CN103540140A - Preparation method of high-performance mould-press type mixed silicone rubber - Google Patents
Preparation method of high-performance mould-press type mixed silicone rubber Download PDFInfo
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Abstract
The invention relates to the field of silicone rubber materials and particularly relates to a preparation method of high-performance mould-press type mixed silicone rubber. The preparation method comprises the following steps: matching raw materials, kneading the raw materials, curing the rubber material, introducing steam, and performing vacuumizing treatment. The tensile strength, the tear strength, the elongation and other parameters of a rubber product produced by the silicone rubber after treatment by vulcanization are obviously improved, the thermal aging permanent deformation parameter is also in a relatively small range, and the comprehensive mechanical properties are further improved.
Description
Technical field
The present invention relates to silastic material field, particularly a kind of preparation method of high-performance molded type melting silicone rubber.
Background technology
Organosilicon, as a kind of high-tech new type chemical material, has had both the performance of inorganic materials and organic materials, is widely used in the industries such as aerospace, electric, building, transportation, chemical industry, weaving, food, light industry, medical treatment.Along with the sustainable growth of organosilicon quantity and kind, Application Areas is constantly widened, and forms the staple product system that new chemical materials circle is taken the course of its own, and many kinds are that other chemical cannot substitute and requisite.
In material Application Areas, not only require organosilicon material to there is good chemical property, more require it to there is good physicals, in electric wire field of accessories, mechanical property for silastic material has higher requirement, the melting silicone rubber that existing electric wire annex adopts, tensile strength at yield is about 8KN/M, elongation is generally in 800% left and right, tear strength is generally less than 30KN/M, thermal ageing tension set is generally greater than 15%, these parameters are generally determining the scope of application and the work-ing life of rubber, but in some high-end cable accessory goods field, the existing mechanical property of these elastomeric materials still far can not be satisfied the demand.
High-performance molded type melting silicone rubber, in general tear strength >=30KN, tension set≤15%, produce the organic silicon rubber material of this more strong mechanical performance and conventionally need to first prepare special sizing material, then carry out sulfidizing, can obtain the elastomeric material of required performance, and the performance of organo-silicone rubber depends on the properties of rubber before sulfuration to a great extent, the performance of sizing material depends on again composition and the production technique of sizing material, and therefore solving this difficult problem is to obtain more strong mechanical performance and the more key of the silastic material of long life.
Summary of the invention
The object of the present invention is to provide a kind of preparation method for the preparation of thering is the more high performance mold pressing type melting silicone rubber of high tensile strength at yield, high elongation rate, high-tear strength and low thermal ageing tension set.
For achieving the above object, the technical solution adopted in the present invention is: a kind of preparation method of high-performance molded type melting silicone rubber, comprises the following steps:
(1) raw material of the following stated mass parts is mediated evenly:
Methyl vinyl silicon kautschuk total amount is 320～380 parts, and described methyl vinyl silicon kautschuk adopts the different A group rubber of following contents of ethylene and B group rubber to form:
A organizes rubber: contents of ethylene is 0.04%, 0.08%, 0.16%, 0.22%, and any two in 0.30% methyl vinyl silicon kautschuk account for 80%～99% of rubber total amount,
B organizes rubber: contents of ethylene is any one or two kinds of in 2%, 3%, 5%, 10% methyl vinyl silicon kautschuk, accounts for 1%～20% of rubber total amount;
Silicone oil auxiliary agent total amount is 11～18 parts, and described silicone oil auxiliary agent is mixed by following C group silicone oil and D group silicone oil:
C organizes silicone oil: a kind of or several combinations in hydroxy silicon oil, dimethyldimethoxysil,ne, dimethyldiethoxysilane, vinyl hydroxy silicone oil, and every kind of combination must contain first three plants at least one in described silicone oil, C group silicone oil accounts for 80%～95% of silicone oil auxiliary agent total amount;
D organizes silicone oil: silicon oil of low hydrogen content, high containing hydrogen silicone oil one or both, D group silicone oil accounts for 5%～20% of silicone oil auxiliary agent total amount; The hydrogen content of silicon oil of low hydrogen content is generally 0.1%～0.8%, and high hydrogeneous hydrogen content is generally 1.0%～1.6%.
