CN102516931A - Ketoxime-alcohol removal type room-temperature vulcanized silicon rubber sealant and preparation method thereof - Google Patents
Ketoxime-alcohol removal type room-temperature vulcanized silicon rubber sealant and preparation method thereof Download PDFInfo
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- CN102516931A CN102516931A CN2011104024355A CN201110402435A CN102516931A CN 102516931 A CN102516931 A CN 102516931A CN 2011104024355 A CN2011104024355 A CN 2011104024355A CN 201110402435 A CN201110402435 A CN 201110402435A CN 102516931 A CN102516931 A CN 102516931A
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Abstract
The invention discloses a ketoxime-alcohol removal type room-temperature vulcanized silicon rubber sealant and a preparation method thereof. The ketoxime-alcohol removal type room-temperature vulcanized silicon rubber sealant comprises a component A of 100 parts by weight of a ketoxime group-terminiated polydimethylsiloxane, a component B of 10 to 100 parts by weight of a filling material, a component C of 5 to 10 parts by weight of a cross-linking agent, a component D of 1 to 5 parts by weight of a silane coupling agent, a component E of 0.5 to 2 parts by weight of a moisture scavenger, a component F of 1 to 10 parts of fumed silica and a component G of 0.5 to 2 parts by weight of a catalyst. The ketoxime-alcohol removal type room-temperature vulcanized silicon rubber sealant can effectively reduce the quality of micro-molecular ketoxime gas released in single-component silica rubber vulcanization crosslinking, retain excellent performances belonging to a deketoxime type single-component silicone rubber sealant, reduce corrosion produced by ketoxime gas, and satisfy the requirements of future European Union regulations.
Description
Technical field
The present invention relates to a kind of ketoxime-pure type room temperature vulcanized silicone rubber sealing agent and preparation method thereof that takes off; This takes off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent is to be base polymer with the end capped organopolysiloxane of ketoxime base; The organoalkoxysilane that adds three-functionality-degree is as linking agent; Adding the tin catalyst of being known is catalyzer; At room temperature absorb airborne moisture sulfurized silicone rubber sealant, this takes off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent can be widely used in building, industry and electronic enterprises, compares with traditional ketoxime removing type single-component room-temperature vulcanized silicone rubber sealing agent; When keeping its mechanical property, can effectively improve the one-component silicone rubber sealing agent to the adhesiveproperties of base material, reduce the burst size of ketoxime micro-molecular gas when solidifying, reduce corrosion to copper product.
Background technology
At present; The ketoxime removing type one-component silicone rubber is the bigger silica gel of market sales volume; Be mainly used in building, automotive industry, electronic enterprises, traditional ketoxime removing type single-component room-temperature vulcanized silicone rubber is that silane with the three-functionality-degree or four functionality that contain the ketoxime base is as linking agent, under the moisture effect in atmosphere; The silane hydrolytic reactions that contains the ketoxime group forms Si-OH and base resin α; Alpha, omega-dihydroxy polydimethyl siloxane generation vulcanization crosslinking reacts and forms cross-linked network, and the ketoximinosilanes of hydrolytic reactions discharges by product ketoxime gas simultaneously, and the copper oxime gas of release is corrosive to copper product slightly; Simultaneously; The rules of following European Union are to the conditional trend of ketoxime gas, and therefore, the burst size that reduces small molecules ketoxime gas in the reaction of ketoxime removing type single-component room-temperature vulcanized silicone rubber is a new research direction.
Summary of the invention
The objective of the invention is for solving the problem that above-mentioned prior art exists; Adopting the end capped organopolysiloxane of ketoxime base is base polymer; The organoalkoxysilane that adds three-functionality-degree is as linking agent, and adding the tin catalyst of being known is catalyzer, because prepared sealing agent has adopted organoalkoxysilane as linking agent; Containing ketoximinosilanes than employing compares as the ketoxime removing type single-component room-temperature vulcanized silicone rubber of linking agent; It is methyl alcohol or alcohol gas that organoalkoxysilane absorbs the by product that discharges after the airborne moisture hydrolyzes, keep traditional take off ketoxime single-component room-temperature vulcanized silicone rubber sealing agent excellent properties in, reduce small molecules ketoxime gas vol.
