CN103834173B - Silicon rubber and its preparation method - Google Patents
Silicon rubber and its preparation method Download PDFInfo
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- CN103834173B CN103834173B CN201310754182.7A CN201310754182A CN103834173B CN 103834173 B CN103834173 B CN 103834173B CN 201310754182 A CN201310754182 A CN 201310754182A CN 103834173 B CN103834173 B CN 103834173B
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Abstract
The present invention discloses a kind of silicon rubber and its preparation method, and this silicon rubber contains: the methyl vinyl silicone rubber of 100 weight parts; The white carbon black of 30��40 weight parts; The dimethyldiethoxysilane of 3��6 weight parts; The calcium stearate of 0.10��0.15 weight part; The silica powder of 20��30 weight parts; The calcium carbonate of 6��10 weight parts; The cerium oxide of 1��3 weight part; The isocaprylic acid iron organic solution of 0.1��0.7 weight part; The Vinyl MQ silicon resin of 2��5 weight parts; And 1.5 two (t-butylperoxy) hexanes of 2,5-dimethyl-2,5-of weight part. Silicon rubber according to embodiments of the present invention has high rebound resilience and lower compression set performance simultaneously.
Description
Technical field
The present invention relates to organic synthesis field, specifically, the present invention relates to a kind of silicon rubber and its preparation method.
Background technology
Owing to high-temperature silicon disulfide rubber goods have excellent over-all properties, at aviation, electronics, electrically, the industry such as chemical industry, instrument, automobile and health care, daily life every field obtain a wide range of applications. Along with the development of science and technology, compression set and rebound performance to silicon rubber it is also proposed higher requirement, in prior art, silicon rubber generally exists that compression set is relatively big, rebound degree is lower or both can not take into account, can not meet the particular requirement of some product on market, automobile shafts seal as high-end in some, pad, sealing sundries etc. Therefore, reducing the compression set of silicon rubber and improve its rebound performance, the Application Areas widening silicon rubber is the problem of silicon rubber technical field active research.
Summary of the invention
The present invention is intended to one of solve the problems of the technologies described above at least to a certain extent. For this reason, it is an object of the present invention to propose a kind of silicon rubber and its preparation method, this silicon rubber has higher rebound performance and low tension set performance simultaneously.
In one of the embodiment of the present invention, the present invention proposes a kind of silicon rubber, this silicon rubber contains: the methyl vinyl silicone rubber of 100 weight parts; The white carbon black of 30��40 weight parts; The dimethyldiethoxysilane of 3��6 weight parts; The calcium stearate of 0.10��0.15 weight part; The silica powder of 20��30 weight parts; The calcium carbonate of 6��10 weight parts; The cerium oxide of 1��3 weight part; The isocaprylic acid iron organic solution of 0.1��0.7 weight part; The Vinyl MQ silicon resin of 2��5 weight parts; And 1.5 two (t-butylperoxy) hexanes of 2,5-dimethyl-2,5-of weight part. Thus so that silicon rubber has higher rebound performance and low tension set performance simultaneously, it is possible to meet the particular requirement of some product on market.
In addition, silicon rubber according to the above embodiment of the present invention can also have following additional technology feature:
In some embodiments of the invention, the molecular-weight average of described methyl vinyl silicone rubber is 60��650,000, and the contents of ethylene of described methyl vinyl silicone rubber is 0.20��0.25 mole of %. Thus, it is possible to improve the rebound resilience of silicon rubber further and reduce tension set performance.
In some embodiments of the invention, described white carbon black is gas-phase silica or precipitated silica. Thus, it is possible to improve the rebound resilience of silicon rubber further and reduce tension set performance.
In some embodiments of the invention, in described silica powder, silicon-dioxide particle diameter D50 is 2.5 microns. Thus, it is possible to improve the rebound resilience of silicon rubber further and reduce tension set performance. Thus, it is possible to improve the rebound resilience of silicon rubber further and reduce tension set performance.
In some embodiments of the invention, described isocaprylic acid iron organic solution contains 10��15 quality % octanes, 10��15 quality % nonanes, 70��80 quality % heptane and 10 quality % isocaprylic acid iron. Thus, it is possible to improve the rebound resilience of silicon rubber further and reduce tension set performance.
