CN106220855A - A kind of synthetic method of acrylate modified fluorine silicon coating - Google Patents
A kind of synthetic method of acrylate modified fluorine silicon coating Download PDFInfo
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- CN106220855A CN106220855A CN201610768831.2A CN201610768831A CN106220855A CN 106220855 A CN106220855 A CN 106220855A CN 201610768831 A CN201610768831 A CN 201610768831A CN 106220855 A CN106220855 A CN 106220855A
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- Prior art keywords
- synthetic method
- acid
- acrylate
- fluorine silicon
- modified fluorine
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/24—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen halogen-containing groups
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention relates to the synthetic method of a kind of acrylate modified fluorine silicon coating, synthesis step includes: add a certain amount of acid in reaction bulb or alkali, polymerization inhibitor and flucride siloxane are sufficiently stirred for, then heat to 60 90 DEG C, start to drip acrylate slowly, 4 6h it are incubated after being added dropwise to complete, lower the temperature, be washed to PH=6 7, obtain acrylate modified fluorine silicon coating.The synthetic method of the present invention has the features such as cementability is high, reaction condition is gentle, controllability is strong, yield is high in experiment, environmentally friendly.
Description
Technical field
The present invention relates to the synthetic method of acrylate modified fluorine silicon coating, belong to synthesis chemical field.
Background technology
Low-surface-energy anticorrosion and antifouling functional coating is applicable to metal, pottery, cement, plastics, glass, fiberglass, timber etc.
The goods of various material and the surfacecti proteon of engineering and decoration.Can be used as metal anti-corrosive paint, building coating, plastic paint, wood
The electronic products such as device coating, car paint, offshore platform coating, ship hull coating material, appliance finishes, kitchen kitchen tools coating and mobile phone
Screen waterproof and oilproof, the waterproof and oilproof etc. of historical relic.
Low-surface-energy anticorrosion and antifouling functional paint is usually by alkenes fluoropolymer monomer, fluorinated acrylate and organosilicon
Monomer copolymerization prepares low-surface-energy macromolecule resin, then with the low-surface-energy macromolecule resin of this fluorine silicon, novel nano
The materials such as material, filler and functional aid are manufactured through special process and nanotechnology.
Existing fluorine silicon coating there is the defects such as cementability is low, hardness is little, anti-fouling effect is poor, limit fluorine silicon coating
Application.
Summary of the invention
For the deficiencies in the prior art, the present invention provides that a kind of cementability is high, reaction condition is gentle, experiment controllability is strong,
The synthetic method of the acrylate modified fluorine silicon coating that yield is high, environmentally friendly.
Technical scheme is as follows:
The synthetic method of a kind of acrylic acid modified fluorine silicon coating: add a certain amount of acid or alkali, polymerization inhibitor in reaction bulb
It is sufficiently stirred for flucride siloxane, then heats to 60-90 DEG C, start to drip acrylate slowly, be incubated after being added dropwise to complete
4-6h, lowers the temperature, is washed to PH=6-7, obtains acrylate modified fluorine silicon coating.
Wherein acid or the 0.5%-2% that quality is reactant gross mass of alkali；The quality of polymerization inhibitor is reactant gross mass
0.4%-1%；Acrylate is 1:1 3:1 with the mol ratio of flucride siloxane.
According to currently preferred, acid is in sulphuric acid, hydrochloric acid, phosphoric acid, trifluoromethane sulfonic acid, acid cation exchange resin
One；Alkali is the one in potassium hydroxide, sodium hydroxide, potassium ethoxide, Sodium ethylate；
According to currently preferred, described flucride siloxane is perfluoro capryl triethoxysilane, perfluoro capryl trimethoxy
Base silane, perfluoro decyl trimethoxy silane, perfluoro decyl triethoxysilane and 4-methyl-(perfluoro hexyl ethyl) propyl group three
One in methoxy silane；
According to currently preferred, described acrylate is caprolactone and pentaerythritol triacrylate；
According to currently preferred, polymerization inhibitor is MEHQ；
According to currently preferred, described reaction temperature is 60-90 DEG C；
According to currently preferred, described acrylate is 1:1 3:1 with the mol ratio of flucride siloxane.
