CN103232707B - Curable silicone rubber composition and solidifying product thereof and coating and curing method - Google Patents
Curable silicone rubber composition and solidifying product thereof and coating and curing method Download PDFInfo
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Abstract
The object of the present invention is to provide a kind of curable silicone rubber composition, after its solidification, there is high refractive index, good class rubber performance and strength characteristics and almost there is no surface viscosity.And develop a kind of coating agent based on said composition.This kind of curable silicone rubber composition, comprise: component A contains the methyl phenyl silicone of aliphatics unsaturated link(age), the viscosity of its 25 ° of C degree is 2000 ~ 20000mPas, B component is the methyl phenyl silicone that each molecule contains multiple si-h bond, its viscosity of 25 DEG C is 2000 ~ 20000mPas, component C platinum metal catalysts, wherein the quality of B component accounts for the 10%-90% of the total mass of component A and B component.
Description
Technical field
The present invention relates to a kind of curable silicone rubber containing cyclic organohydrogensiloxanes and solidifying product thereof, in particular to a kind of preparation, there is high refractive index, good class rubber performance and strength characteristics, and the curable silicone rubber composition of the extremely low solidifying product of surface viscosity and the solidifying product using said composition to prepare and curing.
Background technology
Constantly perfect along with power type white light LED manufacturing technology, its luminous efficiency, brightness and power all have increased significantly; Meanwhile, also more and more higher to the requirement of packaged material, require that outer envelope material can have higher specific absorption to ultraviolet, to prevent ultraviolet leakage while the high transparent of maintenance visible region.The packaged material of use high refractive index, high UV resistant and heat-proof aging ability, low-stress also can significantly improve optical output power and the work-ing life of illuminating device.Traditional LED encapsulation material based on epoxy resin and urethane can not meet the requirement of power type white light LED, high-powerly at present forms primarily of organosilicon material by high-end LED encapsulation material.
The packaged material of use high refractive index, high UV resistant and heat-proof aging ability, low-stress also can significantly improve optical output power and the work-ing life of illuminating device.The preparation-obtained material of prior art still can not be satisfactory in above characteristic index.
Summary of the invention
The object of the present invention is to provide a kind of curable silicone rubber composition, the product after its solidification has high refractive index, good class rubber performance and strength characteristics and does not almost have surface viscosity.And develop a kind of coating agent based on said composition.
For realizing goal of the invention, the invention provides a kind of curable silicone rubber composition, comprising:
Component A contains the methyl phenyl silicone of aliphatics unsaturated link(age), and the viscosity of its 25 ° of C degree is 2000 ~ 20000mPas,
B component is the methyl phenyl silicone that each molecule contains multiple si-h bond, and its viscosity of 25 DEG C is 2000 ~ 20000mPas,
Component C platinum metal catalysts,
Wherein the quality of B component accounts for the 10%-90% of the total mass of component A and B component.
Preferably, the structure of component A is compound shown in following general formula:
R in formula
1group represents the identical or different monovalence representative examples of saturated aliphatic alkyl that carbonatoms is 1-6, R
2group represents identical or different monovalence unsaturated fatty hydrocarbons base or the monovalence representative examples of saturated aliphatic alkyl that carbonatoms is 1-6, R
3group represents the monovalence representative examples of saturated aliphatic alkyl that phenyl or carbonatoms are 1-6, n and m represents the positive integer of 10-100 separately.
More preferably, n and m gets the numerical value of 20-30 respectively.
R
1group can be selected from following group: methyl, ethyl, n-hexyl;
R
2group can be selected from following group: methyl, ethyl, n-hexyl, vinyl, allyl group;
R
3group can be selected from following group: methyl, ethyl, n-hexyl, phenyl, 4-ethenylphenyl, 4-aminomethyl phenyl, 4-vinyloxy group, 4-allyl phenyl, 4-alkene propoxy phenyl, the acrylate-based phenyl of 4-, the acrylate-based phenyl of 4-, 1-hexenyl, 1-butylene base;
More preferably, n and m represents the positive integer of 20-30 separately.
Preferably, the structure of B component is compound shown in following general formula:
R in formula
1group represents the identical or different monovalence representative examples of saturated aliphatic alkyl that carbonatoms is 1-6, R
3group represents the monovalence representative examples of saturated aliphatic alkyl that phenyl, substituted-phenyl or carbonatoms are 1-6, R
4group represents identical or different monovalence representative examples of saturated aliphatic alkyl or the hydrogen functional group that carbonatoms is 1-6, has two R
4a R is had at least in a chain link of group
4group is hydrogen functional group, p and q is respectively the positive integer of 10-100
R
1group can be selected from following group: methyl, ethyl, n-hexyl;
R
3group can be selected from following group: methyl, ethyl, n-hexyl, phenyl, 4-ethenylphenyl, 4-aminomethyl phenyl, 4-vinyloxy group, 4-allyl phenyl, 4-alkene propoxy phenyl, the acrylate-based phenyl of 4-, the acrylate-based phenyl of 4-, 1-hexenyl, 1-butylene base;
R
4group can be selected from following group: methyl, ethyl, n-hexyl;
Preferably, in the structure of described B component, p and q is respectively the positive integer of 20-30.Preferably, curable silicone rubber composition of the present invention, the specific refractory power before its solidification is greater than 1.5.Although refractive index data obtains for solidification pre-test, consider that the volumetric shrinkage before and after packaging plastic solidification is less, the variations in refractive index before and after its solidification is very little.
