CN102181265A - Heat-resistant silicon rubber adhesive and preparation method thereof - Google Patents
Heat-resistant silicon rubber adhesive and preparation method thereof Download PDFInfo
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- CN102181265A CN102181265A CN2011101341847A CN201110134184A CN102181265A CN 102181265 A CN102181265 A CN 102181265A CN 2011101341847 A CN2011101341847 A CN 2011101341847A CN 201110134184 A CN201110134184 A CN 201110134184A CN 102181265 A CN102181265 A CN 102181265A
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Abstract
The invention discloses heat-resistant silicon rubber adhesive and a preparation method thereof. The adhesive comprises the following components in part by weight: 100 parts of hydroxy terminated polydimethylsiloxane with viscosity of 4,000 to 12,000mPa.s, 10 to 40 parts of silicon dioxide, 1 to 10 parts of cross-linking agent, 0.1 to 1 part of catalyst, 0.1 to 5 parts of hydroxy treatment agent and 1 to 6 parts of heat resistant additive; and the adhesive is prepared in a blending mode. By compounding nano tin dioxide and room temperature vulcanized-1 (RTV-1) silicon rubber adhesive, the heat resistance of the RTV-1 silicon rubber adhesive is improved, the using temperature of the RTV-1 silicon rubber adhesive is improved, and the application range of the RTV-1 silicon rubber adhesive is broadened.
Description
Technical field
The present invention relates to the engineering materials field, more particularly, relate to a kind of high temperature resistant room temperature vulcanized silicone rubber adhesive and preparation method thereof.
Background technology
Single-component room-temperature vulcanized (hereinafter to be referred as RTV-1) silicon rubber has good heat-resisting, anti-weather aging, flame resistant, moisture-proof and permeability, and performances such as excellent electric performance and unreactiveness.They can keep elasticity for a long time in extremely wide temperature range (60～200 ℃), it has following characteristics: (1) single-component packing, and easy to use; (2) condition of cure gentleness, self-vulcanizing need not heating; Do not have heat release and heat absorption phenomenon when (3) solidifying, it is little to solidify post-shrinkage ratio; (4) cementability to material is good.Therefore, mainly as tackiness agent and seal gum, other is used and also comprises in-place mo(u)lding pad, protective coating and jointing material etc.The RTV-1 silicone rubber adhesive has automatic adhesiveproperties to multiple material such as various metal (aluminium alloy, nickel, cadmium etc.), macromolecular material (rubber, plastics etc.), glass, pottery and concrete.
The RTV-1 silicone rubber adhesive is because easy to use, need not hot setting, thereby be widely used in the bonding of high temperature resistant element, in recent years, research to monocomponent adhesive just mainly concentrates on novel cross-linking system, mechanism of crosslinking, the effective catalyst preparation, several aspects such as thermal destruction mechanism, itself has outstanding high temperature resistance silicon rubber, generally can be at 200 ℃ of following life-time service, but progress along with modern science and technology, its thermotolerance is had higher requirement, especially along with aviation, the development of spationautics, the thermotolerance that further improves single-component room temperature vulcanized silicone rubber adhesive becomes the research focus.
Summary of the invention
The object of the present invention is to provide a kind of room temperature vulcanized silicone rubber adhesive and preparation method thereof, be intended to improve the resistance toheat of single-component room-temperature vulcanized rubber (RTV-1), improve its use temperature.
Purpose of the present invention is achieved by following technical proposals:
A kind of heat-resisting silicone rubber adhesive takes by weighing following component according to parts by weight:
Viscosity is 100 parts of the hydroxyl-terminated injecting two methyl siloxanes of 4000～12000mPas
0～40 part of silica 1
1～10 part of linking agent
0.1～1 part of catalyzer
0.1～5 part of hydroxyl treatment agent
1～6 part of heat-resisting additive
Prepare according to following step:
(1) be that hydroxyl-terminated injecting two methyl siloxane, silicon-dioxide and the heat-resisting additive of 4000～12000mPas mixes dry deaeration with described viscosity;
(2) in the mixture of step (1) preparation, add described hydroxyl treatment agent, catalyzer and linking agent, mix, promptly make resistant to elevated temperatures room temperature vulcanized silicone rubber adhesive.
