CN102775619A - Preparation method of peroxide vulcanized rubber - Google Patents
Preparation method of peroxide vulcanized rubber Download PDFInfo
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- CN102775619A CN102775619A CN2012102425098A CN201210242509A CN102775619A CN 102775619 A CN102775619 A CN 102775619A CN 2012102425098 A CN2012102425098 A CN 2012102425098A CN 201210242509 A CN201210242509 A CN 201210242509A CN 102775619 A CN102775619 A CN 102775619A
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Abstract
The invention discloses a preparation method of peroxide vulcanized rubber. The preparation method comprises the following steps: a) providing 100 parts by weight of crude rubber and 40-60 parts by weight of packing, and conducting vacuum kneading on the crude rubber and the packing to obtain a kneaded material, wherein the packing is fumed silica; and b) stirring the kneaded material to obtain a peroxide vulcanized rubber product. According to the preparation method of peroxide vulcanized rubber disclosed by the embodiment of the invention, the method is simple in operation, convenient in implementation and mild in preparation conditions; the fumed silica which is adopted as the packing can have the reinforcing effect similar to carbon black; and the peroxide vulcanized rubber which is prepared through modification by utilizing the interaction between fumed silica particles, as well as between the particles and polymer matrix has good resistance to heat, cold, ozone, steam and chemical reagent, as well as good compression permanent deformation property and electrical insulating property.
Description
Technical field
The present invention relates to the rubber technology field, more specifically, the present invention relates to a kind of preparation method of peroxo-type vulcanized rubber.
Background technology
High temperature vulcanizate is the basic glue of high-temperature mixing glue and various vulcanized rubbers, and use temperature is at-5～250 ℃, uses high temperature vulcanizate after the gas-phase silica modification to have good heat-resisting, winter hardiness, anti-ozone, water-fast steam and chemical reagent resistance; Good compression tension set property; Excellent electric insulating.As one type of special synthetic rubber; It has obtained using widely in national economy every field such as aerospace, defence and military, electric, machinofacture, building materials, petrochemical complex, health care, daily lifes, and becomes requisite advanced material.
The crosslinked of high-temperature silicon disulfide rubber mainly realize through organo-peroxide, and specific superoxide decomposes under 100 ℃ the condition being higher than, and produces highly active chemical radical, and these radicals cause the crosslinked of two polysiloxane chains.Each polymer chain generally has 20-40 cross-linking set, and this number deficiency to be producing required physical strength, thereby influences performances such as it is heat-resisting, winter hardiness, anti-ozone.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or provides a kind of useful commerce to select at least.
For this reason, one object of the present invention is to propose the preparation method that a kind of method is simple, implement the vulcanized rubber of peroxo-type easily.
Preparing method according to the peroxo-type vulcanized rubber of the embodiment of the invention; May further comprise the steps: the rubber of 100 weight parts and the filler of 40～60 weight parts a) are provided, and said rubber and filler are carried out vacuum kneading, obtain kneaded material; Wherein, said filler is an aerosil; B) said kneaded material is stirred obtain peroxo-type vulcanized rubber product.
Preparing method according to the peroxo-type vulcanized rubber of the embodiment of the invention; This method is simple to operate; It is convenient to implement; And preparation condition is gentle, adopts aerosil as filler, can have the sooty of being similar to strengthening action; The peroxo-type vulcanized rubber that utilizes interaction and the interaction modification between particulate and the polymeric matrix between the fumed silica particles to make has good thermotolerance, winter hardiness, anti-ozone, water-fast steam and chemical reagent resistance, and has good compression tension set property and excellent electric insulating.
In addition, the preparation method of peroxo-type vulcanized rubber according to the above embodiment of the present invention can also have following additional technical characterictic:
According to one embodiment of present invention; Said rubber is a methyl vinyl silicon kautschuk, and said methyl vinyl silicon kautschuk is obtained by octamethylcyclotetrasiloxane or dimethyl-ring siloxane mixture and tetramethyl-tetrem thiazolinyl cyclotetrasiloxane or the ring-opening polymerization under the katalysis of catalyzer of methyl ethylene ring siloxane mixture.
According to one embodiment of present invention, said catalyzer is Me
4NOH, the catalyzed reaction temperature is 90～110 ℃.