Acrylic acid modified fluorine silicon coating prepared by the present invention be mainly used in the electronic products such as mobile phone screen waterproof and oilproof,
The waterproof and oilproof of historical relic.
The method of the present invention has that cementability is high, reaction condition gentle, controllability is strong, yield is high in experiment, environmentally friendly
Etc. feature.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but is not limited to this.
Embodiment 1
0.45g concentrated sulphuric acid, 0.23g MEHQ and 28.40g perfluoro decyl trimethoxy silicon is added in reaction bulb
Alkane is sufficiently stirred for, and then heats up 60 DEG C, starts dropping 16.50g pentaerythritol triacrylate slowly, heats up after being added dropwise to complete
To 80 DEG C of insulation 5h, lower the temperature, be washed to PH=7, obtain acrylate modified fluorine silicon coating.
Embodiment 2
0.45g concentrated sulphuric acid, 0.23g MEHQ and 28.40g perfluoro decyl trimethoxy silicon is added in reaction bulb
Alkane is sufficiently stirred for, and then heats up 60 DEG C, starts dropping 33.00g pentaerythritol triacrylate slowly, heats up after being added dropwise to complete
To 80 DEG C of insulation 5h, lower the temperature, be washed to PH=7, obtain acrylate modified fluorine silicon coating.
Embodiment 3
0.45g concentrated sulphuric acid, 0.46g MEHQ and 25.52g perfluoro capryl triethoxysilicane is added in reaction bulb
Alkane is sufficiently stirred for, and then heats up 70 DEG C, starts dropping 33.00g pentaerythritol triacrylate slowly, heats up after being added dropwise to complete
To 80 DEG C of insulation 5h, lower the temperature, be washed to PH=7, obtain acrylate modified fluorine silicon coating.
Embodiment 4
0.45gKOH, 0.46g MEHQ and 25.52g perfluoro capryl triethoxysilane is added in reaction bulb
It is sufficiently stirred for, then heats up 70 DEG C, start dropping 17.20g caprolactone slowly, be added dropwise to complete rear 70 DEG C of insulation 5h,
Lower the temperature, be washed to PH=7, obtain acrylate modified fluorine silicon coating.
Embodiment 5
0.45gKOH, 0.46g MEHQ and 25.52g perfluoro capryl triethoxysilane is added in reaction bulb
It is sufficiently stirred for, then heats up 70 DEG C, start dropping 51.60g caprolactone slowly, be added dropwise to complete rear 70 DEG C of insulation 5h,
Lower the temperature, be washed to PH=7, obtain acrylate modified fluorine silicon coating.
The contact angle of acrylate modified silicon fluoride paint prepared by table 1 embodiment 1-5 and hardness
From the experimental result of embodiment 1-5 it can be seen that the acrylate modified silicon fluoride paint of preparation has dredging of excellence
Water oleophobic property and the hardness of excellence.Along with the growth of carbon fluorine chain in flucride siloxane in acrylate modified silicon fluoride paint, hydrophobic
Oleophobic performance improves；Along with the raising of acrylate molar content, the hardness of acrylate modified silicon fluoride paint raises, hydrophobic thin
Oiliness reduction slightly.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (5)
1. the synthetic method of an acrylate modified fluorine silicon coating, it is characterised in that synthesis step includes: add in reaction bulb
Enter a certain amount of acid or alkali, polymerization inhibitor and flucride siloxane are sufficiently stirred for, then heat to 60-90 DEG C, start to drip slowly
Acrylate, is added dropwise to complete rear insulation reaction 4-6h, lowers the temperature, is washed to PH=6-7, obtains acrylate modified fluorine silicon and is coated with
Layer；
The quality of described acid or alkali is the 0.5%-2% of reactant gross mass；The quality of polymerization inhibitor is reactant gross mass
0.4%-1%；Acrylate is 1:1-3:1 with the mol ratio of flucride siloxane.
