CN104448322A - Alkoxy MQ silicon resin as well as preparation method and application of alkoxy MQ silicon resin - Google Patents
Alkoxy MQ silicon resin as well as preparation method and application of alkoxy MQ silicon resin Download PDFInfo
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Abstract
The invention relates to an alkoxy MQ silicon resin as well as a preparation method and an application of the alkoxy MQ silicon resin. The chemical formula 1 of the alkoxy MQ silicon resin is as shown in the specification, wherein R refers to a monovalent hydrocarbyl of C1-C8, the ratio of (a+b)/c is 0.6-1.8, and the mole fraction of the alkoxy is 0.4-4.5mmol/g. The active alkoxy group in the alkoxy MQ silicon resin is capable of reacting with an active group in a vulcanized silicone rubber polymer to form a chemical crosslinked point, and compared with the existing silicone rubber products, the mechanical properties of the silicone rubber are greatly improved; and besides, the preparation method of the alkoxy MQ silicon resin is simple and practicable, high in production efficiency, and suitable for industrial production.
Description
Technical field
The present invention relates to modified silicone resin technical field, be specifically related to a kind of alkoxyl group MQ silicone resin and its preparation method and application.
Background technology
Room temperature vulcanized silicone rubber is under the effect not having strengthening agent, and the intensity of itself is very low, usually only has 0.2 ~ 0.3MPa, does not possess any use value.Although the strengthening agents such as calcium carbonate have good reinforcing effect, cannot prepare transparent product, and white carbon black is due to its significant thickening effectiveness, when using as strengthening agent, addition is also unsuitable excessive.Once mention MQ silicone resin in document, because itself and silicon rubber have good consistency, cause any thickening effectiveness hardly, and excellent transparency, can be described as the optimal selection of preparation low viscosity, high transparency vulcanized rubber at room temperature.But current MQ silicone resin is considerably less in the application of room temperature vulcanized silicone rubber, the active group mainly due to MQ silicone resin is little, and when being applied to room temperature vulcanized silicone rubber, the reflecting point of participation is few, and strengthening action is little, and its advantage cannot be embodied fully; And the MQ silicone resin of high hydroxyl content when using in single component condensed room temperature vulcanized silicone rubber, directly can cause hydrogel or not solidify.
Summary of the invention
The object of the invention is to the defect that active group is few, strengthening action is poor overcoming MQ silicone resin in above-mentioned prior art, a kind of alkoxyl group MQ silicone resin is provided; In MQ silicone resin molecule of the present invention, there is a large amount of active alkoxy bases, during for the preparation of silicon rubber, can greatly improve the mechanical property of silicon rubber.
Another object of the present invention is the preparation method providing a kind of alkoxyl group MQ silicone resin.
Above-mentioned purpose of the present invention is achieved by following technical solution:
A kind of alkoxyl group MQ silicone resin, the chemical formula of described alkoxyl group MQ silicone resin is
formula 1;
Wherein R is the monovalent hydrocarbon of C1 ~ C8, and the ratio of (a+b)/c is 0.6 ~ 1.8, and the molar fraction of alkoxyl group is 0.4 ~ 4.5 mmol/g.
In alkoxyl group MQ silicone resin structure provided by the invention ,-Si (OR)
3after group hydrolysis can with the active cross-linking set generation chemical crosslink reaction of sulphurated siliastic, thus improve greatly the mechanical property of silicon rubber, its improvement in performance is mainly reflected in the aspect of performance such as tensile strength, tensile yield, hardness of silicon rubber.
Preferably, in formula 1, described R is the monovalent hydrocarbon of C1 ~ C4.More preferably, R is the saturated hydrocarbyl of C1 ~ C4.More preferably, described R is methyl or ethyl.
Preferably, in formula 1, the ratio of (a+b)/c is 0.6 ~ 1.6.More preferably, the ratio of (a+b)/c is 0.8 ~ 1.2.
Preferably, in formula 1, the molar fraction of alkoxyl group is 0.8 ~ 3.6 mmol/g.More preferably, the molar fraction of alkoxyl group is 1.2 ~ 3.0 mmol/g.
