CN106751859A - A kind of method that dealcoholized silicone rubber is prepared with microwave treatment hydrophilic white carbon - Google Patents
A kind of method that dealcoholized silicone rubber is prepared with microwave treatment hydrophilic white carbon Download PDFInfo
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- CN106751859A CN106751859A CN201611184607.5A CN201611184607A CN106751859A CN 106751859 A CN106751859 A CN 106751859A CN 201611184607 A CN201611184607 A CN 201611184607A CN 106751859 A CN106751859 A CN 106751859A
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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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a kind of method for preparing dealcoholized silicone rubber with microwave treatment hydrophilic white carbon, specially：Under nitrogen protection; after plasticizer dimethicone, white carbon inorganic agent, alkoxy end-capped dimethyl silicone polymer are mixed with planetary mixer; add the hydrophilic gas-phase silica of microwave treatment; after well mixed, vacuum 0.090Mpa abjection low-boiling-point substance 30min sequentially add crosslinking agent, catalyst, coupling agent, stabilizer afterwards; after well mixed; vacuum 0.097 removes low-boiling-point substance 30min to 0.092Mpa, then moves to extruder, extrudes filling；Being processed hydrophilic gas-phase silica by the way of microwave treatment for the invention, makes the free water content on its surface less than 0.1%, shows hydrophobicity, and prepared SiClx rubber surface is bright and clean, and particle is few, and performance is very excellent.
Description
Technical field
The invention belongs to single-component room-temperature-vulsilicone silicone rubber technical field, and in particular to a kind of white with microwave treatment hydrophilic
The method that carbon black prepares dealcoholized silicone rubber.
Background technology
In organic silicone fluid sealant field, dealcoholized type one-component is widely used in because of its feature of environmental protection, non-corrosiveness, economy
The bonding in the field such as building, electric, Aero-Space, auto industry, medical and health and sealing.
The polymer based on alkoxy end-capped dimethyl silicone polymer, the gas-phase silica of surface treatment is used as filling out
Material, MTMS are that crosslinking agent, organotin are the transparent system original of the alcohol type of tackifier as catalyst, amino silane
Material is easy to get, it is not necessary to special auxiliary agent.But using the hydrophobic gas-phase silica of surface treatment, value is expensive, economically can not
Take.
White carbon makes itself and base polymer wellability extreme difference because of the hydroxyl that its surface is present, and the colloid surface of preparation is not only
It is clean, there is more or less particle.Viscosity increases during storage, or even structuring；Deep cure is poor.Hydrophilic white carbon
Seldom directly used in alcohol type system.
Patent and document on producing the preparation method of alcohol type transparent adhesive tape as filler with white carbon are many both at home and abroad.Application number
201310374663.5 storages for referring to product and yellowing resistance energy, prepare silicone adhesive its curing rate and do not possess soon in its method
The performance of speed solidification.US, 4467063 provide the free hydroxyl group and alcohol during a kind of HMDS treatment storage, obtain
Obtain and preferably store effect, but it uses the gas-phase silica that filler is surface-treated for D4.
The content of the invention
For above-mentioned deficiency of the prior art, it is an object of the invention to provide one kind with hydrophilic gas-phase silica to fill out
Material, hydrophilic meteorology white carbon is processed so as to obtain any surface finish, the few dealcoholized type one-component room of particle by microwave early stage
The preparation method of temperature vulcanizable silicone rubber.
The purpose of the present invention is achieved through the following technical solutions.
A kind of method for preparing dealcoholized silicone rubber with microwave treatment hydrophilic white carbon, comprises the following steps:
(1) by hydrophilic gas-phase silica under the microwave of 2000-3000MHz dewater treatment 3-60min, until white carbon
Free water content is less than 0.3%；
(2) raw material is prepared by following mass component proportioning：
(3) under nitrogen protection, by plasticizer dimethicone, white carbon inorganic agent, alkoxy end-capped polydimethylsiloxanes
After alkane is mixed with planetary mixer, hydrophilic gas-phase silica in filler (1) is added, after being uniformly dispersed, vacuum -0.090Mpa takes off
Go out low-boiling-point substance 30min, crosslinking agent, catalyst, coupling agent, stabilizer are sequentially added afterwards, vacuum -0.097 is de- to -0.092Mpa
Except low-boiling-point substance 30min, extruder is then moved to, extrusion is filling, obtains a kind of transparent dealcoholized type sulphur of one component room temperature rapid curing
SiClx rubber.
Wherein, the frequency of microwave is 2450MHz during the microwave dehydration.
The end-capping reagent of described alkoxy end-capped dimethyl silicone polymer is MTMS, tetramethoxy-silicane
One or several mixture in alkane, vinyltrimethoxy silane, the alkoxy end-capped dimethyl silicone polymer
Viscosity is 2000-100000mPas.
The viscosity of described plasticizer dimethicone is 100-2000mPas.
The white carbon inorganic agent is HMDS, octamethylcyclotetrasilazane one or several mixing
Thing.
The catalyst is in stannous octoate, di-n-butylacetic acid tin, dibutyl tin laurate, dibutyl tin laurate
One or several mixture.