Synthetic method the most according to claim 1, it is characterised in that described acid is sulphuric acid, hydrochloric acid, phosphoric acid, trifluoromethyl
One in sulfonic acid, acid cation exchange resin；Described alkali is in potassium hydroxide, sodium hydroxide, potassium ethoxide, Sodium ethylate
Kind.
Synthetic method the most according to claim 1, it is characterised in that described flucride siloxane is perfluoro capryl triethoxy
Silane, perfluoro capryl trimethoxy silane, perfluoro decyl trimethoxy silane, perfluoro decyl triethoxysilane and 4-methyl-
One in (perfluoro hexyl ethyl) propyl trimethoxy silicane.
Synthetic method the most according to claim 1, it is characterised in that described acrylate is caprolactone or season penta
Tetrol triacrylate.
Synthetic method the most according to claim 1, it is characterised in that described polymerization inhibitor is MEHQ.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610768831.2A CN106220855B (en) | 2016-08-30 | 2016-08-30 | A kind of synthetic method of acrylate modified fluorine silicon coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610768831.2A CN106220855B (en) | 2016-08-30 | 2016-08-30 | A kind of synthetic method of acrylate modified fluorine silicon coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106220855A true CN106220855A (en) | 2016-12-14 |
| CN106220855B CN106220855B (en) | 2019-03-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610768831.2A Expired - Fee Related CN106220855B (en) | 2016-08-30 | 2016-08-30 | A kind of synthetic method of acrylate modified fluorine silicon coating |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110952336A (en) * | 2018-09-26 | 2020-04-03 | 上海汽车集团股份有限公司 | Three-proofing finishing agent for fabric, and preparation method and use method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304726A (en) * | 2013-05-28 | 2013-09-18 | 中国船舶重工集团公司第七二五研究所 | Preparation method of side chain grafted fluorine-containing monomer acrylic polymer |
| CN103897586A (en) * | 2012-12-26 | 2014-07-02 | 财团法人工业技术研究院 | Coating composition, method for preparing the same, and film layer formed from the coating composition |
| CN104629620A (en) * | 2015-02-06 | 2015-05-20 | 浙江大学 | Method for preparing superhydrophobic anti-icing paint and coating |
| CN104910779A (en) * | 2015-06-04 | 2015-09-16 | 西安交通大学 | Super-hydrophobic acrylic polyurethane coating and preparation method thereof |
-
2016
- 2016-08-30 CN CN201610768831.2A patent/CN106220855B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103897586A (en) * | 2012-12-26 | 2014-07-02 | 财团法人工业技术研究院 | Coating composition, method for preparing the same, and film layer formed from the coating composition |
| CN103304726A (en) * | 2013-05-28 | 2013-09-18 | 中国船舶重工集团公司第七二五研究所 | Preparation method of side chain grafted fluorine-containing monomer acrylic polymer |
| CN104629620A (en) * | 2015-02-06 | 2015-05-20 | 浙江大学 | Method for preparing superhydrophobic anti-icing paint and coating |
| CN104910779A (en) * | 2015-06-04 | 2015-09-16 | 西安交通大学 | Super-hydrophobic acrylic polyurethane coating and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110952336A (en) * | 2018-09-26 | 2020-04-03 | 上海汽车集团股份有限公司 | Three-proofing finishing agent for fabric, and preparation method and use method thereof |
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| Publication number | Publication date |
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| CN106220855B (en) | 2019-03-29 |
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Effective date of registration: 20190202 Address after: 264006 Kaifeng Road 3-3 Renewable Resource Processing Demonstration Zone, Yantai Development Zone, Shandong Province Applicant after: Yantai Darbond Technology Co., Ltd. Address before: 264000 Yantai Development Zone, Shandong Province, 3-3 Kaifeng Road Resource Regeneration and Processing Demonstration Zone Applicant before: Yantai Debang Advanced Silicon Materials Co.,Ltd. |
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Granted publication date: 20190329 Termination date: 20190830 |