White carbon black is 100～125 parts, and specific area is 200m
2/ g～400m
2/ g;
(2) sizing material obtaining in step (1) is placed at room temperature health 1～12 hour; Described health exactly sizing material is placed on a pallet and cover layer of plastic film after standing.
(3) after the stirring of the sizing material after step (2) health is agglomerating, start logical steam, make sizing material be warming up to 100 ℃～130 ℃, Steam pressure control is between 0.2MPa～0.8MPa, and temperature-rise period is controlled at 1～2 hour;
(4) sizing material, after step (3) temperature-rise period completes, starts to vacuumize, and vacuum degree control is at-0.02MPa～-0.08MPa, and sizing material temperature is controlled at 120 ℃～180 ℃, and the pumpdown time is controlled at 1～3 hour, and the sizing material obtaining is filtered and obtain product.
In order to make rubber there is good processing characteristics, in raw material, be added with the inner pattern releasing agent applicable of 0.05～2.6 part.
In above-mentioned raw materials: the rubber collocation of at least 3 kinds of different contents of ethylene, can make cross-linking set relatively concentrated, cross-linked network comparatively dense, such sizing material, can reach high anti-tear, and the requirements such as high tensile, can control again tension set in 15%.Use multiple silicone oil auxiliary agent as antistructurizing agent, if the amount that silicone oil auxiliary agent adds is too much, sizing material can be clamminess, processing is got up very difficult, if the amount that silicone oil auxiliary agent adds is very few, the silicon rubber quality guaranteed period not long, mechanical property also can variation, silicone oil auxiliary agent also helps the processing to white carbon black, extends the quality guaranteed period of silicon rubber.Above-mentioned raw materials collocation and step can make sizing material have good processing characteristics and mechanical property.
Adopt the high-temperature mixing silicone rubber products of aforesaid method acquisition through 175 ℃ of sulfidizing, after compressing tablet approximately 8 minutes, carry out Mechanical Data analytical test, can obtain than general silastic material, the feature with high tensile strength at yield, high elongation rate, high-tear strength and thermal ageing tension set, can meet the demand of making high-end cable accessory rubber item, and be with a wide range of applications.
Embodiment
Below in conjunction with embodiment, the present invention is made to concrete elaboration.
Embodiment 1
The preparation method of type melting silicone rubber: methyl vinyl silicon kautschuk total amount is a 350kg, therein ethylene base content is to be respectively 0.04%, 0.3%, 5% methyl vinyl silicon kautschuk respectively to account for 60%, 35%, 5% of rubber total amount; Silicone oil auxiliary agent total amount is 15kg, and hydroxy silicon oil accounts for 85%, and silicon oil of low hydrogen content accounts for 15%; Selecting specific area is 300m
2the white carbon black of/g is 120kg; Adopt kneader to mediate evenly above-mentioned raw materials, then the sizing material after mediating is put at room temperature health 6 hours; Again that the sizing material stirring after health is agglomerating, pass into the steam that pressure is 0.4MPa, make sizing material be warming up to 120 ℃, temperature-rise period is controlled at 1.5 hours; After sizing material heats up, start to vacuumize, vacuum degree control is at-0.04MPa, and sizing material temperature is controlled at 150 ℃, and the pumpdown time is controlled at 2 hours, and the sizing material that will obtain obtains product after filtering.
Product is carried out to stripping and slicing and open refining to smooth, adopt two two or five vulcanizing agents at 175 ℃, compressing tablet 8 minutes, carries out Mechanics Performance Testing to rubber, and test result is in Table 1.
