptizer comprises, by weight, 20% to 25% of mercaptobenzothiazole, 40% to 50% of aromatic acids and the balance fatty glyceride, wherein the weight ratio between the mercaptobenzothiazole and the aromatic acid is 1:2. The invention further discloses a preparation method of the rubber compound peptizer. According to the rubber compound peptizer, high physical plasticizing and chemical peptization effects on the rubber can be achieved through synergistic effect of all components, the mooney viscosity of the rubber can be remarkably reduced, the plasticity of rubber materials is improved, the uniform dispersion of carbon black and other compounding agents in the rubber materials during rubber mixing can be improved, the crosslinking density of vulcanized rubber and thermostability of a cross bond are improved, and physical and mechanical properties and anti-aging performance of the vulcanized rubber are increased.
Description
Technical field
The invention belongs to field of material engineering technology, be specifically related to a kind of rubber combined peptizer and preparation method thereof.
Background technology
Before solid rubber is processed into rubber item, must plasticate, this is that particularly natural rubber molecular weight is high because of rubber, high resilience, cause the interpolation of required other auxiliary agents to mix all very difficult, let alone homogeneity, thus without the rubber of plasticating particularly natural rubber to be difficult to direct machine-shaping be the rubber item that has use value.The object of plasticating ruptures rubber molecular chain with mechanical shear stress, thereby molecular weight is reduced, make rubber change plastic state into by elastic stage, increase the plasticity-of rubber, be convenient to the further mixed refining process such as rubber and other auxiliary agent materials, weighting agent, strengthening agent.Physical method is realized and being plasticated by extruding, method broken, that shear with powerful machinery, and its time of plasticating is long, and energy consumption is large, labour productivity is low.Peptizer carrys out the Reinforced Rubber effect of plasticating by chemical action, shortens the time of plasticating, has improved labor productivity greatly, has reduced energy consumption.So peptizer is in modern rubber industry, particularly tire industry is used widely.Desirable peptizer should have the good solution effect of moulding, and the vulcanization of rubber, without impact, is not reduced to the physical property of vulcanized rubber, is applicable to modern rubber processing means, nontoxic, pollution-free, consumption is few, effect is strong, the processing temperature wide ranges that adapts to.On market at present main rubber peptizer to have aromatic series thiophenols and aromatic disulfides and aromatic series thiophenols and aromatic series curing be the compound peptizer that principal constituent adds metal complex.Although aromatic series thiophenol and its result of use of aromatic series thiophenols metal-salt peptizer are obvious, the processing temperature scope adapting to is wider, but because it is chlorine-containing compound, to use or produce all can produce severe contamination to environment, more owing to finding that it may have carinogenicity, the developed countries such as current European Union, the U.S., Japan have prohibited and have used ，Er China also to be listed in the chemical list that use is eliminated in restriction.It is mainly DBD(chemical name 2 that aromatic disulfides obtains often applying such peptizer at present; 2;-dibenzoyl Diphenyl disulfide compound); this product is for hot mastication (120 ℃ and more than) successful; but at cold plastication (80 ℃ and following) without positive effect; and Costco Wholesale is high, applies and be subject to certain restriction.Mercaptobenzothiazole compounds has good chemistry to rubber and moulds solution effect, but it is again a kind of thiofide simultaneously, thereby be directly used in rubber plastic steelmaking, particularly under the condition of high temperature, and easily cause sizing material incipient scorch, thereby use and be never promoted as peptizer.Compounded rubber peptizer of the present invention is researched and developed under this technical background.
Along with country requires more and more higher to energy-conserving and environment-protective, rubber industry particularly tyre industry is the enterprise of high energy consumption type, tyre industry needs energy saving and environment friendly peptizer, and his exploitation is bound to can be to rubber industry, and particularly strong pushing effect is played in the energy-conserving and environment-protective work of tyre industry.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of rubber combined peptizer of moulding very by force solution effect that all has under high temperature and cold condition.
The technical problem that the present invention also will solve is to provide the preparation method of above-mentioned rubber combined peptizer.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A peptizer, it comprises the component of following weight percent:
Mercaptobenzothiazole 20 ~ 25%;
Aromatic acid 40 ~ 50%;
Glycerin fatty acid ester complements to 100%;
Wherein, the weight ratio of mercaptobenzothiazole and aromatic acid is 1:2.
