CN103834173A - Silicone rubber and preparation method thereof - Google Patents
Silicone rubber and preparation method thereof Download PDFInfo
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- CN103834173A CN103834173A CN201310754182.7A CN201310754182A CN103834173A CN 103834173 A CN103834173 A CN 103834173A CN 201310754182 A CN201310754182 A CN 201310754182A CN 103834173 A CN103834173 A CN 103834173A
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Abstract
The invention discloses a silicone rubber and a preparation method thereof. The silicone rubber contains, by weight, 100 parts of methyl vinyl silicone rubber, 30 to 40 parts of white carbon black, 3 to 6 parts of dimethyldiethoxylsilane, 0.10 to 0.15 part of calcium stearate, 20 to 30 parts of quartz powder, 6 to 10 parts of calcium carbonate, 1 to 3 parts of cerium oxide, 0.1 to 0.7 part of an iron isocaprylate organic solution, 2 to 5 parts of vinyl MQ silicone resin and 1.5 parts of 2,5-dimethyl-2,5-bis(t-butylperoxy)hexane. According to embodiments in the invention, the silicone rubber has high resilience and low compression set performance at the same time.
Description
Technical field
The present invention relates to organic synthesis field, particularly, the present invention relates to a kind of silicon rubber and preparation method thereof.
Background technology
Because high-temperature silicon disulfide rubber goods have excellent over-all properties, in the industry such as aviation, electronics, electric, chemical industry, instrument, automobile and health care, daily life every field, obtain a wide range of applications.Along with scientific and technological development, compression set and rebound performance to silicon rubber are also had higher requirement, in prior art, the compression set of silicon rubber ubiquity is large, 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, reduce the compression set of silicon rubber and improve its rebound performance, the Application Areas of 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, one object of the present invention is to propose a kind of silicon rubber and preparation method thereof, and this silicon rubber has higher rebound performance and low tension set performance simultaneously.
Aspect 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 silicone resin of 2～5 weight parts; And 1.5 weight parts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane.Thus, make silicon rubber there is higher rebound performance and low tension set performance simultaneously, can 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 technical characterictic:
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 % by mole.Thus, can further improve the rebound resilience of silicon rubber and reduce tension set performance.
In some embodiments of the invention, described white carbon black is gas-phase silica or precipitated silica.Thus, can further improve the rebound resilience of silicon rubber 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, can further improve the rebound resilience of silicon rubber and reduce tension set performance.Thus, can further improve the rebound resilience of silicon rubber 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, can further improve the rebound resilience of silicon rubber and reduce tension set performance.
In some embodiments of the invention, described vinyl MQ silicone resin is prepared by tetraethyl silicate, hexamethyldisiloxane and tetramethyl divinyl disiloxane.Thus, can further improve the rebound resilience of silicon rubber and reduce tension set performance.
In some embodiments of the invention, the M/Q value of described vinyl MQ silicone resin is 0.9, and contents of ethylene is 2.5 quality %.Thus, can further improve the rebound resilience of silicon rubber 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 silicone resin and silica powder are mixed, to obtain silicone rubber compounds; By described silicone rubber compounds and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane 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 silicone resin, described silica powder and described 2,5-dimethyl-2, the consumption of 5-bis(t-butylperoxy) hexane 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 silicone resin of 2～5 weight parts; And 1.5 weight parts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane.Can effectively prepare the silicon rubber simultaneously with high resilience and low compression set performance according to the preparation method of the silicon rubber of the embodiment of the present invention.