Described alkoxyl group MQ silicone resin reacts obtained by Vinyl MQ silicon resin and organoalkoxysilane under the effect of catalyzer; Wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 2.5:1 ~ 1:2.5 by vinyl and hydrogen base molar ratio computing;
The chemical formula of described Vinyl MQ silicon resin is
formula 2;
Described organoalkoxysilane chemical formula is
formula 3;
Wherein, R represents the monovalent hydrocarbon of C1 ~ C8;
In formula 2, the ratio of (a+b)/c is 0.6 ~ 1.8, and the molar fraction of vinyl is 0.2 ~ 1.5 mmol/g.
A preparation method for described alkoxyl group MQ silicone resin, is dissolved in Vinyl MQ silicon resin in toluene, under the effect of catalyzer, then react obtained with organoalkoxysilane; Wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 2.5:1 ~ 1:2.5 by vinyl and hydrogen base molar ratio computing;
The chemical formula of described Vinyl MQ silicon resin is
formula 2;
Described organoalkoxysilane chemical formula is
formula 3;
Wherein, R represents the monovalent hydrocarbon of C1 ~ C8;
In formula 2, the ratio of (a+b)/c is 0.6 ~ 1.8, and the molar fraction of vinyl is 0.2 ~ 1.5 mmol/g.
Preferably, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 2:1 ~ 1:2 by vinyl and hydrogen base molar ratio computing; Further preferably, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 1:1 ~ 1:1.5 by vinyl and hydrogen base molar ratio computing.Contriver finds, if Vinyl MQ silicon resin is too much excessive, there is a large amount of unreacted vinyl group in system, reinforced effects there will be decline.If the amount of organoalkoxysilane is excessive, then easily cause the waste of raw material.
Preferably, in formula 2, described R is the monovalent hydrocarbon of C1 ~ C4.More preferably, R is the saturated hydrocarbyl of C1 ~ C4.More preferably, R is methyl or ethyl.
Preferably, in formula 2, the ratio of (a+b)/c is 0.6 ~ 1.6.More preferably, the ratio of (a+b)/c is 0.8 ~ 1.2.
Preferably, in formula 2, the molar fraction of described vinyl is 0.4 ~ 1.2 mmol/g.More preferably, the molar fraction of described vinyl is 0.6 ~ 1.0 mmol/g.
Preferably, described catalyzer is the catalyzer of platiniferous; Preferred further, described catalyzer is Platinic chloride, the platinum catalyst of tetrahydrofuran (THF) coordination, the platinum catalyst of methyl vinyl silicone coordination, the platinum catalyst of diethyl phthalate coordination.
The concentration of described catalyzer is based on the total mass meter of all substances in reaction system; Preferably, the concentration when reacting initial is 1 ~ 100 μ g/g, and more preferably, concentration is 1 ~ 50 μ g/g, is more preferably 5 ~ 30 μ g/g.
Above-mentioned reaction is carried out in a heated condition, and preferable reaction temperature is 50 ~ 100 DEG C, more preferably 70 ~ 90 DEG C.
Above-mentioned reaction is preferably carried out at ambient pressure.
The reaction times of above-mentioned reaction is preferably 1 ~ 4 hour, is more preferably 2 ~ 3 hours.
Another object of the present invention is to provide a kind of alkoxyl group MQ silicone resin preparing the application in sulphurated siliastic.With the addition of a certain amount of above-mentioned alkoxyl group MQ silicone resin in this sulphurated siliastic, utilize its-Si (OR)
3can react with the active group in silastic polymer after group hydrolysis, form firmly chemically crosslinked point, thus improve the mechanical property of silicon rubber greatly.
Preferably, the consumption of described alkoxyl group MQ silicone resin when preparing dealcoholized type room temperature vulcanized silicone rubber is 10 ~ 50% of dealcoholized type room temperature vulcanized silicone rubber total mass.
Sulphurated siliastic described in the present invention is dealcoholized type room temperature vulcanized silicone rubber, namely in self-vulcanizing process, carries out condensation reaction, discharges the alcohols material such as methyl alcohol, ethanol.
