CN103087273A - Improved grafting and crosslinking vulcanization compound and method for vulcanizing silicon rubber - Google Patents
Improved grafting and crosslinking vulcanization compound and method for vulcanizing silicon rubber Download PDFInfo
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- CN103087273A CN103087273A CN2013100259539A CN201310025953A CN103087273A CN 103087273 A CN103087273 A CN 103087273A CN 2013100259539 A CN2013100259539 A CN 2013100259539A CN 201310025953 A CN201310025953 A CN 201310025953A CN 103087273 A CN103087273 A CN 103087273A
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Abstract
The invention provides an improved grafting and crosslinking vulcanization compound and a method for vulcanizing silicon rubber. A vulcanization system comprises an organic peroxide initiator and a silane crosslinking agent in a specific structure. The method for vulcanizing the silicon rubber comprises the following steps of: mixing raw silicon rubber and fumed silica, adding the organic peroxide initiator and the silane crosslinking agent, mixing, vulcanizing the mixed materials at the temperature of 160-200 DEG C by mould pressing, and vulcanizing for the second time at the temperature of 180-200 DEG C. Due to the adoption of the grafting and crosslinking vulcanization system, a carbon-carbon bond crosslinked structure and a silicon-oxygen bond micro-crosslinked structure are generated in the process of vulcanizing the silicon rubber, so that the mechanical properties of the vulcanized silicon rubber are improved greatly.
Description
Technical field
The present invention relates to a kind of for silicon rubber the graft crosslinking vulcanization system and make the method for silicon rubber vulcanization, belong to the rubber technology field.
Background technology
High-temperature silicon disulfide rubber is one of most important organosilicon product.Sulfuration is one of main processes of rubber item processing, is also last manufacturing procedure during rubber item is produced.In this operation, rubber will experience the chemical transformation of series of complex, becomes elastomeric cross-linked rubber by the rubber unvulcanizate of plasticity, thereby obtains perfect physical and mechanical properties and chemical property, gives elastomeric material use value.Therefore, sulfuration is of great significance manufacturing and the application tool of rubber and goods thereof.
Sulfidation is the process of rubber macromolecule chain generation chemical crosslink reaction, comprises the series of chemical that occurs between rubber molecule and vulcanizing agent and other Synergist S-421 95s and the various side reactions of following generation when forming reticulated structure.Can be divided into three phases:
1. induction period: the reaction between vulcanizing agent, promoting agent, promotor, generate active intermediate compound, then further cause rubber molecular chain, produce crosslinkable free radical or ion.
2. crosslinking reaction stage: produce chain reaction between crosslinkable free radical or ion and rubber molecular chain, generate cross-link bond.
3. net is configured to the stage: the rearrangement of cross-link bond, shortization, backbone modification, cracking.
1839, American Charles Goodyear discovery rubber and Sulfur heat together can obtain cross-linked rubber;
1906-1914 has determined that the vulcanization of rubber is theoretical, thinks that sulfuration is mainly at the intermolecular sulfide that generated;
1846, Parkes found that the solution of SCl or steam at room temperature also can vulcanized rubbers, is called " cold vulcanization method ";
1915, found peroxide cure;
1918, found the sulfuration of the elements such as selenium, tellurium;
Nineteen thirty, found the low-sulfur vulcanization process;
1940, in succession found the sulfuration of resin cure and quinone oximes;
Nineteen forty-three, found sulfur-donor cure;
Novel vulcanization system has appearred again later in World War II, as finding radiation vulanization the fifties; The seventies urea alkane vulcanization system; Balance curing system has been proposed the eighties.
Silicon rubber mainly contains three the most frequently used vulcanization systems at present: the condensation vulcanization system of peroxide vulcanizing system, silicon hydrogen addition vulcanization system, functional group.Various cross-linking systems have the different scope of application and application conditions.
The graft crosslinking vulcanization system of silicon rubber is a kind of novel vulcanization system in the silicon rubber field, but graft crosslinking is in other materials such as polypropylene, the existing research in polyethylene field.The people such as Shieb, Sen with the method for FUR, DSC research silane grafted polyethylene reaction, studies the reaction of Silane Grafted high density polyethylene(HDPE) and Low Density Polyethylene in recent years.Silane grafting and crosslinking polyethylene products such as cable, heat-shrink tube, hot-water line etc. have obtained widespread use.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of improved graft crosslinking cure system composition and the method that makes silicon rubber vulcanization.