In addition, the preparation method of silicon rubber according to the above embodiment of the present invention can also have following additional technical characterictic:
In some embodiments of the invention, the preparation method of described silicon rubber comprises: (1) adds described methyl vinyl silicone rubber, described calcium stearate, described white carbon black, described dimethyldiethoxysilane 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) described molding materials temperature is reduced to 80 degrees Celsius; (4) in described kneader, add described calcium carbonate, described cerium oxide, described isocaprylic acid iron organic solution, vinyl MQ silicone resin and described silica powder, to obtain silicone rubber compounds; And (5) are by described silicone rubber compounds and described 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane add opening rubber mixing machine mixing evenly after, putting in vulcanizing press is 170 degrees Celsius of sulfurations 5～15 minutes in temperature, to obtain described silicon rubber.Thus, can effectively prepare the silicon rubber simultaneously with high resilience and low compression set performance.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Embodiment
Describe embodiments of the invention below in detail.Embodiment described below is exemplary, is intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
Along with scientific and technological development, compression set and rebound performance to silicon rubber are had higher requirement, but silicon rubber ubiquity of the prior art compression set is large, rebound degree is lower or both can not take into account, therefore cannot meet the particular requirement of some product on market, automobile shafts seal as high-end in some, pad, sealing member etc.The present inventor, by silastic elastomer technology is explored, is intended to solve defect of the prior art, is had 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 silicone resin of 2～5 weight parts; And 1.5 weight parts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane.
According to the silicon rubber of the embodiment of the present invention 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, 5-bis(t-butylperoxy) hexane is vulcanizing agent, vinyl MQ silicone resin is for improving rebound resilience auxiliary agent, calcium stearate is the silicon rubber that obtains of releasing agent reduces silicon rubber compression set by adding isocaprylic acid iron organic solution, improve the rebound performance of silicon rubber by adding vinyl MQ silicone resin, therefore make gained silicon rubber there is 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 being not particularly limited in methyl ethylene, according to a particular embodiment of the invention, the contents of ethylene of methyl vinyl silicone rubber can be 0.20～0.25 % by mole.Contriver's discovery, the rebound performance of silicon rubber generally increases along with the increase of contents of ethylene, but contents of ethylene is too high, and the easy embrittlement of silicon rubber, causes mechanical property variation.
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 large or precipitated silica are as weighting agent, the free hydroxyl on white carbon black surface and silicon rubber molecule have formed physics or Chemical bond, formed silicon rubber molecular adsorption layer 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, thereby significantly improved silicon rubber rebound resilience.
According to embodiments of the invention, silicon-dioxide particle diameter being not particularly limited in silica powder, according to a particular embodiment of the invention, in silica powder, silicon-dioxide particle diameter D50 is 2.5 microns.The cumulative particle sizes distribution that it should be explained that D50 representative sample reaches 50% corresponding particle diameter.Contriver's discovery, 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 silicone resin is also not particularly limited, and according to a particular embodiment of the invention, vinyl MQ silicone resin can be for to 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's discovery, in the time that the M/Q of vinyl MQ silicone resin value is too low, vinyl polysiloxane is silicon gel, poor with the consistency of silicon rubber; In the time that M/Q value is too high, improve not obvious to the rebound performance of silicon rubber.According to embodiments of the invention, the contents of ethylene of vinyl MQ silicone 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, can have and be selected from following advantage one of at least according to the silicon rubber of the embodiment of the present invention:
Have low compression deformation rate according to the silicon rubber of the embodiment of the present invention, compression set rate is less than 10%.
The rebound degree higher according to the silicon rubber tool of the embodiment of the present invention, rebound degree is up to more than 65%.
According to the chemical substance that does not contain contaminate environment in the silicone rubber material of the embodiment of the present invention.
In another aspect of the present invention, the present invention proposes a kind of preparation method 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 silicone resin and silica powder are mixed, to obtain silicone rubber compounds; By silicone rubber compounds and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane mixes, so that acquisition silicon rubber, wherein, methyl vinyl silicone rubber, calcium stearate, white carbon black, dimethyldiethoxysilane, calcium carbonate, cerium oxide, isocaprylic acid iron organic solution, vinyl MQ silicone resin, silica powder and 2,5-dimethyl-2, the consumption of 5-bis(t-butylperoxy) hexane 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 silicone resin of 2～5 weight parts; And 1.5 weight parts 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane.