In some embodiments of the invention, described Vinyl MQ silicon resin is prepared by tetraethyl silicate, hexamethyldisiloxane and tetramethyl divinyl disiloxane. Thus, it is possible to improve the rebound resilience of silicon rubber further and reduce tension set performance.
In some embodiments of the invention, the M/Q value of described Vinyl MQ silicon resin is 0.9, and contents of ethylene is 2.5 quality %. Thus, it is possible to improve the rebound resilience of silicon rubber further and reduce tension set performance.
In another aspect of the present invention, the present invention proposes the preparation method of silicon rubber, comprise: methyl vinyl silicone rubber, calcium stearate, white carbon black, dimethyldiethoxysilane, calcium carbonate, cerium oxide, isocaprylic acid iron organic solution, Vinyl MQ silicon resin and silica powder are mixed, to obtain silicone rubber compounds; By described silicone rubber compounds and 2,5-dimethyl-2, two (t-butylperoxy) hexane of 5-mixes, to obtain described silicon rubber, wherein, described methyl vinyl silicone rubber, described calcium stearate, described white carbon black, described dimethyldiethoxysilane, described calcium carbonate, described cerium oxide, described isocaprylic acid iron organic solution, described Vinyl MQ silicon resin, described silica powder and described 2, the consumption of two (t-butylperoxy) hexane of 5-dimethyl-2,5-is: the methyl vinyl silicone rubber of 100 weight parts; The white carbon black of 30��40 weight parts; The dimethyldiethoxysilane of 3��6 weight parts; The calcium stearate of 0.10��0.15 weight part; The silica powder of 20��30 weight parts; The calcium carbonate of 6��10 weight parts; The cerium oxide of 1��3 weight part; The isocaprylic acid iron organic solution of 0.1��0.7 weight part; The Vinyl MQ silicon resin of 2��5 weight parts; And 1.5 two (t-butylperoxy) hexanes of 2,5-dimethyl-2,5-of weight part. The preparation method of silicon rubber according to embodiments of the present invention can effectively prepare the silicon rubber with high resilience and low compression set performance.
In addition, the preparation method of silicon rubber according to the above embodiment of the present invention can also have following additional technology feature:
In some embodiments of the invention, the preparation method of described silicon rubber comprises: described methyl vinyl silicone rubber, described calcium stearate, described white carbon black, described dimethyldiethoxysilane are added in kneader by (1), to obtain molding materials; (2) described molding materials is heated to 150��160 degrees Celsius, vacuumizes, and be incubated 2��3 hours; (3) by described molding materials decrease in temperature to 80 degree Celsius; (4) in described kneader, described calcium carbonate, described cerium oxide, described isocaprylic acid iron organic solution, Vinyl MQ silicon resin and described silica powder is added, to obtain silicone rubber compounds; And (5) are by described silicone rubber compounds and described 2,5-dimethyl-2, two (t-butylperoxy) hexane of 5-add opening rubber mixing machine mixing evenly after, putting in vulcanizing press in temperature is 170 degrees Celsius of sulfurations 5��15 minutes, to obtain described silicon rubber. Thus, it is possible to effectively preparation has high resilience and the silicon rubber of low compression set performance simultaneously.
The additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by the practice of the present invention.
Embodiment
Embodiments of the invention are described below in detail. Embodiment described below is exemplary, it is intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
Along with the development of science and technology, compression set and rebound performance to silicon rubber are had higher requirement, but silicon rubber of the prior art generally exists, and compression set is relatively big, rebound degree is lower or both can not take into account, therefore the particular requirement of some product on market cannot be met, automobile shafts seal as high-end in some, pad, sealing member etc. The present inventor is by exploring synthesis silicon rubber technology, it is intended to solve defect of the prior art, obtains having the silicon rubber of high resilience energy and low compression set performance simultaneously.