A kind of ketoxime-pure type room temperature vulcanized silicone rubber sealing agent that takes off of the present invention, this silicone rubber sealant comprises following A, B, C, D, E, F and G component, each is following by weight:
A: 100 parts of the end capped YSR 3286s of ketoxime base
B: filler 10-100 part
C: linking agent 5-10 part
D: silane coupling agent 1-5 part
E: moisture scavenger 0.5-2 part
F: thermal silica 1-10 part
G: catalyzer 0.5-2 part
The end capped YSR 3286 of ketoxime base of said A component comprises that end group contains that the end capped YSR 3286 of ketoxime base, an end group contain two end capped YSR 3286s of ketoxime base or end group contains three end capped YSR 3286s of ketoxime base;
The filler of described B component is selected one or more in lime carbonate, silicon powder, rhombspar, cristobalite, kaolin or the wilkinite for use;
The linking agent of described C component is selected for use in methyltrimethoxy silane or the vinyltrimethoxy silane at least a;
The silane coupling agent of described D component comprises one or more in mercaptosilane coupling agents, zirconium base silane coupling agent, amino silicane coupling agent, epoxy silane coupling or the acryloxy silane coupling agent;
The moisture scavenger of described E component is selected a kind of in molecular sieve, zeolite, calcium chloride or the magnesium chloride for use;
The thermal silica of described F group is the hydrophobicity aerosil through dimethyldichlorosilane(DMCS) or hexamethyldisilazane surface-treated;
Described G component catalyst is an organotin catalysts, comprises one or more the mixture in monoalkyl organo-tin compound, dialkyl group organo-tin compound, trialkyl organo-tin compound, tetraalkyl organo-tin compound and their inner complex.
The present invention also proposes a kind of ketoxime-pure type room temperature vulcanized silicone rubber sealing agent that preferably takes off, and each component is following by weight:
The A component: the end group that 25 ℃ of following viscositys are 20000cps contains 100 parts of two end capped YSR 3286s of ketoxime base
The B component: the surface is through 100 parts in stearic acid-treated lime carbonate
C component: 8 parts of vinyltrimethoxy silanes
3 parts of D component: N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan
E component: 1 part in molecular sieve
F component: 5 parts of the thermal silicas of handling through hexamethyldisilazane
G component: 1 part of dibutyl tin laurate.
The present invention also proposes a kind of preparation method who takes off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent, and the method comprising the steps of:
(1) successively A, B are fed in the kneader under the condition of vacuum tightness 0.09-0.1MPa by above-mentioned massfraction and mixed 20-40 minute;
(2) at N
2After adding C, D, E under the situation of protection, under the condition of vacuum tightness 0.09-0.1MPa, stirred 30-60 minute;
(3) adding the F component stirred 20-40 minute under the condition of vacuum tightness 0.09-0.1MPa;
(4) at N
2Add under the situation of protection (G), under the condition of vacuum tightness 0.09-0.1MPa, stirred 20-40 minute, can make and take off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent.
The small molecules ketoxime gas vol that the present invention discharges in the time of can effectively reducing single component silica gel vulcanization crosslinking reduces the corrosion of ketoxime gas when keeping ketoxime removing type one-component silicone rubber sealing agent excellent properties, meet the requirement of following European Union rules simultaneously.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment and conjunction with figs., to further explain of the present invention;
The present invention relates to a kind of ketoxime-pure type room temperature vulcanized silicone rubber sealing agent and preparation method thereof that takes off, it is characterized in that this silicone rubber sealant comprises following A-G component, each component is following by weight:
A: 100 parts of the end capped YSR 3286s of ketoxime base
B: filler 10-100 part
C: linking agent 5-10 part
D: silane coupling agent 1-5 part
E: moisture scavenger 0.5-2 part
F: thermal silica 1-10 part
G: catalyzer 0.5-2 part
Described A component is the end capped YSR 3286 of ketoxime base; The end capped YSR 3286 of said ketoxime base comprises that end group contains that the end capped YSR 3286 of ketoxime base, an end group contain two end capped YSR 3286s of ketoxime base and end group contains three end capped YSR 3286s of ketoxime base, and viscosity is 3000-100000mpa.s in the time of 25 ℃; Preferred viscosity is at 10000-30000mp.s, and end group contains two end capped YSR 3286s of ketoxime base;
Described B component is a filler, selects in lime carbonate, silicon powder, rhombspar, cristobalite, kaolin, the wilkinite one or more for use; Preferred surface adopts stearic acid-treated lime carbonate as reinforced filling;
Described C component is a linking agent, selects for use in methyltrimethoxy silane and the vinyltrimethoxy silane at least a; The preferred vinyl Trimethoxy silane is as the vulcanization crosslinking agent;
Described D component is a silane coupling agent, and said coupling agent comprises one or more in mercaptosilane coupling agents, zirconium base silane coupling agent, amino silicane coupling agent, epoxy silane coupling, the acryloxy silane coupling agent; Preferred amino silicane coupling agent and epoxy silane coupling;
Described (E) component is a moisture scavenger, selects a kind of in molecular sieve, zeolite, calcium chloride and the magnesium chloride for use; Preferred molecular sieve is as moisture scavenger;
Described F component is generally selected the aerosil of dimethyldichlorosilane(DMCS) or hexamethyldisilazane modification for use for the hydrophobicity aerosil through surface-treated; The aerosil that preferred surface adopts hexamethyldisilazane to handle.