Wherein, described mercaptobenzothiazole is 2-mercaptobenzothiazole.
Wherein, described aromatic acid is phenylformic acid.
Wherein, described glycerin fatty acid ester is glyceryl monostearate.Should (be glyceryl monostearate?)
The first preparation method of above-mentioned rubber combined peptizer, mixes the mercaptobenzothiazole of formula ratio, aromatic acid and glycerin fatty acid ester.Above-mentioned mercaptobenzothiazole, aromatic acid and glycerin fatty acid ester can directly be bought from the market.
The second preparation method of above-mentioned rubber combined peptizer; glycerin fatty acid ester is first added in reactor to heat fused while stirring; then be warming up to 100 ~ 110 ℃, then aromatic acid is added rapidly in 5 minutes, temperature is controlled at 100 ~ 120 ℃ until phenylformic acid fusing; finally mercaptobenzothiazole is added; continue to stir, temperature remains on 100 ~ 125 ℃ until molten state material mixes, and blowing drips; through the granulation of convolution condensation granulator, obtain.
The method of calculation that 2-mercaptobenzothiazole, phenylformic acid, glyceryl monostearate add are as follows: by the weight percent of each component, recently calculate charging capacity.
For example total charging capacity is 500Kg, and 2-mercaptobenzothiazole is 25%, phenylformic acid is 50%, glyceryl monostearate is 25%:
2-mercaptobenzothiazole charging capacity=500Kg * 0.25=125Kg;
Phenylformic acid=500Kg * 0.5=250Kg;
Glyceryl monostearate=500Kg * 0.25=125Kg.
For example total charging capacity is 500Kg, and 2-mercaptobenzothiazole is 23%, phenylformic acid is 46%, glyceryl monostearate is 31%:
2-mercaptobenzothiazole charging capacity=500Kg * 0.23=115Kg;
Phenylformic acid=500Kg * 0.46=230Kg;
Glyceryl monostearate=500Kg * 0.31=155Kg.
The action principle of rubber combined its design of peptizer of the present invention is: utilize component rubber to certain physics plasticising and interior lubrication, to there is chemistry and mould solution function, 2-mercaptobenzothiazole component with sulfur-containing radicals structure is fully dissolved in rubber, after under high temperature, 2-mercaptobenzothiazole is heated, under the effect of oxygen, sulfydryl (sulfur-containing radicals) and the rubber molecule generation hydrogen abstraction reaction of decomposing, accelerate to have caused rubber molecular chain generation oxidative degradation, reach the object of quick rubber plastic steelmaking.Under cold condition, under the effect of mechanical shear stress, there is rubber molecule splitting of chain in rubber, the sulfur-containing radicals of 2-mercaptobenzimidazole can be sealed the rubber molecular chain end group of fracture while plasticating very soon, it is lost activity, stop it again to tie poly-, thereby reach the object of rubber plastic steelmaking.And aromatic acid in component has good anti-incipient scorch function and physics plasticising function in mixing process, can assist 2-mercaptobenzothiazole to dissolve in rapidly in rubber, thereby chemistry that 2-mercaptobenzothiazole is good being moulded separate function is able to fast effectively performance, effectively suppresses again 2-mercaptobenzothiazole and may cause the incipient scorch of sizing material under high-temperature condition simultaneously.
Beneficial effect: rubber combined peptizer of the present invention has following advantage:
1. rubber combined peptizer of the present invention is by the synergy between each component, and its action effect is obviously better than single component chemistry peptizer.Through test, confirm, phenylformic acid in component of the present invention and glyceryl monostearate have certain softening and physics plasticising function for rubber, glyceryl monostearate is dissolved in rubber and has good interior lubrication, make that rubber is had to chemistry and mould solution performance with very fast the dissolving in sizing material of 2-mercaptobenzothiazole of sulfur-containing radicals structure, it is moulded solution effect and is able to better performance, both synergies, thus the performance of peptizer effectively improved.