For this reason, in one aspect of the invention, the present invention proposes a kind of silicon rubber, according to embodiments of the invention, this silicon rubber contains: the methyl vinyl silicone rubber of 100 weight parts; The white carbon black of 30��40 weight parts; The dimethyldiethoxysilane of 3��6 weight parts; The calcium stearate of 0.10��0.15 weight part; The silica powder of 20��30 weight parts; The calcium carbonate of 6��10 weight parts; The cerium oxide of 1��3 weight part; The isocaprylic acid iron organic solution of 0.1��0.7 weight part; The Vinyl MQ silicon resin of 2��5 weight parts; And 1.5 two (t-butylperoxy) hexanes of 2,5-dimethyl-2,5-of weight part.
Silicon rubber according to embodiments of the present invention is taking methyl vinyl silicone rubber (rubber) as body material, white carbon black, silica powder, calcium carbonate and cerium oxide are filler, isocaprylic acid iron organic solution is for reducing compression set auxiliary agent, dimethyldiethoxysilane is constitution controller, 2, 5-dimethyl-2, two (t-butylperoxy) hexane of 5-is vulcanizing agent, Vinyl MQ silicon resin is for improving rebound resilience auxiliary agent, calcium stearate is the compression set that the silicon rubber that releasing agent obtains reduces silicon rubber by adding isocaprylic acid iron organic solution, the rebound performance of silicon rubber is improved by adding Vinyl MQ silicon resin, therefore make gained silicon rubber have high resilience energy and low compression set performance simultaneously.
According to embodiments of the invention, the molecular-weight average of methyl vinyl silicone rubber is also not particularly limited, and according to a particular embodiment of the invention, the molecular-weight average of methyl vinyl silicone rubber can be 60��650,000. According to embodiments of the invention, the contents of ethylene of silicon rubber in methyl ethylene is also not particularly limited, and according to a particular embodiment of the invention, the contents of ethylene of methyl vinyl silicone rubber can be 0.20��0.25 mole of %. Contriver finds, the rebound performance of silicon rubber generally increases along with the increase of contents of ethylene, but contents of ethylene is too high, and silicon rubber is easily brittle, causes mechanical property to be deteriorated.
According to embodiments of the invention, the particular type of white carbon black is also not particularly limited, and according to a particular embodiment of the invention, white carbon black can be gas-phase silica or precipitated silica. Thus, the gas-phase silica that employing specific surface area is big or precipitated silica are as weighting agent, free hydroxyl and the silicon rubber molecule on white carbon black surface define physics or Chemical bond, silicon rubber molecular adsorption layer is defined on white carbon black surface, form the three-dimensional net structure that white carbon black is connected with silicon rubber molecule, effectively limit the deformation of molecular chain, thus significantly improve silicon rubber rebound resilience.
According to embodiments of the invention, silicon-dioxide particle diameter in silica powder is also not particularly limited, and according to a particular embodiment of the invention, in silica powder, silicon-dioxide particle diameter D50 is 2.5 microns. It should be explained that the distribution of the cumulative particle sizes of D50 representative sample reaches the particle diameter corresponding to 50%. Contriver finds, the rebound performance of silicon rubber generally increases along with the increase of particle diameter, and compression set rate reduces along with the increase of particle diameter, but particle diameter is too high, the poor mechanical property of silicon rubber.
According to embodiments of the invention, the concrete cost of isocaprylic acid iron organic solution and ratio are also not particularly limited, according to embodiments of the invention, isocaprylic acid iron organic solution can contain 10��15 quality % octanes, 10��15 quality % nonanes, 70��80 quality % heptane and 10 quality % isocaprylic acid iron.
According to embodiments of the invention, the source of Vinyl MQ silicon resin is also not particularly limited, and according to a particular embodiment of the invention, Vinyl MQ silicon resin can for be prepared by tetraethyl silicate, hexamethyldisiloxane and tetramethyl divinyl disiloxane. According to embodiments of the invention, the M/Q value of vinyl silicon MQ resin is also not particularly limited, according to embodiments of the invention, the M/Q value of vinyl silicon MQ resin can be 0.9, it should be explained that M represents the silica unit of single functionality, Q represents the silica unit of four functionality, and M/Q value is the silica unit of single functionality and the silica element number ratio of four functionality. Contriver finds, when the M/Q value of Vinyl MQ silicon resin is too low, vinyl polysiloxane is Silica hydrogel, poor with the consistency of silicon rubber; When M/Q value is too high, the rebound performance of silicon rubber is improved not obvious. According to embodiments of the invention, the contents of ethylene of Vinyl MQ silicon resin is also not particularly limited, and according to a particular embodiment of the invention, contents of ethylene can be 2.5 quality %.
