CN109679496A - Release silicone oil of solvent-free organic silicon and preparation method thereof - Google Patents
Release silicone oil of solvent-free organic silicon and preparation method thereof Download PDFInfo
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- CN109679496A CN109679496A CN201811587816.3A CN201811587816A CN109679496A CN 109679496 A CN109679496 A CN 109679496A CN 201811587816 A CN201811587816 A CN 201811587816A CN 109679496 A CN109679496 A CN 109679496A
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- Prior art keywords
- solvent
- silicone oil
- release silicone
- free organic
- organic silicon
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions 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; Coating compositions based on derivatives of such polymers
- C09D183/04—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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/20—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for coatings strippable as coherent films, e.g. temporary coatings strippable as coherent films
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/262—Alkali metal carbonates
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Lubricants (AREA)
- Silicon Polymers (AREA)
Abstract
The present invention proposes a kind of release silicone oil of solvent-free organic silicon and preparation method thereof, the release silicone oil of the solvent-free organic silicon includes following components by mass percentage: the octamethylcy-clotetrasiloxane or dimethyl siloxane mixing ring of 60%-85%, three (vinyl-dimethyl base siloxy) methyl-monosilanes of 5%-20%, the strong acid of 2%-5% is as catalyst, the neutralizer of 5%-15%.The release silicone oil of solvent-free organic silicon proposed by the present invention can directly be coated with use, and be suitable for the product of light off-type force and ultralight off-type force without adding any solvent when use.The present invention also proposes the preparation method of the release silicone oil of the solvent-free organic silicon, can obtain the release silicone oil of no-solvent type of the appearance transparent without obvious smell.
Description
Technical field
The present invention relates to release silicone oil of a kind of solvent-free organic silicon and preparation method thereof.
Background technique
Be coated on currently on the market silicone release agent in PET film be generally using containing solvent type organosilicon from
Type agent, the content of solvent is up to 70%, and is diluted to lower painting being coated with the solvent for having to 5 to 7 times of addition when use
Cloth viscosity, the quantity of solvent that this mould release uses is very big, causes seriously to pollute to environment, and the performance one of the solvent mould release
As, such as remaining rate is lower (85% or less), to cause the reduced performance of glue；There are also the off-type force of the mould release is higher, no
It can be suitably used for the requirement product of light off-type force and ultralight off-type force, which limits its uses.
Summary of the invention
The present invention proposes a kind of release silicone oil of solvent-free organic silicon, without adding any solvent when use, can directly be coated with
It uses, and is suitable for the product of light off-type force and ultralight off-type force.The present invention also proposes the release silicone oil of the solvent-free organic silicon
Preparation method.
The present invention proposes a kind of release silicone oil of solvent-free organic silicon, by mass percentage includes following components: 60%-
85% octamethylcy-clotetrasiloxane or dimethyl siloxane mixing ring, three (vinyl-dimethyl base siloxy) first of 5%-20%
Base silane, the strong acid of 2%-5% is as catalyst, the neutralizer of 5%-15%.
Further, the strong acid is the concentrated sulfuric acid or trifluoromethanesulfonic acid.
Further, the neutralizer is natrium carbonicum calcinatum or Carbon Dioxide calcium.
Further, the release silicone oil of the solvent-free organic silicon, viscosity 230mpa.s-500mpa.s.
The present invention also proposes the preparation method of the release silicone oil of solvent-free organic silicon described in one kind, comprising the following steps:
Step 1, by octamethylcy-clotetrasiloxane or dimethyl siloxane mixing ring and three (vinyl-dimethyl base siloxies)
Methyl-monosilane is dosed into reaction kettle and is stirred.
Step 2 is added strong acid catalyst, and be warming up to 60 DEG C~90 DEG C, stirs under constant temperature under the conditions of nitrogen protection
Then balanced reaction in 5-7 hours stops heating, is cooled to room temperature.
Step 3 is added natrium carbonicum calcinatum, and stirs 3-5 hours, desalination is filtered after standing, filtrate decompression is taken off it is low, most
Lead to nitrogen afterwards, stops heating, takes off low, cooling discharging obtains the release silicone oil of no-solvent type of the appearance transparent without obvious smell.
Further, it is 170 DEG C that decompression described in step 3, which takes off low condition, continues 1.5-2.5 hours.
Beneficial effects of the present invention:
The release silicone oil of solvent-free organic silicon of the invention, viscosity is lower, can be straight in the case where not adding other solvents
Coating is connect, many solvents are saved, it is more friendly to environment.
The present invention is being closed as end-capping reagent containing branched structure using three (vinyl-dimethyl base siloxy) methyl-monosilanes
During at silicone oil, so that silicone oil has been had collateralization phenomenon, i.e., other curing agent are added not yet inside silicone oil
In the case of just produced partial cross-linked structure, and not no feature of common mould release silicone oil needs to add when in use
Curing agent is added just to generate cross-linked structure.And when in use, even if the present invention and the release silicone oil addition of solvent type are identical solid
Agent, the effect that generates after solidifying can be more preferable, i.e., its crosslink density can silicone oil more release than common solvent type it is higher, so as to
Improve its performance (as remaining rate can be more preferable), the application suitable for light off-type force and ultralight release product.