According to one embodiment of present invention, in said step a), also comprise: add the auxiliary agent of 1.5～3 weight parts, said auxiliary agent is to be selected from pigment, heat-resisting additive, fire retardant, the whipping agent one or more.
According to one embodiment of present invention, the kneading temperature in the said step a) is 110～130 ℃, and kneading pressure is 0.070MPa～0.080MPa, and the kneading time is 3～5h.
According to one embodiment of present invention, said step b) comprises: the antistructurizing agent of 5～12 weight parts, 1～1.5 part linking agent and the vulcanizing agent of 1～2 weight part are added kneaded material, stir and obtain peroxo-type vulcanized rubber product.
According to one embodiment of present invention, said antistructurizing agent be selected from divalent alcohol, two organic basic ring silicon ethers, two organic radical silicon diols, organoalkoxysilane, hydroxy silicon oil, contain the Si-N key silicoorganic compound, contain in the silicoorganic compound of Si-O-B key one or more.
According to one embodiment of present invention, said linking agent is vinyl ZGK 5 or Methyl Hydrogen Polysiloxane Fluid.
According to one embodiment of present invention; Said vulcanizing agent is an organo-peroxide; Said organo-peroxide is for being selected from Lucidol, 2; 4-dichlorobenzoperoxide, the peroxo-phenylformic acid tertiary butyl, di-t-butyl peroxide, Di Cumyl Peroxide 99,2,5-dimethyl--2, one or more in the 5-di-t-butyl hexane peroxide.
According to one embodiment of present invention, in said step b), stirring pressure is 0.095MPa～0.100MPa.
According to one embodiment of present invention, also comprise: c) said peroxo-type vulcanized rubber product is distributed into only.
According to one embodiment of present invention, said peroxo-type vulcanized rubber is vertically placed deformation quantity and is not more than 2.5mm, and horizontal positioned does not deform; The extrudability 10s that is not more than of said peroxo-type vulcanized rubber, surface drying time is not more than 3h; Shao Er hardness is 20～60, and said peroxo-type vulcanized rubber is not less than 0.65MP 23 ℃ of stretched intensity.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize through practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage obviously with are easily understood becoming the description of embodiment from combining figs, wherein:
Fig. 1 is the schematic flow sheet according to the preparation method of peroxo-type vulcanized rubber of the present invention.
Embodiment
Describe embodiments of the invention below in detail, the example of said embodiment is shown in the drawings.Be exemplary through the embodiment that is described with reference to the drawings below, only be used to explain the present invention, and can not be interpreted as limitation of the present invention.
At first, the flow process of describing according to the preparation method of peroxo-type vulcanized rubber of the present invention with reference to figure 1.
Particularly, the preparation method of peroxo-type vulcanized rubber of the present invention may further comprise the steps:
A) rubber of 100 weight parts and the filler of 40～60 weight parts are provided, and said rubber and filler are carried out vacuum kneading, obtain kneaded material, wherein, said filler is an aerosil;
B) said kneaded material is stirred obtain peroxo-type vulcanized rubber product.
Preparing method according to the peroxo-type vulcanized rubber of the embodiment of the invention; This method is simple to operate; It is convenient to implement; And preparation condition is gentle, adopts aerosil as filler, can have the sooty of being similar to strengthening action; The peroxo-type vulcanized rubber that utilizes interaction and the interaction modification between particulate and the polymeric matrix between the fumed silica particles to make has good thermotolerance, winter hardiness, anti-ozone, water-fast steam and chemical reagent resistance, and has good compression tension set property and excellent electric insulating.
In said step a), said rubber is a methyl vinyl silicon kautschuk.About said methyl vinyl silicon kautschuk, it will be appreciated that said methyl vinyl silicon kautschuk is by octamethylcyclotetrasiloxane (D
4) or dimethyl-ring siloxane mixture (DMC) and tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4V
i) or methyl ethylene ring siloxane mixture (VMC) ring-opening polymerization under the katalysis of catalyzer obtain.Said catalyzer is TMAH (Me
4NOH), the catalyzed reaction temperature is preferably 90～110 ℃.