Embodiment 2
The preparation method of type melting silicone rubber: methyl vinyl silicon kautschuk total amount is a 320kg, therein ethylene base content is to be respectively 0.04%, 0.22%, 10% methyl vinyl silicon kautschuk respectively to account for 50%, 35%, 15% of rubber total amount; Silicone oil auxiliary agent total amount is 11kg, and wherein hydroxy silicon oil, dimethyldimethoxysil,ne, silicon oil of low hydrogen content respectively account for 50%, 40%, 10% of silicone oil auxiliary agent total amount; Selecting specific area is 200m
2the white carbon black of/g is 110kg; Adopt kneader to mediate evenly above-mentioned raw materials, then the sizing material after mediating is put at room temperature health 1 hour; Again that the sizing material stirring after health is agglomerating, pass into the steam that pressure is 0.2MPa, make sizing material be warming up to 100 ℃, temperature-rise period is controlled at 2 hours; After sizing material heats up, start to vacuumize, vacuum degree control is at-0.02MPa, and sizing material temperature is controlled at 120 ℃, and the pumpdown time is controlled at 1 hour, and the sizing material that will obtain obtains product after filtering.
Product is carried out to stripping and slicing and open refining to smooth, adopt two two or five vulcanizing agents at 175 ℃, compressing tablet 8 minutes, carries out Mechanics Performance Testing to rubber, and test result is in Table 1.
Embodiment 3
The preparation method of type melting silicone rubber: methyl vinyl silicon kautschuk total amount is a 380kg, therein ethylene base content is to be respectively 0.08%, 0.22%, 3%, 5% methyl vinyl silicon kautschuk respectively to account for 60%, 20%, 10%, 10% of rubber total amount; Silicone oil auxiliary agent total amount is 18kg, and wherein dimethyldimethoxysil,ne, vinyl hydroxy silicone oil, high containing hydrogen silicone oil respectively account for 80%, 15%, 5% of silicone oil auxiliary agent total amount; Selecting specific area is 300m
2the white carbon black of/g is 125kg; Adopt kneader to mediate evenly above-mentioned raw materials, then the sizing material after mediating is put at room temperature health 8 hours; Again that the sizing material stirring after health is agglomerating, pass into the steam that pressure is 0.6MPa, make sizing material be warming up to 125 ℃, temperature-rise period is controlled at 2 hours; After sizing material heats up, start to vacuumize, vacuum degree control is at-0.06MPa, and sizing material temperature is controlled at 130 ℃, and the pumpdown time is controlled at 2.5 hours, and the sizing material that will obtain obtains product after filtering.
Product is carried out to stripping and slicing and open refining to smooth, adopt two two or five vulcanizing agents at 175 ℃, compressing tablet 8 minutes, carries out Mechanics Performance Testing to rubber, and test result is in Table 1.
Embodiment 4
The preparation method of type melting silicone rubber: methyl vinyl silicon kautschuk total amount is a 340kg, therein ethylene base content is to be respectively 0.04%, 2%, 10% methyl vinyl silicon kautschuk respectively to account for 80%, 10%, 10% of rubber total amount; Silicone oil auxiliary agent total amount is 14kg, wherein dimethyldimethoxysil,ne, vinyl hydroxy silicone oil, silicon oil of low hydrogen content, high containing hydrogen silicone oil, respectively account for 70%, 20%, 5%, 5% of silicone oil auxiliary agent total amount; Selecting specific area is 200m
2the white carbon black of/g is 110kg; Adopt kneader to mediate evenly above-mentioned raw materials, then the sizing material after mediating is put at room temperature health 4 hours; Again that the sizing material stirring after health is agglomerating, pass into the steam that pressure is 0.5MPa, make sizing material be warming up to 120 ℃, temperature-rise period is controlled at 1.5 hours; After sizing material heats up, start to vacuumize, vacuum degree control is at-0.05MPa, and sizing material temperature is controlled at 140 ℃, and the pumpdown time is controlled at 2 hours, and the sizing material that will obtain obtains product after filtering.
Product is carried out to stripping and slicing and open refining to smooth, adopt two two or five vulcanizing agents at 175 ℃, compressing tablet 8 minutes, carries out Mechanics Performance Testing to rubber, and test result is in Table 1.