As mentioned above, it is necessary, silicon rubber according to embodiments of the present invention can have is selected from following advantage one of at least:
Silicon rubber according to embodiments of the present invention has low compression deformation rate, and compression set rate is less than 10%.
The rebound degree that silicon rubber tool according to embodiments of the present invention is higher, rebound degree is up to more than 65%.
Silicone rubber material according to embodiments of the present invention does not contain the chemical substance of contaminate environment.
In another aspect of the present invention, the present invention proposes the preparation method of a kind of silicon rubber, according to embodiments of the invention, the method comprises: methyl vinyl silicone rubber, calcium stearate, white carbon black, dimethyldiethoxysilane, calcium carbonate, cerium oxide, isocaprylic acid iron organic solution, Vinyl MQ silicon resin and silica powder are mixed, to obtain silicone rubber compounds; By silicone rubber compounds and 2,5-dimethyl-2, two (t-butylperoxy) hexane of 5-mixes, to obtain silicon rubber, wherein, the consumption of two (t-butylperoxy) hexane of methyl vinyl silicone rubber, calcium stearate, white carbon black, dimethyldiethoxysilane, calcium carbonate, cerium oxide, isocaprylic acid iron organic solution, Vinyl MQ silicon resin, silica powder and 2,5-dimethyl-2,5-is: the methyl vinyl silicone rubber of 100 weight parts; The white carbon black of 30��40 weight parts; The dimethyldiethoxysilane of 3��6 weight parts; The calcium stearate of 0.10��0.15 weight part; The silica powder of 20��30 weight parts; The calcium carbonate of 6��10 weight parts; The cerium oxide of 1��3 weight part; The isocaprylic acid iron organic solution of 0.1��0.7 weight part; The Vinyl MQ silicon resin of 2��5 weight parts; And 1.5 two (t-butylperoxy) hexanes of 2,5-dimethyl-2,5-of weight part.
Specifically, methyl vinyl silicon kautschuk and calcium stearate are mediated 3��5 minutes in kneader, then divide 4 times by white carbon black and dimethyldiethoxysilane to add in kneader, stir 30 minute after adding every time; After white carbon black and diethoxy silane and gained mixture mixing moulding, gained forming mixture is warming up to 150��160 degrees Celsius, and vacuumizes, be incubated 2��3 hours; Temperature of charge after being heated up by gained is down to 80 degrees Celsius, adds calcium carbonate, cerium oxide, isocaprylic acid iron organic solution and Vinyl MQ silicon resin successively and mediates in internal rubber mixer 3��5 minutes; Being divided by silica powder four times adds in kneader, adds stirring 20��30 minutes, and control temperature is below 100 degrees Celsius every time; After silica powder and the stirring of gained mixture are shaping, continue stirring and get final product discharging in 30 minutes, then filter, prepare silicone rubber compounds; By two to gained silicone rubber compounds and 2,5-dimethyl-2,5-(t-butylperoxy) hexane in opening rubber mixing machine after Homogeneous phase mixing, putting in vulcanizing press in temperature is 170 degrees Celsius of sulfurations 5��15 minutes, can obtain silicon rubber.
Below with reference to specific embodiment, present invention is described, it is necessary to explanation, and these embodiments are only descriptive, and do not limit the present invention in any way.
Embodiment 1
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 1.0g weight part, the Vinyl MQ silicon resin of 20g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method:
Methyl vinyl silicon kautschuk and calcium stearate are mediated 3��5 minutes in kneader, then divides 4 times by white carbon black and dimethyldiethoxysilane to add in kneader, stir 30 minute after adding every time; After white carbon black and diethoxy silane and gained mixture mixing moulding, gained forming mixture is warming up to 150��160 degrees Celsius, and vacuumizes, be incubated 2��3 hours; Temperature of charge after being heated up by gained is down to 80 degrees Celsius, adds calcium carbonate, cerium oxide, isocaprylic acid iron organic solution and Vinyl MQ silicon resin successively and mediates in internal rubber mixer 3��5 minutes; Being divided by silica powder four times adds in kneader, adds stirring 20��30 minutes, and control temperature is below 100 degrees Celsius every time; After silica powder and the stirring of gained mixture are shaping, continue stirring and get final product discharging in 30 minutes, then filter, prepare silicone rubber compounds; By two to gained silicone rubber compounds and 2,5-dimethyl-2,5-(t-butylperoxy) hexane in opening rubber mixing machine after Homogeneous phase mixing, putting in vulcanizing press in temperature is 170 degrees Celsius of sulfurations 5��15 minutes, can obtain silicon rubber, can obtain silicon rubber.