Specific embodiment
As follows in conjunction with specific embodiments, application scheme is further described:
Embodiment 1
A kind of release silicone oil of solvent-free organic silicon includes following components: 85% four silicon of prestox ring by mass percentage
Oxygen alkane, 5% three (vinyl-dimethyl base siloxy) methyl-monosilanes, 3% concentrated sulfuric acid is as catalyst, 7% Carbon Dioxide
Sodium is as neutralizer.
A kind of preparation method of the release silicone oil of above-mentioned solvent-free organic silicon, comprising the following steps:
Octamethylcy-clotetrasiloxane and three (vinyl-dimethyl base siloxy) methyl-monosilanes are dosed into reaction kettle by step 1
In be stirred.
Step 2 is added the catalyst concentrated sulfuric acid, and be warming up to 70 DEG C, stirs 6 hours under constant temperature under the conditions of nitrogen protection
Then balanced reaction stops heating, is cooled to room temperature.
Step 3 is added natrium carbonicum calcinatum, and stirs 4 hours, and desalination is filtered after standing, filtrate decompression is taken off low 170 DEG C,
Continue 2 hours, finally lead to nitrogen, stops heating, takes off low, cooling discharging obtains no-solvent type of the appearance transparent without obvious smell
Release silicone oil, viscosity 480mpa.s.
Embodiment 2
A kind of release silicone oil of solvent-free organic silicon includes following components: 60% four silicon of prestox ring by mass percentage
Oxygen alkane, 20% three (vinyl-dimethyl base siloxy) methyl-monosilanes, 5% concentrated sulfuric acid is as catalyst, 15% anhydrous carbon
Sour sodium is as neutralizer.
A kind of preparation method of the release silicone oil of above-mentioned solvent-free organic silicon, comprising the following steps:
Octamethylcy-clotetrasiloxane and three (vinyl-dimethyl base siloxy) methyl-monosilanes are dosed into reaction kettle by step 1
In be stirred.
Step 2 is added the catalyst concentrated sulfuric acid, and be warming up to 80 DEG C, stirs 6 hours under constant temperature under the conditions of nitrogen protection
Then balanced reaction stops heating, is cooled to room temperature.
Step 3 is added natrium carbonicum calcinatum, and stirs 4 hours, and desalination is filtered after standing, filtrate decompression is taken off low 170 DEG C,
Continue 2 hours, finally lead to nitrogen, stops heating, takes off low, cooling discharging obtains no-solvent type of the appearance transparent without obvious smell
Release silicone oil, viscosity 242mpa.s.
Embodiment 3
A kind of release silicone oil of solvent-free organic silicon includes following components: 75% dimethyl siloxane by mass percentage
Mixing ring, 10% three (vinyl-dimethyl base siloxy) methyl-monosilanes, 5% trifluoromethanesulfonic acid is as catalyst, and 10%
Carbon Dioxide calcium is as neutralizer.
A kind of preparation method of the release silicone oil of above-mentioned solvent-free organic silicon, comprising the following steps:
Dimethyl siloxane mixing ring is dosed into and is reacted with three (vinyl-dimethyl base siloxy) methyl-monosilanes by step 1
It is stirred in kettle.
Step 2 is added the catalyst concentrated sulfuric acid, and be warming up to 65 DEG C, stirs 7 hours under constant temperature under the conditions of nitrogen protection
Then balanced reaction stops heating, is cooled to room temperature.
Step 3 is added natrium carbonicum calcinatum, and stirs 4 hours, and desalination is filtered after standing, filtrate decompression is taken off low 170 DEG C,
Continue 2 hours, finally lead to nitrogen, stops heating, takes off low, cooling discharging obtains no-solvent type of the appearance transparent without obvious smell
Release silicone oil, viscosity 350mpa.s.
Contrast on effect test:
As a comparison by the release silicone oil of commercially available solvent type (specially DOW CORNING model are as follows: 7458 mould release), with reality
The release silicone oil of no-solvent type for applying a 1-3 is solidificated in PET film in the corresponding auxiliary agent of addition (silicone oil that hydrogen content is 1.6%)
(identical glue thickness, 1.2u) is tested, and properties such as the following table 1 of mould release is specifically measured:
Table 1
The superiority and inferiority judgment criteria of performance are as follows: the off-type force after aging surveys the high-quality of off-type force close to vertical, and remaining rate most connects
Nearly 100% is high-quality.That is the quality of the release silicone oil of the more commercially available solvent type of the release silicone oil of the no-solvent type of embodiment 1-3
Good, remaining rate is high, can remove easily.
It is that above-mentioned preferred embodiment should be regarded as application scheme embodiment for example, all with application scheme thunder
Same, approximate or technology deduction, replacement, improvement for making based on this etc., are regarded as the protection scope of this patent.