Embodiment 5
The preparation method of type melting silicone rubber: methyl vinyl silicon kautschuk total amount is a 360kg, therein ethylene base content is to be respectively 0.08%, 0.3%, 2%, 3% methyl vinyl silicon kautschuk respectively to account for 20%, 65%, 10%, 5% of rubber total amount; Silicone oil auxiliary agent total amount is 16kg, wherein hydroxy silicon oil, dimethyldimethoxysil,ne, dimethyldiethoxysilane, vinyl hydroxy silicone oil, silicon oil of low hydrogen content, high containing hydrogen silicone oil, respectively account for 20%, 25%, 40%, 5%, 5%, 5% of silicone oil auxiliary agent total amount; Selecting specific area is 300m
2the white carbon black of/g is 120kg; Adopt kneader to mediate evenly above-mentioned raw materials, then the sizing material after mediating is put at room temperature health 3 hours; Again that the sizing material stirring after health is agglomerating, pass into the steam that pressure is 0.7MPa, make sizing material be warming up to 125 ℃, temperature-rise period is controlled at 2 hours; After sizing material heats up, start to vacuumize, vacuum degree control is at-0.08MPa, and sizing material temperature is controlled at 170 ℃, and the pumpdown time is controlled at 3 hours, and the sizing material that will obtain obtains product after filtering.
Product is carried out to stripping and slicing and open refining to smooth, adopt two two or five vulcanizing agents at 175 ℃, compressing tablet 8 minutes, carries out Mechanics Performance Testing to rubber, and test result is in Table 1.
The rubber that following table makes for each embodiment, according to standard GB/T/T531.1-2008, GB/T528-2009, the mechanical property of GB/T529-2008 test.
Table 1
The rubber that existing electric wire annex adopts, tensile strength at yield is about 8KN/M, elongation is generally in 800% left and right, tear strength is generally not more than 30KN/M, and thermal ageing tension set is generally greater than 15%, the product that the rubber production of being prepared by the technical program goes out, by table 1 test result, can draw and all be improved significantly aspect the parameters such as tensile strength at yield, tear strength, elongation, thermal ageing tension set parameter is also in lower scope, and comprehensive mechanical property is improved.
Claims (2)
1. a preparation method for high-performance molded type melting silicone rubber, is characterized in that comprising the following steps:
(1) raw material of the following stated mass parts is mediated evenly:
Methyl vinyl silicon kautschuk total amount is 320～380 parts, and described methyl vinyl silicon kautschuk adopts the different A group rubber of following contents of ethylene and B group rubber to form:
A organizes rubber: contents of ethylene is 0.04%, 0.08%, 0.16%, 0.22%, and in 0.30% methyl vinyl silicon kautschuk any two kinds account for 80%～99% of rubber total amount,
B organizes rubber: contents of ethylene is any one or two kinds in 2%, 3%, 5%, 10% methyl vinyl silicon kautschuk, accounts for 1%～20% of rubber total amount;
Silicone oil auxiliary agent total amount is 11～18 parts, and described silicone oil auxiliary agent is mixed by following C group silicone oil and D group silicone oil:
C organizes silicone oil: a kind of or any several combination in hydroxy silicon oil, dimethyldimethoxysil,ne, dimethyldiethoxysilane, vinyl hydroxy silicone oil, and every kind of combination must contain first three plants at least one in described silicone oil, C group silicone oil accounts for 80%～95% of silicone oil auxiliary agent total amount;
D organizes silicone oil: silicon oil of low hydrogen content, high containing hydrogen silicone oil one or both, D group silicone oil accounts for 5%～20% of silicone oil auxiliary agent total amount;
White carbon black is 100～125 parts, and specific area is 200m
2/ g～400m
2/ g;
(2) sizing material obtaining in step (1) is placed at room temperature health 1～12 hour;
(3) after the stirring of the sizing material after step (2) health is agglomerating, start logical steam, make sizing material be warming up to 100 ℃～130 ℃, Steam pressure control is between 0.2MPa～0.8MPa, and temperature-rise period is controlled at 1～2 hour;
(4) sizing material, after step (3) temperature-rise period completes, starts to vacuumize, and vacuum degree control is at-0.02MPa～-0.08MPa, and sizing material temperature is controlled at 120 ℃～180 ℃, and the pumpdown time is controlled at 1～3 hour, and the sizing material obtaining is filtered and obtain product.
2. the preparation method of a kind of high-performance molded type melting silicone rubber as claimed in claim 1, is characterized in that also adding the inner pattern releasing agent applicable of 0.05～2.6 part in the raw material of step (1).