In order to increase the function and the characteristic of said peroxo-type vulcanized rubber, can increase the auxiliary agent of 1.5～3 weight parts as required, said auxiliary agent can be for being selected from pigment, heat-resisting additive, fire retardant, the whipping agent one or more.Said pigment, heat-resisting additive, fire retardant, whipping agent can be chemical field pigment, heat-resisting additive, fire retardant, whipping agent commonly used.The peroxo-type vulcanized rubber that makes thus can have specific color, thermotolerance, flame resistivity and other characteristics.
About the condition of said kneading, preferably mediating temperature is 110～130 ℃, and kneading pressure is 0.070MPa～0.080MPa, and the kneading time is 3～5h.
About said step b); It will be appreciated that; When said kneaded material is stirred; In order to strengthen the performance of said peroxo-type vulcanized rubber, can in said kneaded material, add the vulcanizing agent of antistructurizing agent, 1～1.5 parts by weight of cross-linking agent and 1～2 weight part of 5～12 weight parts.（
Said antistructurizing agent is to make its inactivation with the surperficial silicon hydroxyl effect of aerosil; Improve the affinity between aerosil particle and the rubber; The control aerosil is to the physical adsorption and the Chemical bond of rubber molecule; Suppress the generation of hydrogen bond, prevent structurized purpose thereby reach.Consider the cost problem; Preferably, said antistructurizing agent be selected from divalent alcohol, two organic basic ring silicon ethers, two organic radical silicon diols, organoalkoxysilane, hydroxy silicon oil, contain the Si-N key silicoorganic compound, contain in the silicoorganic compound of Si-O-B key one or more.Wherein, the hydroxy silicon oil of using always that ring silazane, hexamethyldisilazane, Diphenylsilanediol and low molar mass are arranged.
About said linking agent, it will be appreciated that the selection of said linking agent does not have particular restriction, preferably, said linking agent can be vinyl ZGK 5 or Methyl Hydrogen Polysiloxane Fluid.
Said vulcanizing agent is an organo-peroxide; Said organo-peroxide is for being selected from Lucidol, 2; 4-dichlorobenzoperoxide, the peroxo-phenylformic acid tertiary butyl, di-t-butyl peroxide, Di Cumyl Peroxide 99,2; 5-dimethyl--2, one or more in the 5-di-t-butyl hexane peroxide.
About said stirring condition, preferred, stirring pressure is 0.095MPa～0.100MPa.
For being processed, so that transport and use, also can said peroxo-type vulcanized rubber further be processed said peroxo-type vulcanized rubber.Its concrete operations can for: said peroxo-type vulcanized rubber only is distributed into through filling machine, and the controlling quality index is following: said peroxo-type vulcanized rubber is vertically placed deformation quantity and is not more than 2.5mm, and horizontal positioned does not deform; The extrudability 10s that is not more than of said peroxo-type vulcanized rubber, surface drying time is not more than 3h; Shao Er hardness is 20～60, and said peroxo-type vulcanized rubber is not less than 0.65MP 23 ℃ of stretched intensity.
Specifically describe the peroxo-type vulcanized rubber for preparing gained according to above-mentioned preparation method below.
Said peroxo-type vulcanized rubber is obtained through polymerization by rubber raw materials, contains the rubber of 100 weight parts and the filler of 40～60 weight parts in the said rubber raw materials, and said filler is an aerosil.
In one example, said filler carries out modification through the antistructurizing agent of 5～12 weight parts.Said antistructurizing agent is to make its inactivation with the surperficial silicon hydroxyl effect of aerosil; Improve the affinity between aerosil particle and the rubber; The control aerosil is to the physical adsorption and the Chemical bond of rubber molecule; Suppress the generation of hydrogen bond, prevent structurized purpose thereby reach.Consider the cost problem; Preferably, said antistructurizing agent be selected from divalent alcohol, two organic basic ring silicon ethers, two organic radical silicon diols, organoalkoxysilane, hydroxy silicon oil, contain the Si-N key silicoorganic compound, contain in the silicoorganic compound of Si-O-B key one or more.Wherein, the hydroxy silicon oil of using always that ring silazane, hexamethyldisilazane, Diphenylsilanediol and low molar mass are arranged.
In one example, said rubber prepares said peroxo-type vulcanized rubber through 1～1.5 part the linking agent and the vulcanizing agent generation polymerization of 1～2 weight part.