Described each components contents is preferably as follows:
5～30 parts of silica 1s
3～8 parts of linking agents
0.4～0.8 part of catalyzer
1～5 part of hydroxyl treatment agent
2～6 parts of heat-resisting additives
Described each components contents is more preferably as follows:
20～30 parts of silicon-dioxide
3～5 parts of linking agents
0.5～0.8 part of catalyzer
2～5 parts of hydroxyl treatment agents
2～5 parts of heat-resisting additives
Described linking agent is the dichloromethyl triethoxyl silane.
Described catalyzer is a dibutyl tin laurate.
Described hydroxyl treatment agent is pregnancy basic ring three silazane.
Described heat-resisting additive is a nano-stannic oxide.
Preferred 5000～the 10000mPas of the viscosity of described hydroxyl-terminated injecting two methyl siloxane is more preferably 6000～8000mPas, for example the hydroxyl-terminated injecting two methyl siloxane of morning twilight chemical research institute.Described silicon-dioxide is the R8200 model fumed silica of Evonik Degussa company.The product of all the other material choice general chemical manufacturers gets final product.
In the described step (1), dry deaeration optimal process is dry deaeration 1～6h in vacuum drying oven, and temperature is 50～80 ℃, and vacuum tightness is 0.02～0.05MPa.
In the described step (2), preferably stir 0.5～1h down at 20～25 ℃, vacuum tightness is 0.02～0.05MPa.
The nano-stannic oxide that the present invention uses belongs to rutile structure, has characteristics such as high-melting-point, Heat stability is good, corrosion-resistant, good mechanical stability, has obtained using widely at aspects such as solar conversion cells, antistatic material, electrode materialss.Itself has outstanding high temperature resistance silicon rubber, generally can because nano-stannic oxide has higher thermostability, it can be added the thermotolerance of improving tackiness agent in the RTV-1 silicone rubber adhesive at 200 ℃ of following life-time service.Nano-stannic oxide and RTV-1 silicone rubber adhesive are carried out compound, improve the resistance toheat of RTV-1 silicone rubber adhesive, improve the use temperature of RTV-1 silicone rubber adhesive, expand the range of application of RTV-1 silicone rubber adhesive.
Embodiment
The present invention is described further below in conjunction with specific embodiment.Room temperature vulcanized silicone rubber adhesive to the present invention's preparation carries out property detection, the tackiness agent of preparation is made the bonding batten of aluminium-aluminium according to the GB/T7124-2008 standard, self-vulcanizing 7 days, sample is divided into three parts, get wherein two parts of aging 2h under 250 ℃ and 300 ℃ of warm air environment respectively, getting wherein, another part is positioned over (25 ℃) 48h under the room temperature, obtain under the room temperature respectively and aging back sample, and the shearing resistance before and after its thermal ageing of the M350-20KN of Testometric company type pulling force aircraft measurements, velocity of shear is 5mm/min.The hydroxyl-terminated injecting two methyl siloxane that uses among the embodiment is the hydroxyl-terminated injecting two methyl siloxane of morning twilight chemical research institute, silicon-dioxide is the R8200 model fumed silica of Evonik Degussa company, the product of all the other material choice general chemical manufacturers gets final product, for example the nano-stannic oxide of pregnancy basic ring three silazane of the precious chemical industry of the dichloromethyl triethoxyl silane of the dibutyl tin laurate of Tianjin first chemical reagent work, Liyang chemical industry tomorrow company limited, Hangzhou silicon company limited, middle ship heavy industry 725 institutes.