Described G component is the organotin catalysts of being known, comprises one or more the mixture in monoalkyl organo-tin compound, dialkyl group organo-tin compound, trialkyl organo-tin compound, tetraalkyl organo-tin compound and their inner complex;
The above-mentioned preparation method who takes off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent is: successively A, B are fed in the kneader by above-mentioned massfraction and under the condition of vacuum tightness 0.09-0.1MPa, mixed 20-40 minute, at N
2After adding C, D, E under the situation of protection, under the condition of vacuum tightness 0.09-0.1MPa, stirred 30-60 minute, add the F component after stirring 20-40 minute under the condition of vacuum tightness 0.09-0.1MPa at N
2Add under the situation of protection (G), under the condition of vacuum tightness 0.09-0.1MPa, stir to make in 20-40 minute and take off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent;
Embodiment: the end group that to select 25 ℃ of following viscositys for use be 20000cps contains two end capped YSR 3286s of ketoxime base, and its component is following:
End group contains 100 parts of two end capped YSR 3286s of ketoxime base
The surface is through 100 parts in stearic acid-treated lime carbonate
8 parts of vinyltrimethoxy silanes
3 parts of N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan
1 part in molecular sieve
5 parts of the thermal silicas of handling through hexamethyldisilazane
1 part of dibutyl tin laurate
The end group of above-mentioned viscosity and umber is contained the lime carbonate that dewaters under two end capped YSR 3286s of ketoxime base and 120 ℃ be added in the kneader, under the condition of vacuum tightness 0.09-0.1MPa, mixed 40 minutes, at N
2Add vinyltrimethoxy silane, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan and molecular sieve under the situation of protection; Under the condition of vacuum tightness 0.09-0.1MPa, mixed 40 minutes; Add thermal silica then and under the condition of vacuum tightness 0.09-0.1MPa, mixed 40 minutes, add the organic tin catalyzer at last and after mixing 20 minutes under the condition of vacuum tightness 0.09-0.1MPa, can make and take off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent;
Comparative Examples 1: selecting 25 ℃ of following viscositys for use is the α of 20000cps, alpha, omega-dihydroxy polydimethyl siloxane, and its component is following:
α, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes
The surface is through 100 parts in stearic acid-treated lime carbonate
2 parts of methyl tributanoximo silanes
6 parts of vinyl tributanoximo silanes
3 parts of N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan
1 part in molecular sieve
5 parts of the thermal silicas of handling through hexamethyldisilazane
1 part of dibutyl tin laurate
With the α of above-mentioned viscosity and umber, the lime carbonate that dewaters under alpha, omega-dihydroxy polydimethyl siloxane and 120 ℃ is added in the kneader, under the condition of vacuum tightness 0.09-0.1MPa, mixes 40 minutes, at N
2Methylate tributanoximo silane, vinyl tributanoximo silane, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan and molecular sieve under the situation of protection; Under the condition of vacuum tightness 0.09-0.1MPa, mixed 40 minutes; Add thermal silica then and under the condition of vacuum tightness 0.09-0.1MPa, mixed 40 minutes, add the organic tin catalyzer at last and after mixing 20 minutes under the condition of vacuum tightness 0.09-0.1MPa, can make the single-component ketoxime removing type room temperature vulcanized silicone rubber sealing agent;
The room temperature vulcanized silicone rubber sealing agent of preparation in embodiment and the Comparative Examples 1 is carried out sample preparation and test, result such as table 1 as follows:
