CN106398224A - Preparation method of transparent dealcoholized vulcanizing silicone rubber by quickly curing single components at room temperature - Google Patents
Preparation method of transparent dealcoholized vulcanizing silicone rubber by quickly curing single components at room temperature Download PDFInfo
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- CN106398224A CN106398224A CN201610956303.XA CN201610956303A CN106398224A CN 106398224 A CN106398224 A CN 106398224A CN 201610956303 A CN201610956303 A CN 201610956303A CN 106398224 A CN106398224 A CN 106398224A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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Abstract
The invention provides a preparation method of transparent dealcoholized vulcanizing silicone rubber by quickly curing single components at room temperature. The preparation method comprises the following steps: under the protection of nitrogen, mixing dimethyl silicon oil serving as a plasticizer, white carbon black serving as a treating agent and alkoxy-terminated polydimethylsiloxane according to a mixture ratio of mass components by using a planetary mixer, then adding hydrophilic fumed silica serving as filler, uniformly dispersing and performing vacuum desorption on low-boiling-point substances; afterwards, sequentially adding a cross-linking agent, a catalyst, a coupling agent and a stabilizer, desorbing the low-boiling-point substances at the vacuum pressure of -0.097 to -0.092Mpa for 30 minutes, moving to an extrusion machine, extruding and filling, thus obtaining the transparent dealcoholized vulcanizing silicone rubber by quickly curing the single components at the room temperature. According to the preparation method provided by the invention, the hydrophilic fumed silica is adopted as the filler, the corresponding white carbon black is added as the treating agent, the defect that the hydrophobic fumed silica subjected to surface treatment is used as the filler in a traditional method is overcome, and the vulcanizing silicone rubber with the characteristics of low cost, high vulcanizing speed, stable viscosity and structure and excellent storage effect is obtained.
Description
Technical field
The invention belongs to single-component room-temperature-vulsilicone silicone rubber technical field is and in particular to one kind is with hydrophilic gas-phase silica
Preparation method for the dealcoholysis single-component room-temperature-vulsilicone silicone rubber of filler.
Background technology
In organic silicone fluid sealant field, dealcoholized type one-component, because of its feature of environmental protection, non-corrosiveness, economy, is widely used in
Building, the electric, bonding in the field such as Aero-Space, auto industry, medical and health and sealing.
Polymer based on alkoxy end-capped polydimethylsiloxane, the gas-phase silica of surface treatment is as filling out
Material, MTMS are cross-linking agent, organotin is former for the transparent system of alcohol type of viscosifier as catalyst, amino silane
Material is easy to get it is not necessary to special auxiliary agent.But the hydrophobic gas-phase silica using surface treatment, is worth expensive, economically can not
Take.As Chinese patent 103725009A discloses a kind of preparation of fast setting transparent dealcoholized single-component room temperature vulcanized silicone rubber
Method, the gas-phase silica that it is adopted is hydrophobicity.
White carbon makes itself and base polymer wellability extreme difference because of the hydroxyl that its surface exists, and the colloid of preparation was being deposited
In journey, viscosity increases, or even structuring;Deep cure is poor.Hydrophilic white carbon seldom directly adopts in alcohol type system.
The patent of the domestic and international preparation method with regard to producing alcohol type transparent adhesive tape with white carbon for filler and document are a lot.Application number
201310374663.5 storages referring to product and yellowing-resistant performance, prepare its curing rate of silicone adhesive with its method and do not possess soon
The performance of speed solidification.United States Patent (USP) US4467063 provides a kind of hexamethyldisiloxane to process the free hydroxyl group during storing
And alcohol, obtain and preferably store effect, but it adopts the gas-phase silica that filler is D4 surface treatment.
Therefore, research is preferably solidified with obtaining with hydrophilic gas-phase silica for filler and stores the silicone adhesive of effect
It is very significant problem.
Content of the invention
For above-mentioned deficiency of the prior art, it is an object of the invention to provide can for filler with hydrophilic gas-phase silica
Preparation method with expediting setting dealcoholized type single-component room-temperature-vulsilicone silicone rubber.