Compared with prior art, the present invention has following beneficial effect:
The invention discloses a kind of alkoxyl group MQ silicone resin containing active alkoxy base, can react with the active group in sulphurated siliastic polymkeric substance after this active alkoxy base hydrolysis, form chemically crosslinked point, improve the mechanical property of silicon rubber greatly compared with existing silicone rubber products.In addition the preparation method of alkoxyl group MQ silicone resin is simple, and production efficiency is high, is applicable to suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the present invention is further explained, but embodiments of the present invention is not limited in any way.Vinyl MQ silicon resin in the present invention and organoalkoxysilane are all available commercially or are obtained by known method; Unless stated otherwise, involved in embodiment reagent, method are the conventional reagent in this area and method.
Embodiment instrument is as follows:
Mixing machine is DLH-5 type planetary power mixing machine, is produced by Foshan Golden Milky Machine & Equipment Co., Ltd.; Vacuum pump be ZWLW23B type without oily vertical type vacuum pump, produced by Tian Feng vacuum pump company limited.
The Vinyl MQ silicon resin used in embodiment and organoalkoxysilane are commercial raw material, and the chemical formula of described Vinyl MQ silicon resin is
formula 2;
Described organoalkoxysilane chemical formula is
formula 3.
The polydimethylsiloxane structural formula of the trimethoxy end-blocking used in embodiment is
。
the synthesis of embodiment 1 alkoxyl group MQ silicone resin
The Vinyl MQ silicon resin that the present embodiment adopts, the value ratio of (a+b)/c is 0.8, and the molar fraction of described Vinyl MQ silicon resin medium vinyl is 0.67mmol/g; The R of the organoalkoxysilane adopted is methyl; Wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 0.9:1 by vinyl and hydrogen base molar ratio computing.
Preparation method:
100g Vinyl MQ silicon resin is placed in flask, and add 100g toluene Vinyl MQ silicon resin is dissolved completely, and then add the Platinic chloride-aqueous isopropanol (wherein platinum element massfraction is 0.0006% of reactant total mass) of 1.2g massfraction 0.1%, after reactant is heated to 80 DEG C, add 9g organoalkoxysilane, constant temperature stirring reaction 2 hours, be cooled to room temperature and obtain the alkoxyl group MQ silicone resin that alkoxy radical molar mark is 2.0mmol/g, regulate the mass content to 50% of alkoxyl group MQ silicone resin with toluene.
the synthesis of embodiment 2 alkoxyl group MQ silicone resin
The Vinyl MQ silicon resin that the present embodiment adopts, the value ratio of (a+b)/c is 0.6, and the molar fraction of described Vinyl MQ silicon resin medium vinyl is 0.3mmol/g; The R of the organoalkoxysilane adopted is methyl, and wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 1:1 by vinyl and hydrogen base molar ratio computing.
Preparation method:
100g Vinyl MQ silicon resin is placed in flask, and add 100g toluene Vinyl MQ silicon resin is dissolved completely, and then add the platinum catalyst of tetrahydrofuran (THF) coordination of 1.2g massfraction 0.1%, after reactant is heated to 90 DEG C, add 3.7g organoalkoxysilane, constant temperature stirring reaction 3 hours, is cooled to room temperature and obtains the alkoxyl group MQ silicone resin that alkoxy radical molar mark is 0.9 mmol/g, regulates the mass content to 50% of alkoxyl group MQ silicone resin with toluene.
the synthesis of embodiment 3 alkoxyl group MQ silicone resin
The Vinyl MQ silicon resin that the present embodiment adopts, the value ratio of (a+b)/c is 1.4, and the molar fraction of described Vinyl MQ silicon resin medium vinyl is 1.06mmol/g; The R of the organoalkoxysilane adopted is ethyl, and wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 1:1.2 by vinyl and hydrogen base molar ratio computing.
Preparation method:
100g Vinyl MQ silicon resin is placed in flask, and add 100g toluene Vinyl MQ silicon resin is dissolved completely, and then add the platinum catalyst of diethyl phthalate coordination of 1.2g massfraction 0.1%, after reactant is heated to 50 DEG C, add 15.5g organoalkoxysilane, constant temperature stirring reaction 4 hours, is cooled to room temperature and obtains the alkoxyl group MQ silicone resin that alkoxy radical molar mark is 3.2mmol/g, regulates the mass content to 50% of alkoxyl group MQ silicone resin with toluene.
