CN100465242C - Low-superficial area ratio marine antifouling coating of silicofluoride block polymer and its production - Google Patents
Low-superficial area ratio marine antifouling coating of silicofluoride block polymer and its production Download PDFInfo
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- CN100465242C CN100465242C CNB2007100087556A CN200710008755A CN100465242C CN 100465242 C CN100465242 C CN 100465242C CN B2007100087556 A CNB2007100087556 A CN B2007100087556A CN 200710008755 A CN200710008755 A CN 200710008755A CN 100465242 C CN100465242 C CN 100465242C
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Abstract
A fluosilicate block polymer low-surface energy marine anti-fouling coating and its production are disclosed. The coating consists of base material polydimethyl siloxane-b-polymethylmethacrylate-b-polyfluobutyl metacrylic acid ester ternary fluosilicate block copolymer, accessory methyl silicone oil and di-n-octyl ester phthalate and coating solvent butyrin acetate. The process is carried out by mixing methyl silicone oil with di-n-octyl ester phthalate to obtain coating accessory, mixing polydimethyl siloxane-b-polymethylmethacrylate-b-polyfluobutyl metacrylic acid ester ternary fluosilicate block copolymer with pigment to obtain coating base material and pigment mixture, adding coating accessory into mixture of coating base material and pigment, mixing, dissolving it into butyrin acetate and laying aside. It has excellent anti-fouling effect and no environmental pollution.
Description
Technical field
The present invention relates to a kind of marine antifouling coating, especially relate to a kind ofly, and carry out composite marine antifouling coating that is prepared into a kind of utmost point low surface energy and preparation method thereof with other component with fluorine silicon block polymer making coatings base-material.
Background technology
Ship and oceanographic equipment all can face the challenge of marine biofouling, and the loss that biodeterioration caused that the marine organisms of numerous kinds and quantity cause is difficult to estimation.For reducing even eliminate the biodeterioration of oceanographic equipment, common way is to smear marine antifouling coating on oceanographic equipment.
Up to now, according to whether containing toxic agent and the existing marine antifouling coating of antifouling mechanism can be divided into two classes: traditional marine antifouling coating and environmentally friendly marine antifouling coating.The former kills attached to the marine organisms on the equipment by the toxic agent in the release coatings, realizes marine anti-pollution, and this class coating also causes the pollution of ocean environment in antifouling; The latter or only kill attached to the marine organisms on the equipment, and the chemical substance of no pollution of the sea itself by discharging, or owing in the coating low surface energy of containing material is arranged, thereby marine organisms can't stick to coating surface realization marine anti-pollution.The development trend of marine antifouling coating is the exploitation low surface energy antifouling coating for seas at present.This coating is brought into play antifouling effect based on the low surface energy characteristic of (coating) base-material, has lower surface energy, marine organisms are difficult to adhere to or adhere to not firm, when ship's navigation, settled organism is removed, or utilize special cleaning equipment at an easy rate settled organism to be removed, thereby reach antifouling purpose.
Over nearly 20 years, numerous investigators are devoted to develop the low surface energy good marine antifouling coating of anti-fouling effect of holding concurrently.Research and development focus on the selection and the preparation of paint binder, and the base-material that oneself studied has 100 kinds at least, and the material that relates to mainly is organosilicon and organic fluorine two classes.Existing certain breakthrough aspect research of low surface energy antifouling coating for seas base-material and selection at present.As publication number is that the Chinese patent of CN1097447 has been invented a kind of nontoxic low surface energy antifouling coating for seas, is coated on the bottom, naval vessel and can prevents halobiontic stained.The two components of base-material system of this coating, base-material is selected polydimethylsiloxane and Resins, epoxy for use.Though this coating has antifouling environment protecting to a certain degree, effect obviously descends this coating uses certain hour under ocean environment after.Up-to-date low surface energy anti-fouling paint is fluoro polysiloxane coating materials (referring to a U.S. Pat 6265515), and its base-material structure is the linear polysiloxanes that has fluorine carbon side group, has linear polysiloxanes snappiness and high workability and CF concurrently
3The ultra-low surface energy characteristic of group can be used for harbour, buoy, fishing net, boats and ships and the sea soiling protective of basin etc. down.Have silicon and fluorine concurrently in this class paint binder elementary composition, have very low surface energy, anti-fouling effect is also better, but still is difficult to reach industrial requirements duration of service.