At first prepare check sample
(1) be that hydroxyl-terminated injecting two methyl siloxane 100 weight parts, fumed silica 10 weight parts of 9100mPas carry out thorough mixing with viscosity, the mixture that obtains is put into the dry deaeration 2h of vacuum drying oven, and 60 ℃ of temperature, vacuum tightness are 0.04MPa;
(2) under dry environment, in the mixture of step (1) preparation, add pregnancy basic ring three silazane 0.1 weight part, dichloromethyl triethoxyl silane 1 weight part, dibutyl tin laurate 0.1 weight part, stir 0.5h down at 25 ℃, vacuum tightness is 0.05MPa, promptly makes a kind of high temperature resistant RTV-1 silicone rubber adhesive, pours into sealing preservation in the metallic hose.
(3) tackiness agent that (2) are prepared, press GB/T7124-2008 and make the bonding batten of aluminium-aluminium, self-vulcanizing 7 days, sample is divided into three parts, get wherein two parts of aging 2h under 250 ℃ and 300 ℃ of warm air environment respectively, a copy of it is positioned over (25 ℃) 48h under the room temperature, obtains under the room temperature respectively and aging back sample, carries out the shearing resistance test.
Embodiment 1
(1) be that hydroxyl-terminated injecting two methyl siloxane 100 weight parts, fumed silica 15 weight parts and nano-stannic oxide 1 weight part of 9100mPas mixes with viscosity, the mixture that obtains is put into the dry deaeration 2h of vacuum drying oven, 60 ℃ of temperature, vacuum tightness are 0.04MPa;
(2) under dry environment, in the mixture of step (1) preparation, add pregnancy basic ring three silazane 0.5 weight part, dichloromethyl triethoxyl silane 2 weight parts, dibutyl tin laurate 0.2 weight part, stir 0.5h down at 25 ℃, vacuum tightness is 0.05MPa, promptly makes a kind of high temperature resistant RTV-1 silicone rubber adhesive, pours into sealing preservation in the metallic hose.
(3) test by the method and the condition of blank sample.
Embodiment 2
(1) with viscosity is hydroxyl-terminated injecting two methyl siloxane 100 weight parts, fumed silica 20 weight parts and the mixing of nano-stannic oxide 2 weight parts of 9100mPas, the mixture that obtains is put into the dry deaeration 4h of vacuum drying oven, 50 ℃ of temperature, vacuum tightness are 0.04MPa;
(2) under dry environment, in the mixture of step (1) preparation, add pregnancy basic ring three silazane 1 weight part, dichloromethyl triethoxyl silane 3 weight parts, dibutyl tin laurate 0.3 weight part, stir 0.6h down at 25 ℃, vacuum tightness is 0.05MPa, promptly makes a kind of high temperature resistant RTV-1 silicone rubber adhesive, pours into sealing preservation in the metallic hose.
(3) test by the method and the condition of blank sample.
Embodiment 3
(1) with viscosity is hydroxyl-terminated injecting two methyl siloxane 100 weight parts, fumed silica 25 weight parts and the mixing of nano-stannic oxide 3 weight parts of 9100mPas, the mixture that obtains is put into the dry deaeration 3.5h of vacuum drying oven, 80 ℃ of temperature, vacuum tightness are 0.05MPa;
(2) under dry environment, in the mixture of step (1) preparation, add pregnancy basic ring three silazane 3 weight parts, dichloromethyl triethoxyl silane 4 weight parts, dibutyl tin laurate 0.4 weight part, stir 0.7h down at 20 ℃, vacuum tightness is 0.04MPa, promptly makes a kind of high temperature resistant RTV-1 silicone rubber adhesive, pours into sealing preservation in the metallic hose.
(3) test by the method and the condition of blank sample.
Embodiment 4
(1) with viscosity is hydroxyl-terminated injecting two methyl siloxane 100 weight parts, fumed silica 30 weight parts and the mixing of nano-stannic oxide 4 weight parts of 9100mPas, the mixture that obtains is put into the dry deaeration 4h of vacuum drying oven, 50 ℃ of temperature, vacuum tightness are 0.02MPa;
(2) under dry environment, in the mixture of step (1) preparation, add pregnancy basic ring three silazane 4 weight parts, dichloromethyl triethoxyl silane 6 weight parts, dibutyl tin laurate 0.6 weight part, stir 0.8h down at 25 ℃, vacuum tightness is 0.02MPa, promptly makes a kind of high temperature resistant RTV-1 silicone rubber adhesive, pours into sealing preservation in the metallic hose.