Described filler is hydrophilic gas-phase silica, and its 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- epoxies, the third oxygen) propyl trimethoxy silicon
One or several mixture in alkane or N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane.
The crosslinking agent is MTMS, MTES, methyl tripropoxy silane, vinyl
One or several mixture in trimethoxy silane, tetramethoxy-silicane, tetraethoxysilane.
Described stabilizer is the silazane of pregnancy basic ring three or HMDS, in octamethylcyclotetrasilazane one
Kind or two kinds of mixture.
Technique effect of the invention is：The invention by the way of microwave treatment to hydrophilic gas-phase silica
Processed, make the free water content on its surface less than 0.1%, showed hydrophobicity, can be preferably used in alcohol type saturating
In the preparation method of gelatin, and greatly reduced by gas-phase silica surface hydroxyl after microwave treatment, it is soaked in base polymer
Lubricant nature improves, and the colloid surface of preparation is bright and clean, there is few particle, and prepared SiClx rubber surface is bright and clean, and particle is few,
Performance is very excellent.
Specific embodiment
Technical scheme is further elaborated with reference to embodiment：
Embodiment 1
(1) by hydrophilic gas-phase silica under the microwave of 2450MHz dewater treatment 20min, obtain low from moisture
In 0.2% white carbon；
(2) 25 DEG C, nitrogen protection under, by 20 parts of plasticizer dimethicone, white carbon inorganic agent HMDS 2
After part, 100 parts of the alkoxy end-capped dimethyl silicone polymer of 20000mPas are mixed with planetary mixer, in addition filler (1)
8 parts of the hydrophilic gas-phase silica of the 150 ㎡/g for the treatment of, after being well mixed, vacuum -0.090Mpa abjection low-boiling-point substance 30min, it
After sequentially add 3 parts of crosslinking agent MTMS, 0.25 part of catalyst dibutyltin dilaurylate, coupling agent N- (β-
Aminoethyl) 1 part of-γ-aminopropyltrimethoxysilane, 1.5 parts of three silazane of stabilizer pregnancy basic ring, be well mixed after, vacuum-
0.097Mpa removes low-boiling-point substance 30min, then moves to extruder, and extrusion is filling, obtains a kind of one component room temperature rapid curing saturating
Bright dealcoholized type sulphurated siliastic.
Embodiment 2
(1) by hydrophilic gas-phase silica under the microwave of 2450MHz dewater treatment 30min, obtain low from moisture
In 0.1% white carbon；
(2) 25 DEG C, nitrogen protection under, by 30 parts of plasticizer dimethicone, the silicon nitrogen of white carbon inorganic agent prestox ring four
After 5 parts of alkane, 100 parts of the alkoxy end-capped dimethyl silicone polymer of 30000mPas are mixed with planetary mixer, filler is added
(1) 16 parts of the hydrophilic gas-phase silica of the 350 ㎡/g for the treatment of in, after being well mixed, vacuum -0.090Mpa abjection low-boiling-point substances
30min, sequentially adds 5 parts of crosslinking agent vinyltrimethoxy silane, 0.45 part of catalyst dibutyl tin laurate, coupling afterwards
0.7 part of agent γ-aminopropyltrimethoxysilane, 1.5 parts of stabilizer HMDS, after being well mixed, vacuum-
0.097Mpa removes low-boiling-point substance 30min, then moves to extruder, and extrusion is filling, obtains a kind of one component room temperature rapid curing saturating
Bright dealcoholized type sulphurated siliastic.
Embodiment 3
(1) by hydrophilic gas-phase silica under the microwave of 2450MHz dewater treatment 10min, obtain low from moisture
In 0.3% white carbon；
(2) 25 DEG C, nitrogen protection under, by 25 parts of plasticizer dimethicone, white carbon inorganic agent HMDS 3
After part, 100 parts of the alkoxy end-capped dimethyl silicone polymer of 40000mPas are mixed with planetary mixer, in addition filler (1)
20 parts of the hydrophilic gas-phase silica of the 270 ㎡/g for the treatment of, after being well mixed, vacuum -0.090Mpa abjection low-boiling-point substance 30min,
6 parts of crosslinking agent methyl tripropoxy silane, 0.25 part of octoate catalyst stannous, coupling agent γ-(2,3- rings are sequentially added afterwards
Oxygen, the third oxygen) 1 part of propyl trimethoxy silicane, 2 parts of three silazane of stabilizer pregnancy basic ring, be well mixed after, vacuum-
0.097Mpa removes low-boiling-point substance 30min, then moves to extruder, and extrusion is filling, obtains a kind of one component room temperature rapid curing saturating
Bright dealcoholized type sulphurated siliastic.