Summary of the invention
The object of the present invention is to provide a kind of can keep the feature of environmental protection, economy and anti-fouling effect high and can use lastingly make the Fluoro-silicone block copolymer-type low surface energy marine antifouling coating and its preparation method of the utmost point low surface energy of base-material with a class new multicomponent fluorine silicon block polymer.
Fluorine silicon block polymer type low surface energy antifouling coating for seas of the present invention forms by base-material, pigment, auxiliary agent and paint solvent are composite, base-material is the poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-, auxiliary agent is methyl-silicone oil and dinoctyl phthalate, and paint solvent is a N-BUTYL ACETATE.Press quality than the poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-, pigment, methyl-silicone oil, the proportioning of dinoctyl phthalate and N-BUTYL ACETATE is: polydimethylsiloxane-b-polymethylmethacrylate-b-gathers seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers: pigment: methyl-silicone oil: dinoctyl phthalate: N-BUTYL ACETATE=1:(0.1～0.6): (0.02～0.1): (0.02～0.1): (0.2～0.8).
Pigment is selected diarylide yellow or phthalocyanine green for use.
The preparation method of fluorine silicon block polymer type low surface energy antifouling coating for seas of the present invention may further comprise the steps:
1) methyl-silicone oil is mixed with dinoctyl phthalate coatings additive(s);
2) the poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-are mixed with pigment the mixture of paint binder and pigment;
3) coatings additive(s) that step 1) is obtained is added to by step 2) mix to such an extent that mixture is standby in the paint binder that obtains and the mixture of pigment;
4) mixture that step 3) is obtained is dissolved in the N-BUTYL ACETATE solvent and is prepared into mixture;
5) after the mixture that step 4) is obtained leaves standstill, get fluorine silicon block polymer type low surface energy antifouling coating for seas.
Methyl-silicone oil and dinoctyl phthalate blended temperature are preferably 25～30 ℃.Poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-and pigment blended temperature are preferably 25～35 ℃.The coatings additive(s) that step 1) is obtained is added to by step 2) temperature of mixing the mixture of gained in the paint binder that obtains and the mixture of pigment remains on 25～35 ℃.The coatings additive(s) that step 1) is obtained is added drop-wise to by step 2) to mix the time of stirring in the paint binder that obtains and the mixture of pigment and be preferably 1～2h, stirring velocity is preferably 400～600rpm/min.The mixture that step 3) is obtained is dissolved in the temperature that is prepared into mixture in the N-BUTYL ACETATE solvent and is preferably in 25～35 ℃ and stirs 1～2h down, and stirring velocity is 400～600rpm/min; The time that the mixture that step 4) obtains leaves standstill is preferably 4～6h.
Compare with existing marine antifouling coating, the beneficial effect that the present invention has is that the present invention is a base-material with the poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-, with regard to this polymer base material: (1) main polymer chain has the silica block, the side chain of another block contains the fluoro unit, has ultra-low surface energy.(2) PDMS in the polymkeric substance and PHFBMA segment objectionable intermingling can form micro phase separation structure.(3) the PDMS block guarantees that polymer chain has the height kindliness in the polymkeric substance, than lower glass transition temperatures with than small elastic modulus; The PHFBMA block guarantees that then it has low surface energy, improves the good solubility-resistence energy, improves surface property; The consistency of PMMA block and priming paint makes it that enough bounding forces be arranged.(4) under the polymericular weight same case, the needed fluorochemical monomer of preparation ternary block polymer reduces a lot than the required fluorochemical monomer of preparation binary segmented copolymer, and the fluorochemical monomer expense is a major portion in the cost, thereby the polymkeric substance cost reduces greatly.The above characteristics of base-material material make not only environmental protection of marine antifouling coating, the good economy performance that is re-dubbed, and good antifouling effect and stable, long service life, concrete work-ing life is different because of the difference of ocean environment, but obviously is better than the marine antifouling coating mentioned in the background technology.Through the test, its antifouling phase is long, can reach 2 years, and its anti-fouling effect can with the same period poisonous coating identical or close.In addition, the dissolution rate of material in seawater is controlled in the coating, through showing at Chinese Xiamen sea area, Meizhou Bay marine site link plate and patch test of paints on ship hull, uses good reproducibility in the seawater of different quality, and anti-fouling effect is stable.(5) coating that the present invention relates to can be widely used in oceanographic equipment, as the anti-marine biofouling of marine vessel, submerged pipeline etc.