Low-temperature test: take respectively with batch 4 parts of natural rubbers, every part of 100g, wherein 1 part of conduct is blank, another 3 parts of 3 kinds of different peptizers of 1% that add respectively rubber quality, add chemical peptizer DBD(chemical name 2 in respectively, 2,-dibenzoyl Diphenyl disulfide compound), each 1g of the compound peptizer of 2-mercaptobenzimidazole and the present invention, through mill (80 ℃), under equal processing condition, carry out cold plastication, then do the mooney viscosity test of broken-(down)rubber, and contrast with blank, blank Mooney viscosity value is 56, the Mooney viscosity value that adds the compound peptizer of the present invention is 46, 10 Mooney viscosity values have been reduced, and add chemical peptizer DBD and 2-mercaptobenzimidazole Mooney viscosity value is all 55, 1 Mooney viscosity value has only declined, it is to weigh the plastic characteristic parameter of rubber that Mooney viscosity value declines, Mooney viscosity value is lower, the plasticity-of rubber is just better, also be an index of rubber plastic steelmaking complete processing, thereby also reflected the effect of rubber plastic steelmaking.Can illustrate that too peptizer is for the effect of rubber plastic steelmaking.Testing data, also reflect synergistic effect between each component of compounded rubber peptizer of the present invention.
High temperature test 1: take respectively with batch 3 parts of natural rubbers, wherein 1 part of conduct is blank, another 2 parts of 2 kinds of different peptizers that add respectively rubber quality 1%, add chemical peptizer DBD(chemical name 2 in respectively, 2,-dibenzoyl Diphenyl disulfide compound) and each 1g of the compound peptizer of the present invention, through Banbury mixer, under 120 ℃ of same process conditions, plasticate, then do the mooney viscosity test of broken-(down)rubber, and contrast with blank, blank Mooney viscosity value is 72, the Mooney viscosity value that adds the rubber combined peptizer of the present invention is 35, the Mooney viscosity value that adds chemical peptizer DBD is 34, Mooney viscosity value all obviously declines.
High temperature test (equal size test) 2: add the compound peptizer 10g(of the present invention containing 2-mercaptobenzothiazole 25% in 1000g natural rubber), another take respectively with batch 2 parts of natural rubber, every part of 1000g, in 1 part, add the Powdered chemical peptizer of DBD content 25% (DBD+ white carbon black) 10g, in 1 part, add the Powdered 2-mercaptobenzothiazole 10g(2-of content 25% mercaptobenzothiazole+white carbon black), through Banbury mixer, under 120 ℃ of same process conditions, plasticate, then do the mooney viscosity test of broken-(down)rubber, the broken-(down)rubber Mooney viscosity value that adds the rubber combined peptizer of the present invention is 35, and the Mooney viscosity value that adds the broken-(down)rubber of chemical peptizer DBD is 42, the Mooney viscosity value that adds the broken-(down)rubber of 2-mercaptobenzothiazole is 43.Mooney viscosity value all has in various degree and to reduce, and the broken-(down)rubber Mooney viscosity value that adds the rubber combined peptizer of the present invention has reduced more.
The Mooney viscosity value that detects sizing material after hot mastication all occurs obviously declining with blank contrast, in equivalent, use in the compound peptizer of invention and peptizer DBD situation, the Mooney viscosity value that adds the sizing material of peptizer of the present invention is 35, the Mooney viscosity value that adds DBD is 34, than 72 of blank, reduced respectively 37 and 38 Mooney viscosity values, plasticity-is obviously improved.In equal size test, another two contrast glue are compared with blank, low respectively 30 and 29 Mooney viscosity values, all there is obvious reduction, but the rubber combined peptizer of the present invention and single component chemistry peptizer ratio, Mooney viscosity value has declined 37, and this explanation the present invention rubber combined peptizer and single component chemistry peptizer ratio mould that to separate performance stronger.The presentation of results of above two high temperature test compounded rubber peptizer of the present invention there is good high temperature and mould solution function, also reflect between each component under hot conditions to there is synergistic action effect with the same under cold condition simultaneously.Mooney viscosity drop-out value is to weigh the characteristic index of rubber plastic solution effect.It is larger that Mooney viscosity value declines, and illustrate to mould solution effect is unreasonable to think.So no matter compounded rubber peptizer of the present invention is cold condition or hot conditions, all has the good effect of plasticating.And only there is the good solution effect of moulding when the hot mastication as the chemical peptizer DBD of single component etc.But according to rubber item physical property and production process, and Mooney viscosity value is controlled to certain limit in practical application.