For solving the above problems, the technical solution used in the present invention is:
The preparation method of one component room temperature fast setting transparent dealcoholized type sulphurated siliastic, comprises the following steps:
(1) raw materials quality component proportion is:
(2) described preparation method is:Under nitrogen protection, by above-mentioned mass component proportioning by plasticizer dimethicone,
White carbon inorganic agent, alkoxy end-capped polydimethylsiloxane are with, after planetary mixer mixing, adding filler hydrophilic gas phase white
White carbon black, after being uniformly dispersed, vacuum deviates from low-boiling-point substance, then sequentially adds cross-linking agent, catalyst, coupling agent, stabilizer, vacuum-
0.097 to -0.092Mpa removing low-boiling-point substance 30min, moves to extruder, extrudes fill, obtain a kind of one component room temperature quickly solid
Change transparent dealcoholized type sulphurated siliastic.
Wherein, the end-capping reagent of described alkoxy end-capped polydimethylsiloxane is MTMS, four methoxies
One of base silane, vinyltrimethoxy silane or several mixture, viscosity is 2000-100000mPa.s.
The viscosity of described plasticizer dimethicone is 100-2000mPa.s.
Described white carbon inorganic agent is hexamethyldisiloxane, one or several mixing of octamethylcyclotetrasilazane
Thing, preferably hexa methyl silazane.
Described catalyst is stannous octoate, di-n-butylacetic acid stannum, dibutyl tin laurate, in dibutyl tin laurate
One or several mixture.
Described filler is hydrophilic gas-phase silica, and specific surface area is 50-380m2/ g, free water content is not higher than
0.3%.
Described coupling agent is γ-aminopropyltrimethoxysilane, γ-(2,3- epoxy, the third oxygen) propyl trimethoxy silicon
One of alkane or N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane or several mixture.
Described stabilizer is in pregnancy basic ring three silazane, hexamethyldisiloxane or octamethylcyclotetrasilazane
Kind or two kinds of mixture.
Described cross-linking agent is MTMS, MTES, methyl tripropoxy silane, vinyl
One of trimethoxy silane, tetramethoxy-silicane, tetraethoxysilane or several mixture.
The technique effect of the present invention is:(1) present invention adopts hydrophilic gas-phase silica is filler, and adds white accordingly
Carbon black treatment agent, overcomes tradition and is used the hydrophobicity gas-phase silica of surface treatment as the shortcoming of filler, obtain cost
Low, curingprocess rate is fast, viscosity and Stability Analysis of Structures, the sulphurated siliastic of storage excellent effect;
(2) a kind of fast setting of present invention room temperature vulcanization alcohol type transparent silicone rubber preparation method be obtained dealcoholized silicone rubber with
Commonsense method is obtained silicone rubber and compares that thixotropy is good, abnormal smells from the patient is low, and curing rate improves 50% to 80%.
Specific embodiment
With reference to embodiment, technical scheme is further elaborated:
Embodiment 1
Under nitrogen protection, by 100 parts of the alkoxy end-capped polydimethylsiloxane of 20000mPa.s, plasticising at 25 DEG C
After 2 parts of 30 parts of hexamethyldisiloxane of agent dimethicone are mixed 30 minutes with planetary mixer, add filler hydrophilic 150
18 parts of/g gas-phase silica, after being uniformly dispersed, vacuum deviate from low-boiling-point substance, then sequentially add 3 parts of MTMSs,
0.25 part of dibutyl tin laurate, 1 part of N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, 1.5 parts of hexamethyl two silicon
Azane, vacuum -0.097 removes low-boiling-point substance 30min, moves to extruder, extrudes fill, obtains a kind of one component room temperature fast setting
Transparent dealcoholized type sulphurated siliastic.
Comparative example 1.1
Under nitrogen protection, by 100 parts of the alkoxy end-capped polydimethylsiloxane of 20000mPa.s, plasticising at 25 DEG C
After 30 parts of agent dimethicone is mixed 30 minutes with planetary mixer, add 18 parts of filler hydrophilic 150/g gas-phase silica,
After being uniformly dispersed, vacuum deviates from low-boiling-point substance, then sequentially adds 3 parts of MTMSs, 0.25 part of tin dilaurate two fourth
Ji Xi, 1 part of N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, 1.5 parts of hexamethyldisiloxane, vacuum -0.097 removes
Low-boiling-point substance 30min, moves to extruder, extrudes fill, obtains a kind of one component room temperature fast setting transparent dealcoholized type silicon sulfide rubber
Glue.