Embodiment 4
the synthesis of alkoxyl group MQ silicone resin
The Vinyl MQ silicon resin that the present embodiment adopts, the value ratio of (a+b)/c is 0.8, and the molar fraction of described Vinyl MQ silicon resin medium vinyl is 0.67mmol/g; The R of the organoalkoxysilane adopted is methyl; Wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 2.5:1 by vinyl and hydrogen base molar ratio computing.
Preparation method:
100g Vinyl MQ silicon resin is placed in flask, and add 100g toluene Vinyl MQ silicon resin is dissolved completely, and then add the Platinic chloride-aqueous isopropanol (wherein platinum element massfraction is 0.0006% of reactant total mass) of 1.2g massfraction 0.1%, after reactant is heated to 80 DEG C, add 3.3g organoalkoxysilane, constant temperature stirring reaction 2 hours, be cooled to room temperature and obtain the alkoxyl group MQ silicone resin that alkoxy radical molar mark is 0.80mmol/g, regulate the mass content to 50% of alkoxyl group MQ silicone resin with toluene.
Embodiment 5
the synthesis of alkoxyl group MQ silicone resin
The Vinyl MQ silicon resin that the present embodiment adopts, the value ratio of (a+b)/c is 1.1, and the molar fraction of described Vinyl MQ silicon resin medium vinyl is 0.3mmol/g; The R of the organoalkoxysilane adopted is ethyl, and wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 1:2.5 by vinyl and hydrogen base molar ratio computing.
Preparation method:
100g Vinyl MQ silicon resin is placed in flask, and add 100g toluene Vinyl MQ silicon resin is dissolved completely, and then add the platinum catalyst of diethyl phthalate coordination of 1.2g massfraction 0.1%, after reactant is heated to 50 DEG C, add 9g organoalkoxysilane, constant temperature stirring reaction 4 hours, is cooled to room temperature and obtains the alkoxyl group MQ silicone resin that alkoxy radical molar mark is 0.9mmol/g, regulates the mass content to 50% of alkoxyl group MQ silicone resin with toluene.
the preparation of embodiment 6 dealcoholized type room temperature vulcanized silicone rubber
By 90 mass parts viscosity be the obtained alkoxyl group MQ silicone resin toluene solution (alkoxyl group MQ silicone resin effective concentration is 50%) of the polydimethylsiloxane of the trimethoxy end-blocking of 20000 mPas and 20 mass parts embodiments 1 under 120 DEG C of vacuum conditions, stir and remove toluene in 1 hour.Then in dry conditions, add the methyltrimethoxy silane of 6 mass parts, the APTES of 1.5 mass parts, two (ethyl acetoacetic acid) titanium of diisopropoxy of 3 mass parts, under 25 DEG C of vacuum conditions, be uniformly mixed 0.5 hour obtained conventional room temperature vulcanized silicone rubber.Last N
2protection, carries out packing, sealing is preserved under dry condition.
the preparation of embodiment 7 dealcoholized type room temperature vulcanized silicone rubber
With reference to the preparation method of embodiment 6,80 mass parts viscosity are adopted to be the room temperature vulcanized silicone rubber product that the polydimethylsiloxane of the trimethoxy end-blocking of the 20000 mPas alkoxyl group MQ silicone resin toluene solution obtained with 40 mass parts embodiments 1 prepares routine.
the preparation of embodiment 8 dealcoholized type room temperature vulcanized silicone rubber
Adopt the alkoxyl group MQ silicone resin toluene solution of embodiment 2, with reference to preparation method's preparation room temperature vulcanizable silicone rubber product of embodiment 6 dealcoholized type room temperature vulcanized silicone rubber.
the preparation of embodiment 9 dealcoholized type room temperature vulcanized silicone rubber
Adopt the alkoxyl group MQ silicone resin toluene solution of embodiment 3, with reference to preparation method's preparation room temperature vulcanizable silicone rubber product of embodiment 6 dealcoholized type room temperature vulcanized silicone rubber.