Embodiment 2
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 3.0g weight part, the Vinyl MQ silicon resin of 20g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 3
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 5.0g weight part, the Vinyl MQ silicon resin of 20g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 4
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 5.0g weight part, the Vinyl MQ silicon resin of 20g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 5
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 7.0g weight part, the Vinyl MQ silicon resin of 20g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 6
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 3.0g weight part, the Vinyl MQ silicon resin of 40g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 7
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 3.0g weight part, the Vinyl MQ silicon resin of 50g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Comparative example 1
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the Vinyl MQ silicon resin of 20g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method:
Methyl vinyl silicon kautschuk and calcium stearate are mediated 3��5 minutes in kneader, then divides 4 times by white carbon black and dimethyldiethoxysilane to add in kneader, stir 30 minute after adding every time; After white carbon black and diethoxy silane and gained mixture mixing moulding, gained forming mixture is warming up to 150��160 degrees Celsius, and vacuumizes, be incubated 2��3 hours; Temperature of charge after being heated up by gained is down to 80 degrees Celsius, adds calcium carbonate, cerium oxide and Vinyl MQ silicon resin successively and mediates in internal rubber mixer 3��5 minutes; Being divided by silica powder four times adds in kneader, adds stirring 20��30 minutes, and control temperature is below 100 degrees Celsius every time; After silica powder and the stirring of gained mixture are shaping, continue stirring and get final product discharging in 30 minutes, then filter, prepare silicone rubber compounds; By two to gained silicone rubber compounds and 2,5-dimethyl-2,5-(t-butylperoxy) hexane in opening rubber mixing machine after Homogeneous phase mixing, putting in vulcanizing press in temperature is 170 degrees Celsius of sulfurations 5��15 minutes, can obtain silicon rubber.
Comparative example 2
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the Vinyl MQ silicon resin of 50g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with comparative example 1.
Comparative example 3
Composition of raw materials:
The cerium oxide of the silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, 20g, the isocaprylic acid iron organic solution of 1.0g weight part, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method:
Methyl vinyl silicon kautschuk and calcium stearate are mediated 3��5 minutes in kneader, then divides 4 times by white carbon black and dimethyldiethoxysilane to add in kneader, stir 30 minute after adding every time; After white carbon black and diethoxy silane and gained mixture mixing moulding, gained forming mixture is warming up to 150��160 degrees Celsius, and vacuumizes, be incubated 2��3 hours; Temperature of charge after being heated up by gained is down to 80 degrees Celsius, adds calcium carbonate, cerium oxide and isocaprylic acid iron organic solution successively and mediates in internal rubber mixer 3��5 minutes; Being divided by silica powder four times adds in kneader, adds stirring 20��30 minutes, and control temperature is below 100 degrees Celsius every time; After silica powder and the stirring of gained mixture are shaping, continue stirring and get final product discharging in 30 minutes, then filter, prepare silicone rubber compounds; By two to gained silicone rubber compounds and 2,5-dimethyl-2,5-(t-butylperoxy) hexane in opening rubber mixing machine after Homogeneous phase mixing, putting in vulcanizing press in temperature is 170 degrees Celsius of sulfurations 5��15 minutes, can obtain silicon rubber, can obtain silicon rubber.
Comparative example 4
Composition of raw materials:
The cerium oxide of the silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, 20g, the isocaprylic acid iron organic solution of 7.0g weight part, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with comparative example 3.