Technical scheme of the present invention is as follows:
A kind of graft crosslinking cure system composition for sulfuration silicon rubber raw rubber, it comprises:
0.2 the silane crosslinker of ~ 5 parts/100 parts of raw-silastic continuouslies, wherein said silane crosslinker are vinyltrimethoxy silane, vinyltriethoxysilane or vinyl silane tri-butyl peroxy; With
0.01 the organic peroxide evocating agent of ~ 5 parts/100 parts of raw-silastic continuouslies, wherein said organic peroxide evocating agent is 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, dicumyl peroxide, dibenzoyl peroxide, or bis(2，4-dichlorobenzoyl)peroxide;
Above proportioning is weight part, and is lower same.
The preferred graft crosslinking cure system composition according to the present invention, weight part is composed as follows:
0.5 the silane crosslinker of ~ 1.5 parts/100 parts of raw-silastic continuouslies, the organic peroxide evocating agent of 0.1 ~ 1 part/100 parts of raw-silastic continuouslies.
The preferred graft crosslinking cure system composition according to the present invention, wherein, silane crosslinker is vinyltrimethoxy silane or vinyl silane tri-butyl peroxy.
The preferred graft crosslinking cure system composition according to the present invention, wherein, organic peroxide evocating agent is 2,5-dimethyl-2,5-bis(t-butylperoxy) or dicumyl peroxide.
A kind of vulcanizable rubber composition, it comprises:
A, raw-silastic continuously, 100 parts;
B, thermal silica, 30～60 parts;
C, the silane crosslinker of 0.2 ~ 5 part, wherein said silane crosslinker is vinyltrimethoxy silane, vinyltriethoxysilane or vinyl silane tri-butyl peroxy; With
D, the organic peroxide evocating agent of 0.01 ~ 5 part, wherein said organic peroxide evocating agent is 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, dicumyl peroxide, dibenzoyl peroxide, or bis(2，4-dichlorobenzoyl)peroxide;
Above proportioning is weight part, and is lower same.
According to vulcanizable rubber composition of the present invention, wherein, described raw-silastic continuously is selected from methyl vinyl silicone rubber, and molecular weight is 400000～600000(weight average); The vinyl molar content is 0.04%～0.3%.
According to the present invention, a kind of method that makes silicon rubber vulcanization comprises the following steps:
100 parts of raw-silastic continuouslies are provided; 30～60 parts of thermal silicas are provided;
Graft crosslinking cure system composition of the present invention is provided;
Contact with described graft crosslinking cure system composition after making described raw-silastic continuously, thermal silica mixing; With
Vulcanize whereby described raw-silastic continuously, get silicon rubber vulcanization glue.
Preferably make the method for silicon rubber vulcanization according to the present invention, described contact procedure is carried out under 160-200 ℃.
Further preferably make the method for silicon rubber vulcanization according to the present invention, carry out according to the following steps:
By proportioning, raw-silastic continuously, thermal silica are added on mixing roll mixing 20～30 minutes successively, then with the thermal treatment 1 hour under 160 ℃ of conditions of mixing material; Then organic peroxide evocating agent and silane crosslinker are added on mixing roll mixing 10～20 minutes; Material after mixing molded vulcanization 20～25 minutes at 160-200 ℃ of temperature, then carried out post vulcanization 2 hours under 180-200 ℃ of condition.
The present invention is take raw-silastic continuously as basic glue, the strengthening agent of holding concurrently take thermal silica as filler, and the proportioning of the silane crosslinker by adjusting organic peroxide evocating agent and ad hoc structure is carried out graft crosslinking.Improve the mechanical property of silicon rubber by new crosslinking method.The dominant mechanism of graft crosslinking of the present invention is to add the silane of organo-peroxide and ad hoc structure in silicon rubber is the rubber unvulcanizate of basic glue, organo-peroxide is as the initiator of graft reaction, the silane of ad hoc structure is as linking agent, make that carbon carbon can occur between the silicon rubber molecule is crosslinked, as shown in Figure 1, also can make simultaneously and produce the little crosslinking structure of silica silicon between the silicon rubber molecule, as shown in Figure 2.The more traditional silicon rubber vulcanization system of vulcanization system of the present invention can significantly improve the mechanical property of silicon rubber.
Description of drawings
Fig. 1 is the crosslinked schematic diagram of carbon carbon between the silicon rubber molecule.
Fig. 2 produces the schematic diagram of the little crosslinking structure of silica silicon between the silicon rubber molecule.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated, but be not limited to this.The embodiment Raw is described as follows:
Raw-silastic continuously: methyl vinyl silicone rubber, its contents of ethylene ratio is 0.16%; Weight-average molecular weight
Thermal silica: the TS530 that U.S. Cabot Co.,Ltd produces.