Table 1 product performance test data
Wherein, surface drying time: at 23 ± 2 ℃, under 50 ± 5% RH conditions, whenever touched encapsulant surface at a distance from one minute with have gentle hands, the encapsulant surface skinning time is surface drying time;
Hardness: press GB/T 531 test, aging condition is in 85 ℃, 85%RH environment aging 1000 hours;
Tensile strength and elongation at break: press GB/T 528 test, aging condition is in 85 ℃, 85%RH environment aging 1000 hours;
Volume specific resistance: press GB/ T1692 test;
According to GB/T 13477-2002 test mass velocity of variation (solidifying weightless);
Comparative Examples 2: selecting 25 ℃ of following viscositys for use is the α of 20000cps, alpha, omega-dihydroxy polydimethyl siloxane, and its component is following:
α, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes
The surface is through 100 parts in stearic acid-treated lime carbonate
10 parts of vinyl tributanoximo silanes
3 parts of N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan
1 part in molecular sieve
5 parts of the thermal silicas of handling through hexamethyldisilazane
1 part of dibutyl tin laurate
With the α of above-mentioned viscosity and umber, the lime carbonate that dewaters under alpha, omega-dihydroxy polydimethyl siloxane and 120 ℃ is added in the kneader, under the condition of vacuum tightness 0.09-0.1MPa, mixes 40 minutes, at N
2Add vinyl tributanoximo silane, N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan and molecular sieve under the situation of protection; Under the condition of vacuum tightness 0.09-0.1MPa, mixed 40 minutes; Add thermal silica then and under the condition of vacuum tightness 0.09-0.1MPa, mixed 40 minutes, add the organic tin catalyzer at last and after mixing 20 minutes under the condition of vacuum tightness 0.09-0.1MPa, can make the single-component ketoxime removing type room temperature vulcanized silicone rubber sealing agent;
The room temperature vulcanized silicone rubber sealing agent of preparation in embodiment and the Comparative Examples 2 is carried out sample preparation and test as follows, and the result is as shown in table 2:
Table 2 product performance test data
Wherein, surface drying time: at 23 ± 2 ℃, under 50 ± 5% RH conditions, whenever touched encapsulant surface at a distance from one minute with have gentle hands, the encapsulant surface skinning time is surface drying time;
Hardness: press GB/T 531 test, aging condition is in 85 ℃, 85%RH environment aging 1000 hours;
Tensile strength and elongation at break: press GB/T 528 test, aging condition is in 85 ℃, 85%RH environment aging 1000 hours;
Volume specific resistance: press GB/ T1692 test;
According to GB/T 13477-2002 test mass velocity of variation (solidifying weightless);
With preferred embodiment openly as above they are not to be used for limiting the present invention though the present invention is own, and the content that protection scope of the present invention should be defined with the application's claim protection domain is as the criterion.Anyly have the knack of present technique field person, do not breaking away from the spirit and scope of the present invention, various variations of being done or be equal to replacement all should belong to protection scope of the present invention.
Claims (4)
1. one kind is taken off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent, it is characterized in that this silicone rubber sealant comprises following A, B, C, D, E, F and G component, and each is following by weight:
A: 100 parts of the end capped YSR 3286s of ketoxime base
B: filler 10-100 part
C: linking agent 5-10 part
D: silane coupling agent 1-5 part
E: moisture scavenger 0.5-2 part
F: thermal silica 1-10 part
G: catalyzer 0.5-2 part.