The marine antifouling coating that the present invention relates to is as shown in table 1 in different waters application testing data.
Table 1
| Coating (water) contact angle/℃ | The navigation marine site | Coated area/m 2 | Marine life adheres to fraction of coverage |
| 130 | Xiamen sea area | 8 | Do not see that marine life adheres to (1 year) |
| 134 | The Meizhou Bay marine site | 5 | Do not see that marine life adheres to (1 year) |
Embodiment
The present invention is further illustrated by the following examples.
Embodiment 1
1) 0.3 part of methyl-silicone oil and 0.6 part of dinoctyl phthalate are mixed under 25 ℃ is prepared into coatings additive(s);
2) 10 parts of ternary fluorosilicic block copolymers and 2 parts of diarylide yellows are mixed under 25 ℃ be prepared into coatings additive(s); 10 parts of ternary fluorosilicic block copolymers and 2 parts of diarylide yellows are mixed the mixture that is prepared into base-material and pigment in 25 ℃;
3) coatings additive(s) that step 1) is obtained is added drop-wise to by step 2) mix in the paint binder that obtains and the mixture of pigment and stir 1h, the mixing process mixture temperature remains on 25 ℃, and stirring velocity is controlled at 400rpm/min, and the gained mixture is standby;
4) mixture that step 3) is obtained is dissolved in 4 parts the N-BUTYL ACETATE solvent and is prepared into mixture, stirs 1h down at 25 ℃ then, and stirring velocity is controlled at 400rpm/min;
5) after the mixture that step 4) is obtained leaves standstill 4h, the novel sea antifouling paint that must the present invention relates to.
Embodiment 2
1) 0.4 part of methyl-silicone oil and 0.7 part of dinoctyl phthalate are mixed in 27 times is prepared into coatings additive(s);
2) 10 parts of ternary fluorosilicic block copolymers and 2.5 parts of diarylide yellows are mixed the mixture that is prepared into paint binder and pigment in 27 ℃;
3) coatings additive(s) that step 1) is obtained is added drop-wise to by step 2) to mix in the paint binder that obtains and the mixture of pigment and stir 1.5h, the mixing process temperature remains on 27 ℃, and stirring velocity is controlled at 500rpm/min, and the gained mixture is standby;
4) mixture that step 3) is obtained is dissolved in 5 parts the N-BUTYL ACETATE solvent and is prepared into mixture, stirs 1h down at 27 ℃ then, and stirring velocity is controlled at 500rpm/min;
5) after the mixture that step 4) is obtained leaves standstill 5h, the novel sea antifouling paint that must the present invention relates to.
Embodiment 3
1) 0.55 part of methyl-silicone oil and 0.55 part of dinoctyl phthalate are mixed under 29 ℃ is prepared into coatings additive(s);
2) 10 parts of ternary fluorosilicic block copolymers and 3 parts of diarylide yellows are mixed the mixture that is prepared into paint binder and pigment in 29 ℃;
3) coatings additive(s) that step 1) is obtained is added drop-wise to by step 2) mix in the paint binder that obtains and the mixture of pigment and stir 1h, the mixing process mixture temperature remains on 29 ℃, and stirring velocity is controlled at 400rpm/min, and the gained mixture is standby;
4) mixture that step 3) is obtained is dissolved in 4 parts the N-BUTYL ACETATE solvent and is prepared into mixture, stirs 1.5h down at 29 ℃ then, and stirring velocity is controlled at 500rpm/min;
5) after the mixture that step 4) is obtained leaves standstill 4.5h, the novel sea antifouling paint that must the present invention relates to.