Comparative example 1
25 DEG C, nitrogen protection under, by 20 parts of plasticizer dimethicone, 2 parts of white carbon inorganic agent HMDS,
After 100 parts of the alkoxy end-capped dimethyl silicone polymer of 20000mPas is mixed with planetary mixer, 105 DEG C of thermal currents are added
8 parts of the hydrophilic gas-phase silica of 12h is dried, after being well mixed, vacuum -0.090Mpa abjection low-boiling-point substance 30min, afterwards successively
Add 3 parts of crosslinking agent MTMS, 0.25 part of catalyst dibutyltin dilaurylate, coupling agent N- (β-ammonia second
Base) 1 part of-γ-aminopropyltrimethoxysilane, 1.5 parts of three silazane of stabilizer pregnancy basic ring, be well mixed after, vacuum-
0.097Mpa removes low-boiling-point substance 30min, then moves to extruder, and extrusion is filling, obtains a kind of sulphurated siliastic.
The transparent one pack system alcohol type silicone rubber sealant of room temperature vulcanization that will be prepared according to above-mentioned steps, in 25 DEG C, 50%HR
Under damp condition, its surface property is tested.Performance is referring to subordinate list 1
As can be seen from Table 1, the embodiment of the present invention is a kind of with microwave treatment parent respectively by the control of comparative sample and implementation sample
The surface particles of the dealcoholized silicone rubber that water type white carbon is produced are significantly better than the silicon rubber that conventional method is obtained.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the 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
Modified with to the technical scheme described in foregoing embodiments, or equivalent is carried out to which part technical characteristic.
All any modification, equivalent substitution and improvements within the spirit and principles in the present invention, made etc., should be included in of the invention
Within protection domain.
Claims (8)
1. a kind of method that dealcoholized silicone rubber is prepared with microwave treatment hydrophilic white carbon, it is characterised in that including following step
Suddenly:
(1) by hydrophilic gas-phase silica under the microwave of 2000-3000MHz dewater treatment 3-60min, until white carbon is free
Moisture is less than 0.3%；
(2) raw material is prepared by following mass component proportioning：
(3) under nitrogen protection, plasticizer dimethicone, white carbon inorganic agent, alkoxy end-capped dimethyl silicone polymer are used
After planetary mixer mixing, the hydrophilic gas-phase silica for the treatment of in filler (1), after being well mixed, vacuum -0.090Mpa are added
Abjection low-boiling-point substance 30min, sequentially adds crosslinking agent, catalyst, coupling agent, stabilizer afterwards, after being well mixed, vacuum -0.097
Low-boiling-point substance 30min is removed to -0.092Mpa, extruder is then moved to, extrusion is filling, obtains a kind of one component room temperature rapid curing
Transparent dealcoholized type sulphurated siliastic.
2. preparation method according to claim 1, it is characterised in that：The frequency of microwave is during the microwave dehydration
2450MHz。
3. preparation method according to claim 2, it is characterised in that：Described alkoxy end-capped dimethyl silicone polymer
End-capping reagent is the mixed of one or several in MTMS, tetramethoxy-silicane, vinyltrimethoxy silane
Compound, the viscosity of the alkoxy end-capped dimethyl silicone polymer is 2000-100000mPas.
4. preparation method according to claim 2, it is characterised in that：The viscosity of described plasticizer dimethicone is
100-2000mPa·s。
5. preparation method according to claim 2, it is characterised in that：The white carbon inorganic agent is the silicon nitrogen of hexamethyl two
Alkane, octamethylcyclotetrasilazane one or several mixture.
6. the preparation method according to claim 1-2, it is characterised in that：The catalyst is stannous octoate, dibutyl vinegar
One or several mixture in sour tin, dibutyl tin laurate, dibutyl tin laurate.
7. the preparation method according to claim 1-2, it is characterised in that：Described filler is hydrophilic gas-phase silica, its
Specific surface area is 50-380m2/ g, free water content is not higher than 0.1%.
8. the preparation method according to claim 6-7, it is characterised in that：Described coupling agent is γ-aminopropyl trimethoxy
Base silane, γ-(2,3- epoxies, the third oxygen) propyl trimethoxy silicane or N- (β-aminoethyl)-γ-aminopropyltrimethoxysilane
In one or several mixture.
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| CN201611184607.5A CN106751859A (en) | 2016-12-20 | 2016-12-20 | A kind of method that dealcoholized silicone rubber is prepared with microwave treatment hydrophilic white carbon |
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| CN201611184607.5A CN106751859A (en) | 2016-12-20 | 2016-12-20 | A kind of method that dealcoholized silicone rubber is prepared with microwave treatment hydrophilic white carbon |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113620304A (en) * | 2021-09-09 | 2021-11-09 | 无锡恒诚硅业有限公司 | Preparation method of hydrophobic white carbon black |
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| CN103725009A (en) * | 2014-01-02 | 2014-04-16 | 湖北环宇化工有限公司 | Preparation method of fast curing dealcoholization type transparent room-temperature silicon sulfide rubber |
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| CN103725009A (en) * | 2014-01-02 | 2014-04-16 | 湖北环宇化工有限公司 | Preparation method of fast curing dealcoholization type transparent room-temperature silicon sulfide rubber |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113620304A (en) * | 2021-09-09 | 2021-11-09 | 无锡恒诚硅业有限公司 | Preparation method of hydrophobic white carbon black |
| CN113620304B (en) * | 2021-09-09 | 2024-02-23 | 无锡恒诚硅业有限公司 | Preparation method of hydrophobic white carbon black |
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Application publication date: 20170531 |