Comparative example 1.2
Under nitrogen protection, by 100 parts of the alkoxy end-capped polydimethylsiloxane of 20000mPa.s, pregnancy at 25 DEG C
After 2 parts of base disilazane, 30 parts of plasticizer dimethicone are mixed 30 minutes with planetary mixer, add filler hydrophobic type water type
18 parts of 150/g gas-phase silica, after being uniformly dispersed, vacuum deviates from low-boiling-point substance, then sequentially adds 3 parts of methyl trimethoxy epoxide silicon
Alkane, 0.25 part of dibutyl tin laurate, 1 part of N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, 1.5 parts of hexamethyl two
Silazane, vacuum -0.097 removes low-boiling-point substance 30min, moves to extruder, extrudes fill, obtains a kind of one component room temperature quickly solid
Change transparent dealcoholized type sulphurated siliastic.
Embodiment 2
Under nitrogen protection, at 25 DEG C viscosity is 100 parts of the alkoxy end-capped polydimethylsiloxane of 50000mPa.s,
15 parts of plasticizer dimethicone, 3 parts of octamethylcyclotetrasilazane add 200/g hydrophilic gas with after planetary mixer mixing
18 parts of phase white carbon, after being uniformly dispersed, vacuum deviates from low-boiling-point substance, then sequentially adds 6 parts of methyl tripropoxy silane, two Laurels
0.5 part of sour dibutyl tin, γ-(2,3- epoxy, the third oxygen) 0.8 part of propyl trimethoxy silicane, pregnancy basic ring three silazane 1.5
Part, vacuum -0.092Mpa removes low-boiling-point substance 30min, moves to extruder, extrudes fill, obtains a kind of one component room temperature quickly solid
Change transparent dealcoholized type sulphurated siliastic.
Comparative example 2.1
Under nitrogen protection, at 25 DEG C viscosity is 100 parts of the alkoxy end-capped polydimethylsiloxane of 50000mPa.s,
15 parts of plasticizer dimethicone adds 18 parts of 200/g hydrophilic gas-phase silica with after planetary mixer mixing, and dispersion is all
After even, vacuum deviate from low-boiling-point substance, then sequentially add 6 parts of methyl tripropoxy silane, 0.5 part of dibutyl tin laurate, γ-
(2,3- epoxies, the third oxygen) 0.8 part of propyl trimethoxy silicane, 1.5 parts of pregnancy basic ring three silazane, vacuum -0.092Mpa removes
Low-boiling-point substance 30min, moves to extruder, extrudes fill, obtains a kind of one component room temperature fast setting transparent dealcoholized type silicon sulfide rubber
Glue.
Comparative example 2.2
Under nitrogen protection, at 25 DEG C viscosity is 100 parts of the alkoxy end-capped polydimethylsiloxane of 50000mPa.s,
15 parts of plasticizer dimethicone, 3 parts of octamethylcyclotetrasilazane add 200/g hydrophobicity gas with after planetary mixer mixing
18 parts of phase white carbon, after being uniformly dispersed, vacuum deviates from low-boiling-point substance, then sequentially adds 6 parts of methyl tripropoxy silane, two Laurels
0.5 part of sour dibutyl tin, γ-(2,3- epoxy, the third oxygen) 0.8 part of propyl trimethoxy silicane, pregnancy basic ring three silazane 1.5
Part, vacuum -0.092Mpa removes low-boiling-point substance 30min, moves to extruder, extrudes fill, obtains a kind of one component room temperature quickly solid
Change transparent dealcoholized type sulphurated siliastic.
Embodiment 3
Under nitrogen protection, at 25 DEG C viscosity is 100 parts of the alkoxy end-capped polydimethylsiloxane of 80000mPa.s,
25 parts of plasticizer dimethicone, 4 parts of hexamethyldisiloxane add 200/g hydrophilic gas phase with after planetary mixer mixing
22 parts of white carbon, after being uniformly dispersed, vacuum deviates from low-boiling-point substance, then sequentially adds 8 parts of vinyltrimethoxy silane, two Laurels
0.7 part of sour dibutyl tin, 1 part of N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, 2 parts of pregnancy basic ring three silazane, very
Sky -0.095Mpa removes low-boiling-point substance 30min, moves to extruder, extrudes fill, obtains a kind of one component room temperature fast setting transparent
Dealcoholized type sulphurated siliastic.