Claims (6)
1. a kind of release silicone oil of solvent-free organic silicon, which is characterized in that by mass percentage include following components: 60%-85%
Octamethylcy-clotetrasiloxane or dimethyl siloxane mixing ring, three (vinyl-dimethyl base siloxy) methyl silicon of 5%-20%
Alkane, the strong acid of 2%-5% is as catalyst, the neutralizer of 5%-15%.
2. the release silicone oil of solvent-free organic silicon according to claim 1, which is characterized in that the strong acid is the concentrated sulfuric acid or three
Fluorine methanesulfonic acid.
3. the release silicone oil of solvent-free organic silicon according to claim 1, which is characterized in that the neutralizer is Carbon Dioxide
Sodium or Carbon Dioxide calcium.
4. the release silicone oil of solvent-free organic silicon according to claim 1-3, which is characterized in that viscosity is
230mpa.s-500mpa.s。
5. a kind of preparation method of the release silicone oil of described in any item solvent-free organic silicons of claim 1-4, which is characterized in that packet
Include following steps:
Step 1, by octamethylcy-clotetrasiloxane or dimethyl siloxane mixing ring and three (vinyl-dimethyl base siloxy) methyl
Silane is dosed into reaction kettle and is stirred；
Under the conditions of nitrogen protection strong acid catalyst is added, and be warming up to 60 DEG C~90 DEG C in step 2, and it is small that 5-7 is stirred under constant temperature
When balanced reaction, then stop heating, be cooled to room temperature；
Step 3 is added natrium carbonicum calcinatum, and stirs 3-5 hours, desalination is filtered after standing, filtrate decompression is taken off low, finally leads to
Nitrogen stops heating, takes off low, and cooling discharging obtains the release silicone oil of no-solvent type of the appearance transparent without obvious smell.
6. the preparation method of the release silicone oil of solvent-free organic silicon according to claim 5, which is characterized in that described in step 3
Decompression take off low condition be 170 DEG C, continue 1.5-2.5 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811587816.3A CN109679496A (en) | 2018-12-25 | 2018-12-25 | Release silicone oil of solvent-free organic silicon and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811587816.3A CN109679496A (en) | 2018-12-25 | 2018-12-25 | Release silicone oil of solvent-free organic silicon and preparation method thereof |
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| CN109679496A true CN109679496A (en) | 2019-04-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811587816.3A Pending CN109679496A (en) | 2018-12-25 | 2018-12-25 | Release silicone oil of solvent-free organic silicon and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444449A (en) * | 2021-07-15 | 2021-09-28 | 惠州市永卓科技有限公司 | Ultraviolet-cured solvent-free release silicone oil and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0842996A1 (en) * | 1996-11-14 | 1998-05-20 | Dow Corning Toray Silicone Company, Ltd. | Solventless silicone release coatings |
| CN101260240A (en) * | 2007-03-05 | 2008-09-10 | 信越化学工业株式会社 | Solvent-free siloxane release agent composition for thin film and stripping thin film using the same |
| CN103351812A (en) * | 2013-07-17 | 2013-10-16 | 浙江池河科技有限公司 | Water-based mold release and preparation method thereof and release paper prepared by utilizing water-based mold release |
| CN104704071A (en) * | 2012-10-09 | 2015-06-10 | 道康宁东丽株式会社 | Releasing laminate and production method thereof |
| CN108130001A (en) * | 2017-12-20 | 2018-06-08 | 中科院广州化学有限公司 | A kind of room temperature rapid curing silicone release agent and preparation method thereof |
| CN108219142A (en) * | 2016-12-14 | 2018-06-29 | 上海飞凯光电材料股份有限公司 | Organic siliconresin and preparation method thereof, application |
-
2018
- 2018-12-25 CN CN201811587816.3A patent/CN109679496A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0842996A1 (en) * | 1996-11-14 | 1998-05-20 | Dow Corning Toray Silicone Company, Ltd. | Solventless silicone release coatings |
| CN101260240A (en) * | 2007-03-05 | 2008-09-10 | 信越化学工业株式会社 | Solvent-free siloxane release agent composition for thin film and stripping thin film using the same |
| CN104704071A (en) * | 2012-10-09 | 2015-06-10 | 道康宁东丽株式会社 | Releasing laminate and production method thereof |
| CN103351812A (en) * | 2013-07-17 | 2013-10-16 | 浙江池河科技有限公司 | Water-based mold release and preparation method thereof and release paper prepared by utilizing water-based mold release |
| CN108219142A (en) * | 2016-12-14 | 2018-06-29 | 上海飞凯光电材料股份有限公司 | Organic siliconresin and preparation method thereof, application |
| CN108130001A (en) * | 2017-12-20 | 2018-06-08 | 中科院广州化学有限公司 | A kind of room temperature rapid curing silicone release agent and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113444449A (en) * | 2021-07-15 | 2021-09-28 | 惠州市永卓科技有限公司 | Ultraviolet-cured solvent-free release silicone oil and preparation method thereof |
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Application publication date: 20190426 |