Embodiment 4
1) 0.7 part of methyl-silicone oil and 0.45 part of dinoctyl phthalate are mixed under 31 ℃ is prepared into coatings additive(s);
2) 10 parts of ternary fluorosilicic block copolymers and 4.5 parts of diarylide yellows are mixed the mixture that is prepared into paint binder and pigment in 28 ℃;
3) coatings additive(s) that step 1) is obtained is added drop-wise to by step 2) mix in the paint binder that obtains and the mixture of pigment and stir 1.5h, the mixing process mixture temperature remains on 31 ℃, and stirring velocity is controlled at 500rpm/min, and the gained mixture is standby;
4) mixture that step 3) is obtained is dissolved in 3.5 parts of N-BUTYL ACETATE solvents and is prepared into mixture, stirs 1.5h down at 31 ℃ then, and stirring velocity is controlled at 500rpm/min;
5) after the mixture that step 4) is obtained leaves standstill 5h, the novel sea antifouling paint that must the present invention relates to.
Embodiment 5
1) 0.85 part of methyl-silicone oil and 0.35 part of dinoctyl phthalate are mixed under 33 ℃ is prepared into coatings additive(s);
2) 10 parts of ternary fluorosilicic block copolymers and 5 parts of phthalocyanine greens are mixed the mixture that is prepared into paint binder and pigment in 33 ℃;
3) coatings additive(s) that step 1) is obtained is added drop-wise to by step 2) mix in the paint binder that obtains and the mixture of pigment and stir 2h, the mixing process mixture temperature remains on 33 ℃, and stirring velocity is controlled at 550rpm/min, and the gained mixture is standby;
4) mixture that step 3) is obtained is dissolved in 7 parts of N-BUTYL ACETATE solvents and is prepared into mixture, stirs 1.5h down at 33 ℃ then, and stirring velocity is controlled at 550rpm/min;
5) after the mixture that step 4) is obtained leaves standstill 5h, the novel sea antifouling paint that must the present invention relates to.
Embodiment 6
1) 0.9 part of methyl-silicone oil and 1 part of dinoctyl phthalate are mixed under 34 ℃ is prepared into coatings additive(s);
2) 10 parts of ternary fluorosilicic block copolymers and 5.5 parts of phthalocyanine greens are mixed the mixture that is prepared into paint binder and pigment in 34 ℃;
3) coatings additive(s) that step 1) is obtained is added drop-wise to by step 2) mix in the paint binder that obtains and the mixture of pigment and stir 2h, the mixing process mixture temperature remains on 34 ℃, and stirring velocity is controlled at 600rpm/min, and the gained mixture is standby;
4) mixture that step 3) is obtained is dissolved in 7 parts of N-BUTYL ACETATE solvents and is prepared into mixture, stirs 1.5h down at 34 ℃ then, and stirring velocity is controlled at 600rpm/min;
5) after the mixture that step 4) is obtained leaves standstill 5h, the novel sea antifouling paint that must the present invention relates to.
Embodiment 7
1) 1 part of methyl-silicone oil and 1 part of dinoctyl phthalate are mixed under 35 ℃ is prepared into coatings additive(s);
2) 10 parts of ternary fluorosilicic block copolymers and 5 parts of phthalocyanine greens are mixed the mixture that is prepared into paint binder and pigment in 35 ℃;
3) coatings additive(s) that step 1) is obtained is added drop-wise to by step 2) mix in the paint binder that obtains and the mixture of pigment and stir 2h, the mixing process mixture temperature remains on 35 ℃, and stirring velocity is controlled at 600rpm/min, and the gained mixture is standby;
4) mixture that step 3) is obtained is dissolved in 7 parts of N-BUTYL ACETATE solvents and is prepared into mixture, stirs 1.5h down at 31 ℃ then, and stirring velocity is controlled at 600rpm/min;
5) after the mixture that step 4) is obtained leaves standstill 5h, the novel sea antifouling paint that must the present invention relates to.
Fluorine silicon block polymer type low surface energy antifouling coating for seas of the present invention need check before use whether precipitation of solid material or other obvious foreign matter are arranged, if can not spray or brush.When the brushing of fluorine silicon block polymer type low surface energy antifouling coating for seas is being had the A of rust-inhibiting paint
SIn the time of on the steel plate, the thickness of rust-inhibiting paint dry film should be in 180～220 mu m ranges.