In one example; Said linking agent is vinyl ZGK 5 or Methyl Hydrogen Polysiloxane Fluid; Said vulcanizing agent is an organo-peroxide, and said organo-peroxide is for being selected from Lucidol, 2,4-dichlorobenzoperoxide, the peroxo-phenylformic acid tertiary butyl, di-t-butyl peroxide, Di Cumyl Peroxide 99,2; 5-dimethyl--2, one or more in the 5-di-t-butyl hexane peroxide.
In one example, said rubber is a methyl vinyl silicon kautschuk.About said methyl vinyl silicon kautschuk, it will be appreciated that said methyl vinyl silicon kautschuk is by octamethylcyclotetrasiloxane (D
4) or dimethyl-ring siloxane mixture (DMC) and tetramethyl-tetrem thiazolinyl cyclotetrasiloxane (D
4V
i) or methyl ethylene ring siloxane mixture (VMC) ring-opening polymerization under the katalysis of catalyzer obtain.Said catalyzer is TMAH (Me
4NOH), the catalyzed reaction temperature is preferably 90～110 ℃.
In one example, also be added with the auxiliary agent of 1.5～3 weight parts in the said rubber raw materials, said auxiliary agent is to be selected from pigment, heat-resisting additive, fire retardant, the whipping agent one or more.
In one example, said peroxo-type vulcanized rubber is vertically placed deformation quantity and is not more than 2.5mm, and horizontal positioned does not deform; The extrudability 10s that is not more than of said peroxo-type vulcanized rubber, surface drying time is not more than 3h; Shao Er hardness is 20～60, and said peroxo-type vulcanized rubber is not less than 0.65MP 23 ℃ of stretched intensity.
Below in conjunction with specific embodiment the preparation method according to peroxo-type vulcanized rubber of the present invention is described.
Embodiment 1
Get the methyl vinyl silicon kautschuk of 100 weight parts, the aerosil of 40～60 weight parts, 1～1.5 parts by weight of cross-linking agent is carried out vacuum kneading, and mediating temperature is 110～130 ℃, and kneading pressure is 0.07～0.08Mpa, and the kneading time is 3～5h.
Get the ring silazane of 5～12 weight parts; 2 of 1～2 weight part; 5-dimethyl--2,5-di-t-butyl hexane peroxide solution is at vacuum tightness-0.095～0.100Mpa; Nitrogen protection during adding assistant 1.5～3 weight part C glue (tetrabromo-bisphenol) is used planet machine high speed, stirring at low speed and is reached requirement fineness≤50 μ m; Denseness 9.3～10.3 obtains peroxo-type vulcanized rubber product.
Peroxo-type vulcanized rubber product only is distributed into through filling machine, and controlling index is not more than 2.5mm for the vertical deformation quantity of placing, and horizontal positioned does not deform; The extrudability 10s that is not more than of said peroxo-type vulcanized rubber, surface drying time is not more than 3h; Shao Er hardness is 20～60, and said peroxo-type vulcanized rubber is not less than 0.65MP 23 ℃ of stretched intensity, obtains peroxo-type vulcanized rubber.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means the concrete characteristic, structure, material or the characteristics that combine this embodiment or example to describe and is contained at least one embodiment of the present invention or the example.In this manual, the schematic statement to above-mentioned term not necessarily refers to identical embodiment or example.And concrete characteristic, structure, material or the characteristics of description can combine with suitable manner in any one or more embodiment or example.
Although illustrated and described embodiments of the invention; Those having ordinary skill in the art will appreciate that: under the situation that does not break away from principle of the present invention and aim, can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited claim and equivalent thereof.
Claims (12)
1. the preparation method of a peroxo-type vulcanized rubber is characterized in that, may further comprise the steps:
A) rubber of 100 weight parts and the filler of 40～60 weight parts are provided, and said rubber and filler are carried out vacuum kneading, obtain kneaded material, wherein, said filler is an aerosil;
B) said kneaded material is stirred obtain peroxo-type vulcanized rubber product.
2. the preparation method of peroxo-type vulcanized rubber according to claim 1; It is characterized in that; Said rubber is a methyl vinyl silicon kautschuk, and said methyl vinyl silicon kautschuk is obtained by octamethylcyclotetrasiloxane or dimethyl-ring siloxane mixture and tetramethyl-tetrem thiazolinyl cyclotetrasiloxane or the ring-opening polymerization under the katalysis of catalyzer of methyl ethylene ring siloxane mixture.