Comparative example 5
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 4.0g weight part, the Vinyl MQ silicon resin of 70g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Comparative example 6
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 10g weight part, the Vinyl MQ silicon resin of 40g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Comparative example 7
Composition of raw materials:
The silica powder of the dimethyldiethoxysilane of the methyl vinyl silicone rubber of 1000g, the white carbon black of 350g, 50g, the calcium stearate of 1.4g, 250g, the calcium carbonate of 80g, the cerium oxide of 20g, the isocaprylic acid iron organic solution of 10g weight part, the Vinyl MQ silicon resin of 70g, the 2 of 15g, 5-dimethyl-2,5-two (t-butylperoxy).
Preparation method: with embodiment 1.
Evaluate:
1, respectively embodiment 1-7 gained silicon rubber mechanical property is evaluated.
2, evaluation index and testing method:
The test of hardness: GB/T531.1-2008
The test of tensile strength: GB/T528-1998
The test of elongation: GB/T528-1998
The test of compression set rate: GB/T7759-1996
Elastic test: GB/T1681-2009
Test result is as shown in table 1:
Table 1 silicon rubber mechanical property contrasts
| Hardness (HA) | Tensile strength (MPa) | Elongation (%) | Compression set rate (%) | Rebound degree (%) | |
| Embodiment 1 | 61 | 7.24 | 213 | 9 | 65 |
| Embodiment 2 | 62 | 7.12 | 212 | 8 | 66 |
| Embodiment 3 | 63 | 6.85 | 186 | 8 | 65 |
| Embodiment 4 | 65 | 6.34 | 168 | 9 | 65 |
| Embodiment 5 | 62 | 7.01 | 203 | 8 | 67 |
| Embodiment 6 | 63 | 7.85 | 155 | 9 | 65 |
| Embodiment 7 | 63 | 7.63 | 110 | 11 | 65 |
| Comparative example 1 | 60 | 7.15 | 220 | 16 | 65 |
| Comparative example 2 | 60 | 7.35 | 150 | 18 | 65 |
| Comparative example 3 | 60 | 7.05 | 235 | 9 | 60 |
| Comparative example 4 | 64 | 6.55 | 225 | 9 | 59 |
| Comparative example 5 | 64 | 7.66 | 115 | 16 | 63 |
| Comparative example 6 | 67 | 7.54 | 146 | 11 | 62 |
| Comparative example 7 | 68 | 7.33 | 104 | 16 | 62 |
Conclusion: by the above results, silicon rubber prepared by the embodiment of the present invention has high rebound resilience and lower compression set rate simultaneously, and silicon rubber prepared by embodiment 5 has best over-all properties, and compression set rate is 8%, and rebound degree is 67%. Documents 1-2, compared with embodiment, does not use isocaprylic acid iron organic solution; Comparative example 3-4 does not use Vinyl MQ silicon resin; Although comparative example 5-7 employs isocaprylic acid iron organic solution and Vinyl MQ silicon resin, but in the two add-on one of at least outside protection domain of the present invention.
Data from table 1 show, in comparative example 1-2, the silicon rubber of preparation has good rebound resilience, but compression set rate is bigger; In comparative example 3-4, the silicon rubber of preparation has lower compression set rate, but rebound resilience is poor; Silicon rubber prepared by comparative example 5-7 also can not have good rebound resilience and lower compression set rate simultaneously.
In the description of this specification sheets, at least one embodiment that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to be contained in the present invention in conjunction with concrete feature, structure, material or feature that this embodiment or example describe or example. In this manual, the schematic representation of above-mentioned term is not necessarily referred to identical embodiment or example. And, the concrete feature of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although above it has been shown and described that embodiments of the invention, it is understandable that, above-described embodiment is exemplary, can not being interpreted as limitation of the present invention, above-described embodiment can be changed when not departing from principle and the objective of the present invention, revises, replace and modification by the those of ordinary skill of this area within the scope of the invention.
Claims (9)
1. a silicon rubber, it is characterised in that, contain:
The methyl vinyl silicone rubber of 100 weight parts;
The white carbon black of 30��40 weight parts;
The dimethyldiethoxysilane of 3��6 weight parts;
The calcium stearate of 0.10��0.15 weight part;
The silica powder of 20��30 weight parts;
The calcium carbonate of 6��10 weight parts;
The cerium oxide of 1��3 weight part;
The isocaprylic acid iron organic solution of 0.1��0.7 weight part;
The Vinyl MQ silicon resin of 2��5 weight parts; And
Two (t-butylperoxy) hexane of the 2,5-dimethyl-2,5-of 1.5 weight parts,
Wherein,
The contents of ethylene of described methyl vinyl silicone rubber is 0.20��0.25 mole of %,
The M/Q value of described Vinyl MQ silicon resin is 0.9.