Comparative example 3.1
Under nitrogen protection, at 25 DEG C viscosity is 100 parts of the alkoxy end-capped polydimethylsiloxane of 80000mPa.s,
25 parts of plasticizer dimethicone adds 22 parts of 200/g hydrophilic gas-phase silica with after planetary mixer mixing, and dispersion is all
After even, vacuum deviate from low-boiling-point substance, then sequentially add 8 parts of vinyltrimethoxy silane, 0.7 part of dibutyl tin laurate,
1 part of N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, 2 parts of pregnancy basic ring three silazane, vacuum -0.095Mpa removing is low
Boiling thing 30min, moves to extruder, extrudes fill, obtains a kind of transparent dealcoholized type sulphurated siliastic of one component room temperature fast setting.
Comparative example 3.2
Under nitrogen protection, at 25 DEG C viscosity is 100 parts of the alkoxy end-capped polydimethylsiloxane of 80000mPa.s,
25 parts of plasticizer dimethicone, 4 parts of hexamethyldisiloxane add 200/g hydrophobic type gas phase with after planetary mixer mixing
22 parts of white carbon, after being uniformly dispersed, vacuum deviates from low-boiling-point substance, then sequentially adds 8 parts of vinyltrimethoxy silane, two Laurels
0.7 part of sour dibutyl tin, 1 part of N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane, 2 parts of pregnancy basic ring three silazane, very
Sky -0.095Mpa removes low-boiling-point substance 30min, moves to extruder, extrudes fill, obtains a kind of one component room temperature fast setting transparent
Dealcoholized type sulphurated siliastic.
By the room temperature vulcanization prepared according to above-mentioned steps transparent one pack system alcohol type silicone rubber sealant, at 25 DEG C, 50% is wet
Under the conditions of degree, test its curing performance.Performance is referring to subordinate list 1
Can draw from the experimental data of table 1:The present invention is with hydrophilic gas-phase silica as filler, and passes through at white carbon
After reason agent is processed, obtained sulphurated siliastic has very excellent performance hence it is evident that being better than hydrophilic process and hydrophobic type
Sulphurated siliastic, reached unforeseeable technique effect.
Finally it should be noted that:The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention,
Although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
To modify to the technical scheme described in foregoing embodiments, or equivalent is carried out to wherein some technical characteristics.
All any modification, equivalent substitution and improvement within the spirit and principles in the present invention, made etc., should be included in the present invention's
Within protection domain.
Claims (10)
1. the preparation method of one component room temperature fast setting transparent dealcoholized type sulphurated siliastic is it is characterised in that include following walking
Suddenly:
(1) raw materials quality component proportion is:
(2) described preparation method is:Under nitrogen protection, by above-mentioned mass component proportioning by plasticizer dimethicone, Linesless charcoal
After black inorganic agent, alkoxy end-capped polydimethylsiloxane are mixed with planetary mixer, add filler hydrophilic gas-phase silica,
After being uniformly dispersed, vacuum deviates from low-boiling-point substance, then sequentially adds cross-linking agent, catalyst, coupling agent, stabilizer, vacuum -0.097
Remove low-boiling-point substance 30min to -0.092Mpa, move to extruder, extrude fill, obtain a kind of one component room temperature fast setting transparent
Dealcoholized type sulphurated siliastic.
2. preparation method according to claim 1 it is characterised in that:Described alkoxy end-capped polydimethylsiloxane
End-capping reagent is one of trimethoxy silane, tetramethoxy-silicane, vinyltrimethoxy silane or several mixture,
Viscosity is 2000-100000mPa.s.
3. preparation method according to claim 1 it is characterised in that:The viscosity of described plasticizer dimethicone is
100-2000mPa.s.
4. preparation method according to claim 1 it is characterised in that:Described white carbon inorganic agent is hexamethyl two silicon nitrogen
One or several mixture of alkane, octamethylcyclotetrasilazane.
5. preparation method according to claim 4 it is characterised in that:Described white carbon inorganic agent is hexa methyl silazane.