2. because phenylformic acid has ramollescence to rubber, glyceryl monostearate has good interior lubrication, except having brought into play in the process of plasticating between component synergy; The heat-dissipating of rubber plastic steelmaking process be can alleviate, thereby reach, incipient scorch, particularly natural rubber while being effectively suppressed at rubber high temperature refining glue, occurred.(shifting to an earlier date vulcanization reaction)
3.2-mercaptobenzothiazole is a kind of thiofide, because of and can promote the formation of the cross-link bond of vulcanized rubber when the vulcanization of rubber, thereby play physical and mechanical properties effect and the ageing resistance that improves cross-linked rubber.Overcome the detrimentally affect of peptizer to rubber vulcanization system and cured properties generation.
Embodiment
According to following embodiment, the present invention may be better understood.Yet, those skilled in the art will readily understand, the described content of embodiment is only for the present invention is described, and should also can not limit the present invention described in detail in claims.
Embodiment 1:
Preparation 500Kg, 2-mercaptobenzimidazole is 25%, phenylformic acid is 50%, glyceryl monostearate is 25%:
2-mercaptobenzimidazole charging capacity=500Kg * 0.25=125Kg;
Phenylformic acid=500Kg * 0.5=250Kg;
Glyceryl monostearate=500Kg * 0.25=125Kg.
Take 125Kg glyceryl monostearate and first add in reactor heat fused while stirring, be then warming up to 100-110 ℃, then in 5 minutes, phenylformic acid 250Kg added rapidly; keep temperature to be controlled between 100-120 ℃, cover kettle cover, until phenylformic acid all melts; finally add 125Kg2-mercaptobenzothiazole is disposable; continue to stir, temperature remains on 100 ~ 120 ℃, about 5-10 minute; until material mixes; blowing, through the granulation of convolution condensation granulator, obtains.
Embodiment 2:
Total charging capacity is 500Kg, and 2-mercaptobenzothiazole is 23%, phenylformic acid is 46%, glyceryl monostearate is 31%:
2-mercaptobenzothiazole charging capacity=500Kg * 0.23=115Kg;
Phenylformic acid=500Kg * 0.46=230Kg;
Glyceryl monostearate=500Kg * 0.31=155Kg;
Take 155Kg glyceryl monostearate and first add in reactor heat fused while stirring, be then warming up to 100-110 ℃, then in 5 minutes, phenylformic acid 230Kg added rapidly; keep temperature to be controlled between 100-120 ℃, cover kettle cover, until phenylformic acid all melts; finally add 115Kg2-mercaptobenzothiazole is disposable; continue to stir, temperature remains on 100-120 ℃, about 5-10 minute; until material mixes; blowing, through the granulation of convolution condensation granulator, obtains.
Embodiment 3:
Total charging capacity is 500Kg, and 2-mercaptobenzothiazole is 20%, phenylformic acid is 40%, glyceryl monostearate is 40%:
2-mercaptobenzothiazole charging capacity=500Kg * 0.20=100Kg;
Phenylformic acid=500Kg * 0.40=200Kg;
Glyceryl monostearate=500Kg * 0.40=200Kg;
The mercaptobenzothiazole of formula ratio, aromatic acid and glycerin fatty acid ester are mixed.
Embodiment 4:
The rubber combined peptizer of embodiment 1 preparation of take is detected object, carry out moulding of product of the present invention and separate performance and other quantitative measurements of cross-linked rubber, and the performance of chemical peptizer DBD and blank simultaneous test compares:
1. plasticity test formula is in Table 1.
Table 1
| Starting material title | Blank | Test recipe | Comparative formula |
| Natural rubber | 300g | 300g | 300g |
| Peptizer of the present invention | 3g | ||
| Peptizer DBD | 3g |
Test-results is in Table 2.
Table 2
From table 2 data declaration, the rubber combined peptizer of the present invention (AT-HS), all has and significantly moulds solution effect at high temperature (120 ℃) and low temperature (80 ℃).
2. mechanical property of vulcanized rubber impact test is in Table 3.
Table 3 test recipe content *
Note: * data unit is part one of the percentage of rubber quality (take be 1 part)
2, starting material
Starting material in table 3 are the conventional starting material of tire industry.