2. silicon rubber according to claim 1, it is characterised in that, the molecular-weight average of described methyl vinyl silicone rubber is 60��650,000.
3. silicon rubber according to claim 1, it is characterised in that, described white carbon black is gas-phase silica or precipitated silica.
4. silicon rubber according to claim 1, it is characterised in that, in described silica powder, silicon-dioxide particle diameter D50 is 2.5 microns.
5. silicon rubber according to claim 1, it is characterised in that, described isocaprylic acid iron organic solution contains 10��15 quality % octanes, 10��15 quality % nonanes, 70��80 quality % heptane and 10 quality % isocaprylic acid iron.
6. silicon rubber according to claim 1, it is characterised in that, described Vinyl MQ silicon resin is prepared by tetraethyl silicate, hexamethyldisiloxane and tetramethyl divinyl disiloxane.
7. silicon rubber according to claim 6, it is characterised in that, the contents of ethylene of described Vinyl MQ silicon resin is 2.5 quality %.
8. the preparation method of silicon rubber according to any one of a claim 1-7, it is characterised in that, comprising:
Methyl vinyl silicone rubber, calcium stearate, white carbon black, dimethyldiethoxysilane, calcium carbonate, cerium oxide, isocaprylic acid iron organic solution, Vinyl MQ silicon resin and silica powder are mixed, to obtain silicone rubber compounds;
Two with 2,5-dimethyl-2,5-for described silicone rubber compounds (t-butylperoxy) hexane is mixed, to obtain described silicon rubber,
Wherein, described methyl vinyl silicone rubber, described calcium stearate, described white carbon black, described dimethyldiethoxysilane, described calcium carbonate, described cerium oxide, described isocaprylic acid iron organic solution, described Vinyl MQ silicon resin, described silica powder and described 2, the consumption of two (t-butylperoxy) hexane of 5-dimethyl-2,5-is:
The methyl vinyl silicone rubber of 100 weight parts;
The white carbon black of 30��40 weight parts;
The dimethyldiethoxysilane of 3��6 weight parts;
The calcium stearate of 0.10��0.15 weight part;
The silica powder of 20��30 weight parts;
The calcium carbonate of 6��10 weight parts;
The cerium oxide of 1��3 weight part;
The isocaprylic acid iron organic solution of 0.1��0.7 weight part;
The Vinyl MQ silicon resin of 2��5 weight parts; And
Two (t-butylperoxy) hexane of the 2,5-dimethyl-2,5-of 1.5 weight parts.
9. method according to claim 8, it is characterised in that, comprising:
(1) described methyl vinyl silicone rubber, described calcium stearate, described white carbon black, described dimethyldiethoxysilane are added in kneader, to obtain molding materials;
(2) described molding materials is heated to 150��160 degrees Celsius, vacuumizes, and be incubated 2��3 hours;
(3) by described molding materials decrease in temperature to 80 degree Celsius;
(4) in described kneader, described calcium carbonate, described cerium oxide, described isocaprylic acid iron organic solution, Vinyl MQ silicon resin and described silica powder is added, to obtain silicone rubber compounds; And
(5) by described silicone rubber compounds and described 2,5-dimethyl-2, two (t-butylperoxy) hexane of 5-add opening rubber mixing machine mixing evenly after, putting in vulcanizing press in temperature is 170 degrees Celsius of sulfurations 5��15 minutes, to obtain described silicon rubber.
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| CN107916002A (en) * | 2017-12-01 | 2018-04-17 | 迈高精细高新材料（深圳）有限公司 | A kind of silicon rubber and preparation method thereof |
| CN108948741A (en) * | 2018-08-02 | 2018-12-07 | 广州市瑞合新材料科技有限公司 | Flame-retardant silicone rubber composition and preparation method thereof |
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