Particularly, methyl vinyl silicon kautschuk and calcium stearate are mediated 3～5 minutes in kneader, then white carbon black and dimethyldiethoxysilane are divided 4 times add in kneader, add rear stirring 30 minutes at every turn; 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 gained is heated up is down to 80 degrees Celsius, adds successively calcium carbonate, cerium oxide, isocaprylic acid iron organic solution and vinyl MQ silicone resin in internal rubber mixer, to mediate 3～5 minutes; Silica powder is divided four times and add in kneader, add at every turn and stir 20～30 minutes, and control temperature below 100 degrees Celsius; Stir after moulding until silica powder and gained mixture, continue stirring and within 30 minutes, get final product discharging, then filter, prepare silicone rubber compounds; By gained silicone rubber compounds and 2,5-dimethyl-2, after 5-bis(t-butylperoxy) hexane evenly mixes in opening rubber mixing machine, putting in vulcanizing press is 170 degrees Celsius of sulfurations 5～15 minutes in temperature, can obtain silicon rubber.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiment are only descriptive, and do not limit the present invention in any way.
Embodiment 1
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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, 20g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method:
Methyl vinyl silicon kautschuk and calcium stearate are mediated 3～5 minutes in kneader, then white carbon black and dimethyldiethoxysilane are divided 4 times add in kneader, add rear stirring 30 minutes at every turn; 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 gained is heated up is down to 80 degrees Celsius, adds successively calcium carbonate, cerium oxide, isocaprylic acid iron organic solution and vinyl MQ silicone resin in internal rubber mixer, to mediate 3～5 minutes; Silica powder is divided four times and add in kneader, add at every turn and stir 20～30 minutes, and control temperature below 100 degrees Celsius; Stir after moulding until silica powder and gained mixture, continue stirring and within 30 minutes, get final product discharging, then filter, prepare silicone rubber compounds; By gained silicone rubber compounds and 2,5-dimethyl-2, after 5-bis(t-butylperoxy) hexane evenly mixes in opening rubber mixing machine, putting in vulcanizing press is 170 degrees Celsius of sulfurations 5～15 minutes in temperature, can obtain silicon rubber, can obtain silicon rubber.
Embodiment 2
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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 3.0g weight part, 20g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 3
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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 5.0g weight part, 20g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 4
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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 5.0g weight part, 20g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 5
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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, 20g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 6
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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 3.0g weight part, 40g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Embodiment 7
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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 3.0g weight part, 50g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Comparative example 1
Composition of raw materials:
2 of 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 vinyl MQ silicone resin of 20g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method:
Methyl vinyl silicon kautschuk and calcium stearate are mediated 3～5 minutes in kneader, then white carbon black and dimethyldiethoxysilane are divided 4 times add in kneader, add rear stirring 30 minutes at every turn; 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 gained is heated up is down to 80 degrees Celsius, adds successively calcium carbonate, cerium oxide and vinyl MQ silicone resin in internal rubber mixer, to mediate 3～5 minutes; Silica powder is divided four times and add in kneader, add at every turn and stir 20～30 minutes, and control temperature below 100 degrees Celsius; Stir after moulding until silica powder and gained mixture, continue stirring and within 30 minutes, get final product discharging, then filter, prepare silicone rubber compounds; By gained silicone rubber compounds and 2,5-dimethyl-2, after 5-bis(t-butylperoxy) hexane evenly mixes in opening rubber mixing machine, putting in vulcanizing press is 170 degrees Celsius of sulfurations 5～15 minutes in temperature, can obtain silicon rubber.
Comparative example 2
Composition of raw materials:
2 of 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 vinyl MQ silicone resin of 50g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with comparative example 1.