(3) test by the method and the condition of blank sample.
Embodiment 5
(1) with viscosity is hydroxyl-terminated injecting two methyl siloxane 100 weight parts, fumed silica 35 weight parts and the mixing of nano-stannic oxide 5 weight parts of 9100mPas, the mixture that obtains is put into the dry deaeration 5h of vacuum drying oven, 60 ℃ of temperature, vacuum tightness are 0.03MPa;
(2) under dry environment, in the mixture of step (1) preparation, add pregnancy basic ring three silazane 4.5 weight parts, dichloromethyl triethoxyl silane 8 weight parts, dibutyl tin laurate 0.8 weight part, stir 0.9h down at 25 ℃, vacuum tightness is 0.03MPa, promptly makes a kind of high temperature resistant RTV-1 silicone rubber adhesive, pours into sealing preservation in the metallic hose.
(3) test by the method and the condition of blank sample.
Embodiment 6
(1) with viscosity is hydroxyl-terminated injecting two methyl siloxane 100 weight parts, fumed silica 40 weight parts and the mixing of nano-stannic oxide 6 weight parts of 9100mPas, the mixture that obtains is put into the dry deaeration 6h of vacuum drying oven, 70 ℃ of temperature, vacuum tightness are 0.04MPa;
(2) under dry environment, in the mixture of step (1) preparation, add pregnancy basic ring three silazane 5 weight parts, dichloromethyl triethoxyl silane 10 weight parts, dibutyl tin laurate 1 weight part, stir 1h down at 25 ℃, vacuum tightness is 0.05MPa, promptly makes a kind of high temperature resistant RTV-1 silicone rubber adhesive, pours into sealing preservation in the metallic hose.
(3) test by the method and the condition of blank sample.
As shown in Table 1, the adding of the nano-stannic oxide shearing resistance that can improve tackiness agent improves silicon rubber heat-resisting simultaneously.And as can be seen, behind the adding tindioxide,, still can reach service requirements though decline is arranged 300 ℃ of aging back silicone rubber adhesive shearing resistances, therefore can under 300 ℃ condition, use.
The shearing resistance of RTV-1 silicone rubber adhesive under table 1 differing temps
More than the present invention has been done exemplary description; should be noted that; under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (9)
1. a heat-resisting silicone rubber adhesive is characterized in that, takes by weighing following component according to parts by weight:
Viscosity is 100 parts of the hydroxyl-terminated injecting two methyl siloxanes of 4000～12000mPas
0～40 part of silica 1
1～10 part of linking agent
0.1～1 part of catalyzer
0.1～5 part of hydroxyl treatment agent
1～6 part of heat-resisting additive
Prepare according to following step:
(1) be that hydroxyl-terminated injecting two methyl siloxane, silicon-dioxide and the heat-resisting additive of 4000～12000mPas mixes dry deaeration with described viscosity;
(2) in the mixture of step (1) preparation, add described hydroxyl treatment agent, catalyzer and linking agent, mix, promptly make resistant to elevated temperatures room temperature vulcanized silicone rubber adhesive.
2. a kind of heat-resisting silicone rubber adhesive according to claim 1 is characterized in that, described each components contents is preferably as follows:
5～30 parts of silica 1s
3～8 parts of linking agents
0.4～0.8 part of catalyzer
1～5 part of hydroxyl treatment agent
2～6 parts of heat-resisting additives
3. a kind of heat-resisting silicone rubber adhesive according to claim 1 is characterized in that, described each components contents is more preferably as follows:
20～30 parts of silicon-dioxide
3～5 parts of linking agents
0.5～0.8 part of catalyzer
2～5 parts of hydroxyl treatment agents
2～5 parts of heat-resisting additives
4. a kind of heat-resisting silicone rubber adhesive according to claim 1 is characterized in that,
Described linking agent is the dichloromethyl triethoxyl silane
Described catalyzer is a dibutyl tin laurate
Described hydroxyl treatment agent is pregnancy basic ring three silazane
Described heat-resisting additive is a nano-stannic oxide
5. a kind of heat-resisting silicone rubber adhesive according to claim 1 is characterized in that,
Preferred 5000～the 10000mPas of the viscosity of described hydroxyl-terminated injecting two methyl siloxane is more preferably 6000～8000mPas; Described silicon-dioxide is fumed silica.