2. ketoxime-pure type room temperature vulcanized silicone rubber the sealing agent that takes off according to claim 1 is characterized in that: the end capped YSR 3286 of ketoxime base of said A component comprises that end group contains that the end capped YSR 3286 of ketoxime base, an end group contain two end capped YSR 3286s of ketoxime base or end group contains three end capped YSR 3286s of ketoxime base;
The filler of described B component is selected one or more in lime carbonate, silicon powder, rhombspar, cristobalite, kaolin or the wilkinite for use;
The linking agent of described C component is selected for use in methyltrimethoxy silane or the vinyltrimethoxy silane at least a;
The silane coupling agent of described D component comprises one or more in mercaptosilane coupling agents, zirconium base silane coupling agent, amino silicane coupling agent, epoxy silane coupling or the acryloxy silane coupling agent;
The moisture scavenger of described E component is selected a kind of in molecular sieve, zeolite, calcium chloride or the magnesium chloride for use;
The thermal silica of described F group is the hydrophobicity aerosil through dimethyldichlorosilane(DMCS) or hexamethyldisilazane surface-treated;
Described G component catalyst is an organotin catalysts, comprises one or more the mixture in monoalkyl organo-tin compound, dialkyl group organo-tin compound, trialkyl organo-tin compound, tetraalkyl organo-tin compound and their inner complex.
3. ketoxime-pure type room temperature vulcanized silicone rubber the sealing agent that takes off according to claim 2 is characterized in that each component is following by weight:
The A component: the end group that 25 ℃ of following viscositys are 20000cps contains 100 parts of two end capped YSR 3286s of ketoxime base
The B component: the surface is through 100 parts in stearic acid-treated lime carbonate
C component: 8 parts of vinyltrimethoxy silanes
3 parts of D component: N-(β-aminoethyl)-γ-An Bingjisanjiayangjiguiwan
E component: 1 part in molecular sieve
F component: 5 parts of the thermal silicas of handling through hexamethyldisilazane
G component: 1 part of dibutyl tin laurate.
4. preparation method who takes off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent is characterized in that comprising step:
(1) successively A, B are fed in the kneader under the condition of vacuum tightness 0.09-0.1MPa by above-mentioned massfraction and mixed 20-40 minute;
(2) at N
2After adding C, D, E under the situation of protection, under the condition of vacuum tightness 0.09-0.1MPa, stirred 30-60 minute;
(3) adding the F component stirred 20-40 minute under the condition of vacuum tightness 0.09-0.1MPa;
(4) at N
2Add under the situation of protection (G), under the condition of vacuum tightness 0.09-0.1MPa, stirred 20-40 minute, can make and take off ketoxime-pure type room temperature vulcanized silicone rubber sealing agent.
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| CN2011104024355A CN102516931A (en) | 2011-12-07 | 2011-12-07 | Ketoxime-alcohol removal type room-temperature vulcanized silicon rubber sealant and preparation method thereof |
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| CN2011104024355A CN102516931A (en) | 2011-12-07 | 2011-12-07 | Ketoxime-alcohol removal type room-temperature vulcanized silicon rubber sealant and preparation method thereof |
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| CN102757759A (en) * | 2012-07-11 | 2012-10-31 | 东莞兆舜有机硅新材料科技有限公司 | Single-component catalytic dealcoholized room temperature vulcanized (RTV) silicone rubber and preparation method thereof |
| CN103387811A (en) * | 2013-08-14 | 2013-11-13 | 福建瑞森化工有限公司 | Organic silicon rubber waterproof adhesive and preparation method thereof |
| CN113789149A (en) * | 2021-09-24 | 2021-12-14 | 中天东方氟硅材料有限公司 | Single-component organic silicon molding repair daub and preparation method thereof |
| CN114621724A (en) * | 2022-04-20 | 2022-06-14 | 浙江励德有机硅材料有限公司 | Bi-component organosilicon sealant and preparation method thereof |
| CN117363314A (en) * | 2023-11-02 | 2024-01-09 | 广东高士高科实业有限公司 | Terminal ketoxime group silane-based sealing polydimethyl silane sealant and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117363314A (en) * | 2023-11-02 | 2024-01-09 | 广东高士高科实业有限公司 | Terminal ketoxime group silane-based sealing polydimethyl silane sealant and preparation method thereof |
| CN117363314B (en) * | 2023-11-02 | 2024-04-05 | 广东高士高科实业有限公司 | Terminal ketoxime group silane-based sealing polydimethyl silane sealant and preparation method thereof |
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Application publication date: 20120627 |