embodiment 10
Adopt the alkoxyl group MQ silicone resin toluene solution of embodiment 4, with reference to preparation method's preparation room temperature vulcanizable silicone rubber product of embodiment 6 dealcoholized type room temperature vulcanized silicone rubber.
embodiment 11
Adopt the alkoxyl group MQ silicone resin toluene solution of embodiment 5, with reference to preparation method's preparation room temperature vulcanizable silicone rubber product of embodiment 6 dealcoholized type room temperature vulcanized silicone rubber.
the preparation of comparative example 1 dealcoholized type room temperature vulcanized silicone rubber
Adopt 100 mass parts viscosity to be the polydimethylsiloxane of the trimethoxy end-blocking of 20000 mPas, and do not add the application's alkoxyl group MQ silicone resin, as raw material, all the other techniques are identical with embodiment 4, the room temperature vulcanized silicone rubber product that preparation is conventional.
the preparation of comparative example 2 dealcoholized type room temperature vulcanized silicone rubber
Adopting 100 mass parts viscosity to be the polydimethylsiloxane of the trimethoxy end-blocking of 20000 mPas and 10 mass parts specific surface areas is 300m
2the hydrophobic fumed white carbon black of/g, and do not add the application's alkoxyl group MQ silicone resin, as raw material, all the other techniques are identical with embodiment 4, the room temperature vulcanized silicone rubber product that preparation is conventional.
the preparation of comparative example 3 dealcoholized type room temperature vulcanized silicone rubber
With reference to the preparation method of embodiment 4,50 mass parts viscosity are adopted to be the room temperature vulcanized silicone rubber product that the polydimethylsiloxane of the trimethoxy end-blocking of the 20000 mPas alkoxyl group MQ silicone resin toluene solution obtained with 100 mass parts embodiments 1 prepares routine.
Detect the room temperature vulcanized silicone rubber product that above-described embodiment 4 ~ 8 and comparative example 1 ~ 2 obtain, detected result is as shown in table 1 below.
Wherein, the detection method used comprises:
The detection of viscosity is according to GB: GB/T 2794-1995;
The detection of tensile strength is according to GB: GB/T528-2009;
The detection of tensile yield is according to GB: GB/T528-2009;
The detection of hardness is according to GB: GB/T531.1-2008.
Table 1
As can be seen from embodiment 6 ~ 11 and comparative example 1, in the formula preparing dealcoholized type room temperature vulcanized silicone rubber, add described alkoxyl group MQ silicone resin of the present invention, significantly can promote the mechanical property of dealcoholized type room temperature vulcanized silicone rubber; As can be seen from comparative example 2, in prior art, in order to improve the mechanical property of dealcoholized type room temperature vulcanized silicone rubber, can by adding the mode of strengthening agent, but this strengthening agent can increase the viscosity of system greatly, infringement flowing property, and adopt technical scheme of the present invention, the dealcoholized type room temperature vulcanized silicone rubber of preparation can be made to have good mechanical property and flowing property.As can be seen from comparative example 3, when ratio is too high in dealcoholized type room temperature vulcanized silicone rubber for described alkoxyl group MQ silicone resin, composition in its entirety is more prone to the character showing as resin, and the character of nonrubber, therefore its tensile yield obviously declines, and hardness and tensile strength are closer to alkoxy-pure MQ silicone resin.
Claims (10)
1. an alkoxyl group MQ silicone resin, is characterized in that, the chemical formula of described alkoxyl group MQ silicone resin is
formula 1;
Wherein R is the monovalent hydrocarbon of C1 ~ C8, and the ratio of (a+b)/c is 0.6 ~ 1.8, and the molar fraction of alkoxyl group is 0.4 ~ 4.5 mmol/g.
2. alkoxyl group MQ silicone resin according to claim 1, is characterized in that, described R is the monovalent hydrocarbon of C1 ~ C4, and the ratio of (a+b)/c is 0.6 ~ 1.6, and the molar fraction of alkoxyl group is 0.8 ~ 3.6 mmol/g.