For realizing goal of the invention, present invention also offers above-mentioned various curable silicone rubber composition and being cured to the solidifying product that base material obtains.
Preferably, wherein said base material is electric or electronic unit.
Preferably, wherein said base material is the optical, electrical device of aluminium material and other metal materials.
Preferably, wherein said base material is optoelectronic component.
Preferably, wherein said base material is optics.
The present invention also developed a kind of coating agent, the formula A containing individual packages, formula B and formula C, described formula A, component A, B component and component C in the curable silicone rubber composition that formula B is above-mentioned respectively with formula C.In use three is mixed, obtain the curable silicone rubber composition of any viscosity of the present invention between 2000 ~ 20000mPas.
The method that curable silicone rubber composition coated substrate of the present invention also solidifies, comprises the following steps:
Curable silicone rubber composition described in Claims 1-4 any one is coated to base material,
Solidify described curable silicone rubber composition and form the product after solidifying.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized object and effect, be explained in detail below in conjunction with embodiment.
Embodiment 1:
150g octamethylcyclotetrasiloxane is added in the single port bottle of 500ml drying, 150g octaphenylcyclotetrasiloxane, 5g1,1,3,3-tetramethyl--1,3-divinyl disiloxane is after 50 ° of C vaccum dewaterings, the catalyzer temperature-elevating to 160 adding 2g spends reaction 8 hours, obtains the linear methyl phenyl organopolysiloxane 250g of modified by vinyl, viscosity 20000mPas(component 1 after vacuum removal small molecules).
Embodiment 2:
150g octamethylcyclotetrasiloxane is added in the single port bottle of 500ml drying, 150g octaphenylcyclotetrasiloxane and 30g1,1,3,3-tetramethyl--1,3-divinyl disiloxane, after 50 ° of C vaccum dewaterings, the catalyzer temperature-elevating to 160 adding 4g spends reaction 8 hours, obtains the linear methyl phenyl organopolysiloxane 250g of modified by vinyl, viscosity 2000mPas(component 2 after vacuum removal small molecules).
Embodiment 3
The linear methyl phenyl organopolysiloxane obtained in embodiment 1 and embodiment 2 is mixed according to certain ratio, the linear methyl phenyl polyorganosiloxane mixtures of any viscosity between 2000 ~ 20000mPas can be obtained.
| Component 1 quality (20000mPas) | Component 2 quality (2000mPas) | Mixture viscosity |
| 18g | 2g | 16000mPa·s |
| 15g | 5g | 12000mPa·s |
| 10g | 10g | 8000mPa·s |
| 5g | 15g | 5000mPa·s |
| 2g | 18g | 3000mPa·s |
The viscosity of the property aminomethyl phenyl polyorganosiloxane mixtures obtained that table 1 mixes by different ratios
The product that above-mentioned reaction prepares can be used as the component (A) as the basic components of rubber composition of the present invention.Each molecule comprises plural unsaturated group of aliphatic series, and when 25 ° of C, viscosity is at 2000-20000mPas, and all can substitute product that the present embodiment obtains as component (A) containing the organopolysiloxane of phenyl.
Embodiment 4:
In the single port bottle of 500ml drying, add 150g octamethylcyclotetrasiloxane under ice bath, 150g octaphenylcyclotetrasiloxane, 50g tetramethyl-ring tetrasiloxane, add 0.1g catalyzer subsequently.Be warming up to 60 degree and react 12 hours.Reaction terminates rear use washing with alcohol five times, obtains the linear methyl phenyl organopolysiloxane 200g in molecule with multiple si-h bond, viscosity 20000mPas(component 4 after vacuum removal small molecules).
Embodiment 5:
In the single port bottle of 500ml drying, add 150g octamethylcyclotetrasiloxane under ice bath, 150g octaphenylcyclotetrasiloxane, 50g tetramethyl-ring tetrasiloxane, add 0.5g catalyzer subsequently.Be warming up to 60 degree and react 12 hours.Reaction terminates rear use washing with alcohol five times, obtains the linear methyl phenyl organopolysiloxane 200g in molecule with multiple si-h bond, viscosity 2000mPas(component 5 after vacuum removal small molecules).
Embodiment 6
The linear methyl phenyl organopolysiloxane obtained in embodiment 4 and embodiment 5 is mixed according to certain ratio, the linear methyl phenyl polyorganosiloxane mixtures of any viscosity between 2000 ~ 20000mPas can be obtained.
| Component 4 quality (20000mPas) | Component 5 quality (2000mPas) | Mixture viscosity |
| 18g | 2g | 16000mPa·s |
| 15g | 5g | 12000mPa·s |
| 10g | 10g | 8000mPa·s |
| 5g | 15g | 5000mPa·s |
| 2g | 18g | 3000mPa·s |
The viscosity of the property aminomethyl phenyl polyorganosiloxane mixtures obtained that table 1 mixes by different ratios
The product that above-mentioned reaction prepares can as the component of the basic components of rubber composition of the present invention (B).Any molecule comprises plural si-h bond, and when 25 ° of C, viscosity is at 2000-20000mPas, and the organopolysiloxane simultaneously containing methyl and phenyl all can substitute product that the present embodiment obtains as component (B).