Comparative example 3
Composition of raw materials:
2 of 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, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method:
Methyl vinyl silicon kautschuk and calcium stearate are mediated 3～5 minutes in kneader, then white carbon black and dimethyldiethoxysilane are divided 4 times add in kneader, add rear stirring 30 minutes at every turn; 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 gained is heated up is down to 80 degrees Celsius, adds successively calcium carbonate, cerium oxide and isocaprylic acid iron organic solution in internal rubber mixer, to mediate 3～5 minutes; Silica powder is divided four times and add in kneader, add at every turn and stir 20～30 minutes, and control temperature below 100 degrees Celsius; Stir after moulding until silica powder and gained mixture, continue stirring and within 30 minutes, get final product discharging, then filter, prepare silicone rubber compounds; By gained silicone rubber compounds and 2,5-dimethyl-2, after 5-bis(t-butylperoxy) hexane evenly mixes in opening rubber mixing machine, putting in vulcanizing press is 170 degrees Celsius of sulfurations 5～15 minutes in temperature, can obtain silicon rubber, can obtain silicon rubber.
Comparative example 4
Composition of raw materials:
2 of 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, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with comparative example 3.
Comparative example 5
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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 4.0g weight part, 70g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Comparative example 6
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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 10g weight part, 40g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Comparative example 7
Composition of raw materials:
2 of the vinyl MQ silicone resin of 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 10g weight part, 70g, 15g, 5-dimethyl-2,5-bis(t-butylperoxy).
Preparation method: with embodiment 1.
Evaluate:
1, respectively embodiment 1-7 gained Mechanical Properties of Silicone Rubber 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:
The contrast of table 1 Mechanical Properties of Silicone Rubber
| ? | 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: known 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, 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 silicone resin; Although comparative example 5-7 has used isocaprylic acid iron organic solution and vinyl MQ silicone resin, in the two add-on one of at least outside protection domain of the present invention.
Data from table 1 show, the silicon rubber of preparing in comparative example 1-2 has good rebound resilience, but compression set rate is larger; The silicon rubber of preparing in comparative example 3-4 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, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, the schematic statement of above-mentioned term is not necessarily referred to identical embodiment or example.And specific features, structure, material or the feature of description can be with suitable mode combination in any one or more embodiment or example.
Although illustrated and described embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention in the situation that not departing from principle of the present invention and aim, amendment, replacement and modification.
Claims (9)
1. a silicon rubber, is characterized in that, 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 silicone resin of 2～5 weight parts; And
2 of 1.5 weight parts, 5-dimethyl-2,5-bis(t-butylperoxy) hexane.
2. silicon rubber according to claim 1, is characterized in that, 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 % by mole.
3. silicon rubber according to claim 1, is characterized in that, described white carbon black is gas-phase silica or precipitated silica.
4. silicon rubber according to claim 1, is characterized in that, in described silica powder, silicon-dioxide particle diameter D50 is 2.5 microns.
5. silicon rubber according to claim 1, is characterized 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, is characterized in that, described vinyl MQ silicone resin is prepared by tetraethyl silicate, hexamethyldisiloxane and tetramethyl divinyl disiloxane.
7. silicon rubber according to claim 6, is characterized in that, the M/Q value of described vinyl MQ silicone resin is 0.9, and contents of ethylene is 2.5 quality %.
8. a preparation method for silicon rubber described in any one in claim 1-7, is characterized in that, comprising:
Methyl vinyl silicone rubber, calcium stearate, white carbon black, dimethyldiethoxysilane, calcium carbonate, cerium oxide, isocaprylic acid iron organic solution, vinyl MQ silicone resin and silica powder are mixed, to obtain silicone rubber compounds;
By described silicone rubber compounds and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane 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 silicone resin, described silica powder and described 2,5-dimethyl-2, the consumption of 5-bis(t-butylperoxy) hexane 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 silicone resin of 2～5 weight parts; And
2 of 1.5 weight parts, 5-dimethyl-2,5-bis(t-butylperoxy) hexane.
9. method according to claim 8, is characterized 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) described molding materials temperature is reduced to 80 degrees Celsius;
(4) in described kneader, add described calcium carbonate, described cerium oxide, described isocaprylic acid iron organic solution, vinyl MQ silicone resin and described silica powder, to obtain silicone rubber compounds; And
(5) by described silicone rubber compounds and described 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane add opening rubber mixing machine mixing evenly after, putting in vulcanizing press is 170 degrees Celsius of sulfurations 5～15 minutes in temperature, to obtain described silicon rubber.
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