1 natural gum: Malaysian import;
The import of 2 stearic acid (1801) Indonesia;
3 zinc oxide (indirect method) content, 99.5% Anhui Han Shan zinc oxide factory;
The holy chemical industry difficult to understand in 4 anti-aging agent (4020) Jiangsu;
5 vulcanizing agents (IS7520) Wuxi qian bridge rubber ingredients factory;
6 companies of chemical peptizer DBD Wuhan Jinghe Chemical Co., Ltd;
7 compounded rubber peptizer of the present invention (AT-HS) Jiangsu Ka Ou Chemical Co., Ltd.s.
3, key instrument and equipment
4, on cured properties impact, cured properties test result is in Table 4.
Table 4
From above-mentioned table 4 test data, show, the sizing material through plasticating with the rubber combined peptizer of the present invention and DBD peptizer, carries out cured properties contrast test, with blank contrast, becomes the T of instrument test from sulphur
10/ min plays sulphur time and T
90/ min sulfurizing time is without large difference, and the vulcanization process of compounded rubber peptizer of the present invention to rubber, illustrates not impact.From mechanical properties of rubber compound test data and ageing resistance data, analyze, substantially without large difference, this reflects the performance of cross-linked rubber is not produced to detrimentally affect yet.
Claims (6)
1. a rubber combined peptizer, is characterized in that, it comprises the component of following weight percent:
Mercaptobenzothiazole 20～25%;
Aromatic acid 40～50%;
Glycerin fatty acid ester complements to 100%;
Wherein, the weight ratio of mercaptobenzothiazole and aromatic acid is 1:2.
2. rubber combined peptizer according to claim 1, is characterized in that, described mercaptobenzothiazole is 2-mercaptobenzothiazole.
3. rubber combined peptizer according to claim 1, is characterized in that, described aromatic acid is phenylformic acid.
4. rubber combined peptizer according to claim 1, is characterized in that, described glycerin fatty acid ester is glyceryl monostearate.
5. the preparation method of rubber combined peptizer claimed in claim 1, is characterized in that, the mercaptobenzothiazole of formula ratio, aromatic acid and glycerin fatty acid ester are mixed.
6. the preparation method of rubber combined peptizer claimed in claim 1; it is characterized in that, glycerin fatty acid ester is first added in reactor to heat fused while stirring, be then warming up to 100～110 ℃; again aromatic acid is added rapidly in 5 minutes; temperature is controlled at 100～120 ℃ until aromatic acid fusing finally adds mercaptobenzothiazole, continues to stir; temperature remain on 100～125 ℃ until molten state material mix; blowing drippage, through the granulation of convolution condensation granulator, obtains.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10179479B2 (en) | 2015-05-19 | 2019-01-15 | Bridgestone Americas Tire Operations, Llc | Plant oil-containing rubber compositions, tread thereof and race tires containing the tread |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360622B (en) * | 2013-08-01 | 2015-04-22 | 江苏卡欧化工有限公司 | Rubber heat-resistant activator and preparation method thereof |
| CN113358441B (en) * | 2021-06-29 | 2024-04-12 | 福州大学 | Standard rubber sample for measuring 2-mercaptobenzothiazole and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531777A (en) * | 2009-03-31 | 2009-09-16 | 浙江巍翔科技有限公司 | Rubber peptizer |
| CN102190812A (en) * | 2010-03-06 | 2011-09-21 | 徐州工业职业技术学院 | Preparation method for environmental-friendly reclaimed rubber |
| CN102304074A (en) * | 2011-06-21 | 2012-01-04 | 聊城大学 | Method for preparing rubber peptizing agent, namely 2,2'-dibenzamido diphenyl disulfide compound |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531777A (en) * | 2009-03-31 | 2009-09-16 | 浙江巍翔科技有限公司 | Rubber peptizer |
| CN102190812A (en) * | 2010-03-06 | 2011-09-21 | 徐州工业职业技术学院 | Preparation method for environmental-friendly reclaimed rubber |
| CN102304074A (en) * | 2011-06-21 | 2012-01-04 | 聊城大学 | Method for preparing rubber peptizing agent, namely 2,2'-dibenzamido diphenyl disulfide compound |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10179479B2 (en) | 2015-05-19 | 2019-01-15 | Bridgestone Americas Tire Operations, Llc | Plant oil-containing rubber compositions, tread thereof and race tires containing the tread |
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