Embodiment 1: do not add silane crosslinker, as a comparison case.
Get following component with weight part score another name: 100 parts of raw-silastic continuouslies (methyl vinyl silicone rubber), 50 parts of thermal silicas, organo-peroxide 2,5-dimethyl-2,1 part of 5-bis(t-butylperoxy) hexane.First with the raw-silastic continuously of group component, thermal silica is added on mixing roll mixing 30 minutes successively, then with the thermal treatment 1 hour under 160 ℃ of conditions of mixing material.Then 1 part of organo-peroxide is added on mixing roll mixing 10 minutes.Material after mixing molded vulcanization 20 minutes at 170 ℃ of temperature, then carried out post vulcanization 2 hours under 180 ℃ of conditions.
Embodiment 2:
Get following component with weight part score another name: raw-silastic continuously (methyl vinyl silicone rubber, its contents of ethylene ratio is 0.16%) 100 parts, 50 parts of thermal silicas, organo-peroxide (2, the 5-dimethyl--2,5 bis(t-butylperoxy)s) 1 part, 0.5 part of vinyltrimethoxy silane.First raw-silastic continuously, the thermal silica of group component is added to successively on mixing roll mixing 30 minutes, then with the thermal treatment 1 hour under 160 ℃ of conditions of mixing material.Then 0.5 part of 1 part of organo-peroxide, vinyltrimethoxy silane is added on mixing roll mixing 10 minutes.Material after mixing molded vulcanization 20 minutes at 170 ℃ of temperature, then carried out post vulcanization 2 hours under 180 ℃ of conditions.
Embodiment 3:
Get following component with weight part score another name: raw-silastic continuously (methyl vinyl silicone rubber, its contents of ethylene ratio is 0.16%) 100 parts, 50 parts of thermal silicas, organo-peroxide (2,5-dimethyl-2,5-bis(t-butylperoxy)) 1 part, 0.8 part of vinyltrimethoxy silane.First raw-silastic continuously, the thermal silica of group component is added to successively on mixing roll mixing 30 minutes, then with the thermal treatment 1 hour under 160 ℃ of conditions of mixing material.Then 0.8 part of 1 part of organo-peroxide, vinyltrimethoxy silane is added on mixing roll mixing 10 minutes.Material after mixing molded vulcanization 20 minutes at 170 ℃ of temperature, then carried out post vulcanization 2 hours under 180 ℃ of conditions.
Embodiment 4:
Get following component with weight part score another name: raw-silastic continuously (methyl vinyl silicone rubber, its contents of ethylene ratio is 0.16%) 100 parts, 50 parts of thermal silicas, 0.3 part of organo-peroxide (dicumyl peroxide), 0.5 part of vinyl silane tri-butyl peroxy.First raw-silastic continuously, the thermal silica of group component is added to successively on mixing roll mixing 30 minutes, then with the thermal treatment 1 hour under 160 ℃ of conditions of mixing material.Then 0.5 part of 0.3 part of organo-peroxide, vinyl silane tri-butyl peroxy is added on mixing roll mixing 10 minutes.Material after mixing molded vulcanization 20 minutes at 150 ℃ of temperature, then carried out post vulcanization 2 hours under 200 ℃ of conditions.
Embodiment 5:
Get following component with weight part score another name: raw-silastic continuously (methyl vinyl silicone rubber, its contents of ethylene ratio is 0.16%) 100 parts, 50 parts of thermal silicas, 0.3 part of organo-peroxide (dicumyl peroxide), 1 part of vinyl silane tri-butyl peroxy.First raw-silastic continuously, the thermal silica of group component is added to successively on mixing roll mixing 30 minutes, then with the thermal treatment 1 hour under 160 ℃ of conditions of mixing material.Then 1 part of 0.3 part of organo-peroxide, vinyl silane tri-butyl peroxy is added on mixing roll mixing 10 minutes.Material after mixing molded vulcanization 20 minutes at 150 ℃ of temperature, then carried out post vulcanization 2 hours under 200 ℃ of conditions.
Silicon rubber vulcanization glue goods to above-described embodiment 1～5 gained carry out Mechanics Performance Testing, and tensile strength, elongation at break, 100% stress at definite elongation are pressed the GB/T528-1998 test, and tear strength is pressed the GB/T529-1999 test, and hardness is pressed the GB/T531-1999 test.The results are shown in Table 1.