3. alkoxyl group MQ silicone resin according to claim 2, is characterized in that, R is methyl or ethyl, and the ratio of (a+b)/c is 0.8 ~ 1.2, and the molar fraction of alkoxyl group is 1.2 ~ 3.0 mmol/g.
4. alkoxyl group MQ silicone resin according to claim 1, is characterized in that, described alkoxyl group MQ silicone resin reacts obtained by Vinyl MQ silicon resin and organoalkoxysilane under the effect of catalyzer; Wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 2.5:1 ~ 1:2.5 by vinyl and hydrogen base molar ratio computing;
The chemical formula of described Vinyl MQ silicon resin is
formula 2;
Described organoalkoxysilane chemical formula is
formula 3;
Wherein, R represents the monovalent hydrocarbon of C1 ~ C8;
In formula 2, the ratio of (a+b)/c is 0.6 ~ 1.8, and the molar fraction of vinyl is 0.2 ~ 1.5 mmol/g.
5. a preparation method for the alkoxyl group MQ silicone resin in Claims 1-4 described in any one claim, is characterized in that, Vinyl MQ silicon resin be dissolved in toluene, under the effect of catalyzer, then react obtained with organoalkoxysilane; Wherein, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 2.5:1 ~ 1:2.5 by vinyl and hydrogen base molar ratio computing;
The chemical formula of described Vinyl MQ silicon resin is
formula 2;
Described organoalkoxysilane chemical formula is
formula 3;
Wherein, R represents the monovalent hydrocarbon of C1 ~ C8;
In formula 2, the ratio of (a+b)/c is 0.6 ~ 1.8, and the molar fraction of vinyl is 0.2 ~ 1.5 mmol/g.
6. the preparation method of alkoxyl group MQ silicone resin according to claim 5, is characterized in that, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 2:1 ~ 1:2 by vinyl and hydrogen base molar ratio computing.
7. the preparation method of alkoxyl group MQ silicone resin according to claim 5, is characterized in that, the amount ratio of described Vinyl MQ silicon resin and organoalkoxysilane is 1:1 ~ 1:1.5 by vinyl and hydrogen base molar ratio computing.
8. the preparation method of alkoxyl group MQ silicone resin according to claim 5, is characterized in that, R described in formula 2 is the monovalent hydrocarbon of C1 ~ C4, and the ratio of described (a+b)/c is 0.6 ~ 1.6, and the molar fraction of vinyl is 0.4 ~ 1.2 mmol/g.
9. alkoxyl group MQ silicone resin according to claim 5, is characterized in that, described R is methyl or ethyl, and the ratio of described (a+b)/c is 0.8 ~ 1.2, and the molar fraction of described vinyl is 0.6 ~ 1.0 mmol/g.
10. the alkoxyl group MQ silicone resin in Claims 1-4 described in any one claim, preparing the application in sulphurated siliastic, is characterized in that, described alkoxyl group MQ silicone resin consumption is 10 ~ 50% of sulphurated siliastic total mass.
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| CN111892906A (en) * | 2020-08-13 | 2020-11-06 | 广州市白云化工实业有限公司 | Dealcoholized single-component silicone sealant capable of being rapidly and deeply cured and preparation method thereof |
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| CN114456771A (en) * | 2021-11-23 | 2022-05-10 | 吉安市木林森新材料科技有限公司 | LED insulation condensed type die bonding adhesive and preparation method thereof |
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| CN111892906A (en) * | 2020-08-13 | 2020-11-06 | 广州市白云化工实业有限公司 | Dealcoholized single-component silicone sealant capable of being rapidly and deeply cured and preparation method thereof |
| CN113789057A (en) * | 2021-09-26 | 2021-12-14 | 北京天山新材料技术有限公司 | One-pack type modified liquid silicone rubber, composition for forming same, and application thereof |
| CN114456771A (en) * | 2021-11-23 | 2022-05-10 | 吉安市木林森新材料科技有限公司 | LED insulation condensed type die bonding adhesive and preparation method thereof |
| CN114196372A (en) * | 2021-12-16 | 2022-03-18 | 广州市白云化工实业有限公司 | Low-viscosity high-strength transparent dealcoholized organosilicon sealant and production method thereof |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150325 |