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881390A (en) * | 2014-02-28 | 2014-06-25 | 浙江炬泰新材料科技有限公司 | Ceramic silicon rubber and preparation and test method |
| CN103897403A (en) * | 2014-03-18 | 2014-07-02 | 浙江炬泰新材料科技有限公司 | Liquid silicone rubber of cold shrink power cable accessories as well as preparation method and test method thereof |
| CN103992651A (en) * | 2014-04-28 | 2014-08-20 | 浙江炬泰新材料科技有限公司 | Low-smoke halogen-free flame-retardant ceramic oxygen-barrier material for flame-resistant cable, and preparation and testing methods thereof |
| CN104260217A (en) * | 2014-07-30 | 2015-01-07 | 珠海福尼亚医疗设备有限公司 | Preparation method of liquid storage bag of trace infusion machine |
| CN107868472A (en) * | 2017-12-01 | 2018-04-03 | 迈高精细高新材料（深圳）有限公司 | A kind of silicon rubber and preparation method thereof |
| CN109701087A (en) * | 2018-12-20 | 2019-05-03 | 新安天玉有机硅有限公司 | A kind of silicon rubber rubber master batch, silicon rubber and preparation method thereof |
| CN111019352A (en) * | 2019-11-26 | 2020-04-17 | 东莞市朗晟材料科技有限公司 | Silica gel for electric wire without sticking to conductor, preparation method and use method |
| CN113088090A (en) * | 2021-03-08 | 2021-07-09 | 浙江恒业成有机硅有限公司 | High-resilience low-pressure-change silicone rubber material and preparation method thereof |
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| CN101514260A (en) * | 2009-03-13 | 2009-08-26 | 东莞市贝特利新材料有限公司 | Silastic composition and preparation method thereof |
| CN102061096A (en) * | 2010-11-18 | 2011-05-18 | 东莞市耀盛硅材料科技有限公司 | Silicon rubber and preparation method thereof |
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| CN101514260A (en) * | 2009-03-13 | 2009-08-26 | 东莞市贝特利新材料有限公司 | Silastic composition and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881390A (en) * | 2014-02-28 | 2014-06-25 | 浙江炬泰新材料科技有限公司 | Ceramic silicon rubber and preparation and test method |
| CN103897403A (en) * | 2014-03-18 | 2014-07-02 | 浙江炬泰新材料科技有限公司 | Liquid silicone rubber of cold shrink power cable accessories as well as preparation method and test method thereof |
| CN103992651A (en) * | 2014-04-28 | 2014-08-20 | 浙江炬泰新材料科技有限公司 | Low-smoke halogen-free flame-retardant ceramic oxygen-barrier material for flame-resistant cable, and preparation and testing methods thereof |
| CN104260217A (en) * | 2014-07-30 | 2015-01-07 | 珠海福尼亚医疗设备有限公司 | Preparation method of liquid storage bag of trace infusion machine |
| CN104260217B (en) * | 2014-07-30 | 2017-02-01 | 珠海福尼亚医疗设备有限公司 | Preparation method of liquid storage bag of trace infusion machine |
| CN107868472A (en) * | 2017-12-01 | 2018-04-03 | 迈高精细高新材料（深圳）有限公司 | A kind of silicon rubber and preparation method thereof |
| CN109701087A (en) * | 2018-12-20 | 2019-05-03 | 新安天玉有机硅有限公司 | A kind of silicon rubber rubber master batch, silicon rubber and preparation method thereof |
| CN109701087B (en) * | 2018-12-20 | 2021-07-23 | 新安天玉有机硅有限公司 | Silicone rubber master batch, silicone rubber and preparation method thereof |
| CN111019352A (en) * | 2019-11-26 | 2020-04-17 | 东莞市朗晟材料科技有限公司 | Silica gel for electric wire without sticking to conductor, preparation method and use method |
| CN113088090A (en) * | 2021-03-08 | 2021-07-09 | 浙江恒业成有机硅有限公司 | High-resilience low-pressure-change silicone rubber material and preparation method thereof |
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Application publication date: 20140129 |