Embodiment 7:
In the single port bottle of 100ml drying, add 50g1,1,3,3-tetramethyl--1,3-divinyl disiloxane, 1g Platinic chloride, the filtration after 1 hour that refluxes can obtain the catalyzer that 50g can make the component (C) of the basic components of rubber composition of the present invention.Any molecule comprises more than one platinum courtyard and the organic platinum metal complex of catalyzing addition reaction of silicon with hydrogen can substitute product that the present embodiment obtains as component (C).
Embodiment 8:
Viscosity the various embodiments described above obtained in the ratio of table 1 is the component (A) of 20000mPas, and viscosity is that the component (B) of 2000mPas and component (C) at room temperature fully stir and vacuum defoamation process obtains water white transparency mixed solution and is silicone rubber composition of the present invention.
Embodiment 9:
The composition obtained in embodiment 8 is coated in substrate surface by point gum machine, and being heating and curing as 150 ° of C can obtain organo-silicone rubber solidifying product in 2 hours.The performance of the silicon composition obtained by different ratios formula is in table 1.
The performance of the silicon composition that table 2 mixes in different ingredients ratio
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (10)
1. a curable silicone rubber composition, comprises:
Component A is the methyl phenyl silicone containing aliphatics unsaturated link(age), and the viscosity of its 25 DEG C degree is 5000 ~ 20000mPas,
B component is the methyl phenyl silicone that each molecule contains multiple si-h bond, and its viscosity of 25 DEG C is 12000 ~ 20000mPas,
Component C is platinum metal catalysts,
Wherein the quality of B component accounts for the 10%-20% of the total mass of component A and B component;
Wherein the structure of component A is compound shown in following general formula:
R in formula
1group represents the identical or different monovalence representative examples of saturated aliphatic alkyl that carbonatoms is 1-6, R
2group represents identical or different monovalence unsaturated fatty hydrocarbons base or the monovalence representative examples of saturated aliphatic alkyl that carbonatoms is 1-6, R
3group represents the monovalence representative examples of saturated aliphatic alkyl that phenyl, substituted-phenyl or carbonatoms are 1-6, and in wherein said component A, n and m gets the numerical value of 20-30 respectively;
The structure of wherein said B component is compound shown in following general formula:
R in formula
1group represents the identical or different monovalence representative examples of saturated aliphatic alkyl that carbonatoms is 1-6, R
3group represents the monovalence representative examples of saturated aliphatic alkyl that phenyl, substituted-phenyl or carbonatoms are 1-6, R
4group represents identical or different monovalence representative examples of saturated aliphatic alkyl and the hydrogen functional group that carbonatoms is 1-6, has a R in a chain link at least
4group is hydrogen functional group, and in the structure of described B component, p and q is respectively the positive integer of 20-30.
2. curable silicone rubber composition according to claim 1, the specific refractory power before its solidification is greater than 1.5.
3. curable silicone rubber composition according to claim 1, it mixes the viscosity before after fixing between 2000 ~ 20000mPas, and adjustable arbitrarily.
4. one kind by being cured to the curable silicone rubber composition described in claim 1 to 2 any one the solidifying product that base material obtains.
5. solidifying product according to claim 4, wherein said base material is electric or electronic unit.
6. solidifying product according to claim 4, wherein said base material is the optical, electrical device of aluminium material and other metal materials.
7. solidifying product according to claim 4, wherein said base material is optoelectronic component.
8. solidifying product according to claim 4, wherein said base material is optics.
9. a coating agent, the formula A containing individual packages, formula B and formula C, described formula A, component A, B component and component C in formula B and the formula C curable silicone rubber composition respectively described in corresponding claims 1.
10. use the curable silicone rubber composition coated substrate described in claim 1 to 2 any one and a method for solidification, comprise the following steps:
Curable silicone rubber composition described in claim 1 to 2 any one is coated to base material,
Solidify described curable silicone rubber composition and form the product after solidifying.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104151839A (en) * | 2014-08-08 | 2014-11-19 | 广东省工业技术研究院(广州有色金属研究院) | Phenyl silicone resin for optical fiber matching block |
| CN105670298A (en) * | 2016-03-07 | 2016-06-15 | 惠州赛力珑新材料有限公司 | Addition-type silicon rubber and bonding method thereof |
| CN106832958A (en) * | 2017-02-16 | 2017-06-13 | 广东信翼科技有限公司 | Photocuring add-on type organopolysiloxane composition and its application in LED element encapsulation |
| CN111454662B (en) * | 2020-04-15 | 2021-11-16 | 重庆中弗聚新材料科技有限公司 | Room-temperature-curable organic silicon resin conformal coating and preparation method thereof |
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