The mechanical property of table 1, embodiment of the present invention gained cross-linked rubber product
Do not contain the ad hoc structure silane crosslinker in embodiment 1, do not belong to silicon rubber graft crosslinking vulcanization system of the present invention, be common peroxide vulcanizing system cross-linked rubber.Embodiment 2, embodiment 3, embodiment 4, embodiment 5 adopt silicon rubber graft crosslinking vulcanization system of the present invention.As can be seen from Table 1, the mechanical property by silicon rubber graft crosslinking vulcanization system gained cross-linked rubber of the present invention obviously improves a lot; More than silicon rubber graft crosslinking vulcanization system gained cross-linked rubber of the present invention improves 1Mpa than common cross-linked rubber tensile strength, more than tear strength improves 8KN/m.
Claims (9)
1. graft crosslinking cure system composition that is used for sulfuration silicon rubber raw rubber, it comprises:
0.2 the silane crosslinker of ~ 5 parts/100 parts of raw-silastic continuouslies, wherein said silane crosslinker are vinyltrimethoxy silane, vinyltriethoxysilane or vinyl silane tri-butyl peroxy; With
0.01 the organic peroxide evocating agent of ~ 5 parts/100 parts of raw-silastic continuouslies, wherein said organic peroxide evocating agent is 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, dicumyl peroxide, dibenzoyl peroxide, or bis(2，4-dichlorobenzoyl)peroxide;
Above proportioning is weight part.
2. graft crosslinking cure system composition according to claim 1 is characterized in that weight part is composed as follows:
0.5 the silane crosslinker of ~ 1.5 parts/100 parts of raw-silastic continuouslies, the organic peroxide evocating agent of 0.1 ~ 1 part/100 parts of raw-silastic continuouslies.
3. graft crosslinking cure system composition according to claim 1, is characterized in that described silane crosslinker is vinyltrimethoxy silane or vinyl silane tri-butyl peroxy.
4. graft crosslinking cure system composition according to claim 1, is characterized in that described organic peroxide evocating agent is 2,5-dimethyl-2,5-bis(t-butylperoxy) or dicumyl peroxide.
5. vulcanizable rubber composition, it comprises:
A, raw-silastic continuously, 100 parts;
B, thermal silica, 30～60 parts;
C, the silane crosslinker of 0.2 ~ 5 part, wherein said silane crosslinker is vinyltrimethoxy silane, vinyltriethoxysilane or vinyl silane tri-butyl peroxy; With
D, the organic peroxide evocating agent of 0.01 ~ 5 part, wherein said organic peroxide evocating agent is 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, dicumyl peroxide, dibenzoyl peroxide, or bis(2，4-dichlorobenzoyl)peroxide;
Above proportioning is weight part.
6. vulcanizable rubber composition according to claim 5, is characterized in that described raw-silastic continuously is selected from methyl vinyl silicone rubber, and molecular weight is 400000～600000; The vinyl molar content is 0.04%～0.3%.
7. method that makes silicon rubber vulcanization comprises the following steps:
Provide raw-silastic continuously, 100 parts; Weight part;
Provide thermal silica, 30～60 parts; Weight part;
Provide claim 1 ~ 4 any one described graft crosslinking cure system composition;
Contact with described graft crosslinking cure system composition after making described raw-silastic continuously, thermal silica mixing; With
Vulcanize whereby described raw-silastic continuously, get silicon rubber vulcanization glue.
8. the method that makes silicon rubber vulcanization according to claim 7 is characterized in that described contact procedure carries out under 160-200 ℃.
9. the method that makes silicon rubber vulcanization according to claim 7 is characterized in that carrying out according to the following steps:
By proportioning, raw-silastic continuously, thermal silica are added on mixing roll mixing 20～30 minutes successively, then with the thermal treatment 1 hour under 160 ℃ of conditions of mixing material; Then organic peroxide evocating agent and silane crosslinker are added on mixing roll mixing 10～20 minutes; Material after mixing molded vulcanization 20～25 minutes at 160-200 ℃ of temperature, then carried out post vulcanization 2 hours under 180-200 ℃ of condition.
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Cited By (3)
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| CN103265670A (en) * | 2013-05-11 | 2013-08-28 | 北京化工大学 | Oil-resistant silicon rubber and preparation method thereof by in-situ reaction |
| CN106977926A (en) * | 2017-04-24 | 2017-07-25 | 新昌县恩喜电器有限公司 | A kind of three phase combined over-voltage protector sulphurated siliastic |
| CN114102948A (en) * | 2021-09-26 | 2022-03-01 | 江苏共维电子科技有限公司 | Cable compression molding method adopting solid silica gel |
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| CN114102948A (en) * | 2021-09-26 | 2022-03-01 | 江苏共维电子科技有限公司 | Cable compression molding method adopting solid silica gel |
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Application publication date: 20130508 |