6. preparation method according to claim 1 it is characterised in that:Described catalyst is stannous octoate, di-n-butylacetic acid
One of stannum, dibutyl tin laurate, dibutyl tin laurate or several mixture.
7. preparation method according to claim 1 it is characterised in that:Described filler is hydrophilic gas-phase silica, compares table
Area is 50-380m2/ g, free water content is not higher than 0.3%.
8. preparation method according to claim 1 it is characterised in that:Described coupling agent is γ-aminopropyl trimethoxy
In silane, γ-(2,3- epoxy, the third oxygen) propyl trimethoxy silicane or N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane
One or several mixture.
9. preparation method according to claim 1 it is characterised in that:Described stabilizer be pregnancy basic ring three silazane,
The mixture of one of hexamethyldisiloxane or octamethylcyclotetrasilazane or two kinds.
10. preparation method according to claim 1 it is characterised in that:Described cross-linking agent is MTMS, first
Ethyl triethoxy silicane alkane, methyl tripropoxy silane, vinyltrimethoxy silane, tetramethoxy-silicane, tetraethoxysilane
One of or several mixture.
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CN107353869A (en) * | 2017-07-17 | 2017-11-17 | 四川建筑职业技术学院 | It is a kind of to be used to emulate acid silicone adhesive of dinosaurs handicraft and preparation method thereof |
CN107699194A (en) * | 2017-10-24 | 2018-02-16 | 山东永安胶业有限公司 | Fluid sealant of high transparency yellowing-resistant and preparation method thereof |
CN109206913A (en) * | 2018-07-07 | 2019-01-15 | 深圳市富邦新材科技有限公司 | A kind of dedicated silicon materials of water proof type USB/Type-C and solution |
CN109354875A (en) * | 2018-09-27 | 2019-02-19 | 芜湖扬展新材料科技服务有限公司 | A kind of alcohol type colourful transparent liquid silastic and its preparation method and application |
CN110862801A (en) * | 2019-11-29 | 2020-03-06 | 湖北环宇化工有限公司 | Dealcoholized transparent silicone sealant with long storage life |
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CN112980195A (en) * | 2021-04-09 | 2021-06-18 | 四川省俊川科技有限公司 | Method for preparing high-hardness single-component alcohol-type room temperature vulcanized silicone rubber by using hydrolyzed material |
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CN116254001A (en) * | 2022-12-27 | 2023-06-13 | 湖北环宇化工有限公司 | Dealcoholized RTV-1 silicone rubber with good storage stability and preparation method thereof |
CN116836626A (en) * | 2022-03-23 | 2023-10-03 | 江苏天辰新材料股份有限公司 | Room-temperature-cured high-viscosity self-leveling coating and preparation method thereof |
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CN110862801B (en) * | 2019-11-29 | 2021-11-16 | 湖北环宇化工有限公司 | Dealcoholized transparent silicone sealant with long storage life |
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CN112980195A (en) * | 2021-04-09 | 2021-06-18 | 四川省俊川科技有限公司 | Method for preparing high-hardness single-component alcohol-type room temperature vulcanized silicone rubber by using hydrolyzed material |
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CN115216268A (en) * | 2022-09-02 | 2022-10-21 | 江西蓝星星火有机硅有限公司 | Dealcoholized transparent high-fluidity organosilicon sealant and preparation method thereof |
CN115216268B (en) * | 2022-09-02 | 2023-08-18 | 江西蓝星星火有机硅有限公司 | Dealcoholized transparent high-fluidity organic silicon sealant and preparation method thereof |
CN116162438A (en) * | 2022-12-27 | 2023-05-26 | 湖北环宇化工有限公司 | Dealcoholized RTV-1 silicone rubber with improved storage life and preparation method thereof |
CN116254001A (en) * | 2022-12-27 | 2023-06-13 | 湖北环宇化工有限公司 | Dealcoholized RTV-1 silicone rubber with good storage stability and preparation method thereof |
CN116162438B (en) * | 2022-12-27 | 2024-06-07 | 湖北环宇化工有限公司 | Dealcoholized RTV-1 silicone rubber with improved storage life and preparation method thereof |
CN116254001B (en) * | 2022-12-27 | 2024-06-07 | 湖北环宇化工有限公司 | Dealcoholized RTV-1 silicone rubber with good storage stability and preparation method thereof |
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Application publication date: 20170215 |