6. one kind prepares as weighing the method for 1 described heat-resisting silicone rubber adhesive, it is characterized in that, is prepared according to following step:
(1) be that hydroxyl-terminated injecting two methyl siloxane, silicon-dioxide and the heat-resisting additive of 4000～12000mPas mixes dry deaeration with described viscosity;
(2) in the mixture of step (1) preparation, add described hydroxyl treatment agent, catalyzer and linking agent, mix, promptly make resistant to elevated temperatures room temperature vulcanized silicone rubber adhesive.
7. the method for the heat-resisting silicone rubber adhesive of a kind of preparation room according to claim 6 is characterized in that,
Described linking agent is the dichloromethyl triethoxyl silane
Described catalyzer is a dibutyl tin laurate
Described hydroxyl treatment agent is pregnancy basic ring three silazane
Described heat-resisting additive is a nano-stannic oxide
Preferred 5000～the 10000mPas of the viscosity of described hydroxyl-terminated injecting two methyl siloxane is more preferably 6000～8000mPas; Described silicon-dioxide is fumed silica.
8. a kind of method for preparing heat-resisting silicone rubber adhesive according to claim 6 is characterized in that, in the described step (1), dry deaeration optimal process is dry deaeration 1～6h in vacuum drying oven, and temperature is 50～80 ℃, and vacuum tightness is 0.02～0.05MPa.
9. a kind of method for preparing heat-resisting silicone rubber adhesive according to claim 6 is characterized in that, in the described step (2), preferably stirs 0.5～1h down at 20～25 ℃, and vacuum tightness is 0.02～0.05MPa.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104371600A (en) * | 2014-10-31 | 2015-02-25 | 青岛昌安达药业有限公司 | Glue for plastics |
| CN105605333A (en) * | 2016-03-04 | 2016-05-25 | 孙欣 | Pipeline for conveying pulverized coal |
| CN105778507A (en) * | 2016-03-04 | 2016-07-20 | 攸潇潇 | Material conveying pipeline |
| CN111534271A (en) * | 2020-05-12 | 2020-08-14 | 广东圣堡达高新科技有限公司 | Glue for roads and bridges and preparation method thereof |
| CN113398318A (en) * | 2021-06-11 | 2021-09-17 | 上海达华药业有限公司 | Preparation method of medical adhesive and medical adhesive |
| CN116333499A (en) * | 2023-02-28 | 2023-06-27 | 南京航空航天大学 | Wave-absorbing low-shrinkage methyl vinyl silicone rubber and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104371600A (en) * | 2014-10-31 | 2015-02-25 | 青岛昌安达药业有限公司 | Glue for plastics |
| CN105605333A (en) * | 2016-03-04 | 2016-05-25 | 孙欣 | Pipeline for conveying pulverized coal |
| CN105778507A (en) * | 2016-03-04 | 2016-07-20 | 攸潇潇 | Material conveying pipeline |
| CN111534271A (en) * | 2020-05-12 | 2020-08-14 | 广东圣堡达高新科技有限公司 | Glue for roads and bridges and preparation method thereof |
| CN113398318A (en) * | 2021-06-11 | 2021-09-17 | 上海达华药业有限公司 | Preparation method of medical adhesive and medical adhesive |
| CN113398318B (en) * | 2021-06-11 | 2022-04-08 | 上海达华药业有限公司 | Preparation method of medical adhesive and medical adhesive |
| CN116333499A (en) * | 2023-02-28 | 2023-06-27 | 南京航空航天大学 | Wave-absorbing low-shrinkage methyl vinyl silicone rubber and preparation method thereof |
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Application publication date: 20110914 |