3. the preparation method of peroxo-type vulcanized rubber according to claim 2 is characterized in that, said catalyzer is Me
4NOH, the catalyzed reaction temperature is 90～110 ℃.
4. the preparation method of peroxo-type vulcanized rubber according to claim 1; It is characterized in that; In said step a), also comprise: add the auxiliary agent of 1.5～3 weight parts, said auxiliary agent is to be selected from pigment, heat-resisting additive, fire retardant, the whipping agent one or more.
5. the preparation method of peroxo-type vulcanized rubber according to claim 1 is characterized in that, the kneading temperature in the said step a) is 110～130 ℃, and kneading pressure is 0.070MPa～0.080MPa, and the kneading time is 3～5h.
6. the preparation method of peroxo-type vulcanized rubber according to claim 1; It is characterized in that; Said step b) comprises: the vulcanizing agent of antistructurizing agent, 1～1.5 parts by weight of cross-linking agent and 1～2 weight part of 5～12 weight parts is added kneaded material, stir and obtain peroxo-type vulcanized rubber product.
7. the preparation method of peroxo-type vulcanized rubber according to claim 6; It is characterized in that, said antistructurizing agent be selected from divalent alcohol, two organic basic ring silicon ethers, two organic radical silicon diols, organoalkoxysilane, hydroxy silicon oil, contain the Si-N key silicoorganic compound, contain in the silicoorganic compound of Si-O-B key one or more.
8. the preparation method of peroxo-type vulcanized rubber according to claim 6 is characterized in that, said linking agent is vinyl ZGK 5 or Methyl Hydrogen Polysiloxane Fluid.
9. the preparation method of peroxo-type vulcanized rubber according to claim 6; It is characterized in that; Said vulcanizing agent is an organo-peroxide, and said organo-peroxide is for being selected from Lucidol, 2,4-dichlorobenzoperoxide, the peroxo-phenylformic acid tertiary butyl, di-t-butyl peroxide, Di Cumyl Peroxide 99,2; 5-dimethyl--2, one or more in the 5-di-t-butyl hexane peroxide.
10. the preparation method of peroxo-type vulcanized rubber according to claim 1 is characterized in that, in said step b), stirring pressure is 0.095MPa～0.100MPa.
11. the preparation method of peroxo-type vulcanized rubber according to claim 1 is characterized in that, also comprises:
C) said peroxo-type vulcanized rubber product is distributed into only.
12. the preparation method of peroxo-type vulcanized rubber according to claim 11 is characterized in that, the peroxo-type vulcanized rubber after the said packing is vertically placed deformation quantity and is not more than 2.5mm, and horizontal positioned does not deform; The extrudability 10s that is not more than of said peroxo-type vulcanized rubber, surface drying time is not more than 3h; Shao Er hardness is 20～60, and said peroxo-type vulcanized rubber is not less than 0.65MP 23 ℃ of stretched intensity.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103351621A (en) * | 2013-05-31 | 2013-10-16 | 镇江天信电器有限公司 | Insulation rubber tube for heater, and making method thereof |
| CN106398225A (en) * | 2015-08-03 | 2017-02-15 | 苏州沃尔兴电子科技有限公司 | Flame-retardant silicone rubber heat-shrinkable sleeve and preparation method thereof |
| CN108410171A (en) * | 2018-02-09 | 2018-08-17 | 宁波安工电子有限公司 | A kind of sulfuration resistant LED encapsulation organosilicon material and preparation method thereof |
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2012
- 2012-07-12 CN CN2012102425098A patent/CN102775619A/en active Pending
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103351621A (en) * | 2013-05-31 | 2013-10-16 | 镇江天信电器有限公司 | Insulation rubber tube for heater, and making method thereof |
| CN106398225A (en) * | 2015-08-03 | 2017-02-15 | 苏州沃尔兴电子科技有限公司 | Flame-retardant silicone rubber heat-shrinkable sleeve and preparation method thereof |
| CN108410171A (en) * | 2018-02-09 | 2018-08-17 | 宁波安工电子有限公司 | A kind of sulfuration resistant LED encapsulation organosilicon material and preparation method thereof |
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Application publication date: 20121114 |