When using silicon block polymer type low surface energy antifouling coating for seas to brush, can adopt following method.
1) spraying: under 0.25～0.5Mpa pressure, spray gun and object are maintained on the horizontal throw, coating is sprayed in the rust-inhibiting paint surface;
2) brush: available painting brush is by about the elder generation, and the direction about the back is brushed;
3) coat-thickness that the present invention relates to coating preferably is controlled at 120～160 μ m.
Claims (9)
1. fluorine silicon block polymer type low surface energy antifouling coating for seas, it is characterized in that forming by base-material, pigment, auxiliary agent and paint solvent are composite, base-material is the poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-, auxiliary agent is methyl-silicone oil and dinoctyl phthalate, and paint solvent is a N-BUTYL ACETATE; Press quality than the poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-, pigment, methyl-silicone oil, the proportioning of dinoctyl phthalate and N-BUTYL ACETATE is: polydimethylsiloxane-b-polymethylmethacrylate-b-gathers seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers: pigment: methyl-silicone oil: dinoctyl phthalate: N-BUTYL ACETATE=1: 0.1～0.6: 0.02～0.1: 0.02～0.1: 0.2～0.8.
2. fluorine silicon block polymer type low surface energy antifouling coating for seas as claimed in claim 1 is characterized in that pigment is diarylide yellow or phthalocyanine green.
3. the preparation method of fluorine silicon block polymer type low surface energy antifouling coating for seas as claimed in claim 1 is characterized in that may further comprise the steps:
1) methyl-silicone oil is mixed with dinoctyl phthalate coatings additive(s);
2) the poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-are mixed with pigment the mixture of paint binder and pigment;
3) coatings additive(s) that step 1) is obtained is added to by step 2) mix to such an extent that mixture is standby in the paint binder that obtains and the mixture of pigment;
4) mixture that step 3) is obtained is dissolved in the N-BUTYL ACETATE solvent and is prepared into mixture;
5) after the mixture that step 4) is obtained leaves standstill, get fluorine silicon block polymer type low surface energy antifouling coating for seas.
4. the preparation method of fluorine silicon block polymer type low surface energy antifouling coating for seas as claimed in claim 3 is characterized in that methyl-silicone oil and dinoctyl phthalate blended temperature are 25～30 ℃.
5. the preparation method of fluorine silicon block polymer type low surface energy antifouling coating for seas as claimed in claim 3 is characterized in that with poly-seven fluorine butyl methyl acrylic ester ternary fluorosilicic block copolymers of polydimethylsiloxane-b-polymethylmethacrylate-b-and pigment blended temperature be 25～35 ℃.
6. the preparation method of fluorine silicon block polymer type low surface energy antifouling coating for seas as claimed in claim 3 is characterized in that the coatings additive(s) that step 1) obtains is added to by step 2) temperature of mixing the mixture of gained in the paint binder that obtains and the mixture of pigment remains on 25～35 ℃.
7. the preparation method of fluorine silicon block polymer type low surface energy antifouling coating for seas as claimed in claim 3, it is characterized in that the coatings additive(s) that step 1) obtains is added drop-wise to by step 2) to mix the time of stirring in the paint binder that obtains and the mixture of pigment be 1～2h, stirring velocity is 400～600rpm/min.
8. the preparation method of fluorine silicon block polymer type low surface energy antifouling coating for seas as claimed in claim 3, it is characterized in that the mixture that step 3) obtains is dissolved in the temperature that is prepared into mixture in the N-BUTYL ACETATE solvent stirs 1～2h down at 25～35 ℃, stirring velocity is 400～600rpm/min.
9. the preparation method of fluorine silicon block polymer type low surface energy antifouling coating for seas as claimed in claim 3 is characterized in that the time that mixture that step 4) obtains leaves standstill is 4～6h.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100087556A CN100465242C (en) | 2007-03-27 | 2007-03-27 | Low-superficial area ratio marine antifouling coating of silicofluoride block polymer and its production |
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| CNB2007100087556A CN100465242C (en) | 2007-03-27 | 2007-03-27 | Low-superficial area ratio marine antifouling coating of silicofluoride block polymer and its production |
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| CN100465242C true CN100465242C (en) | 2009-03-04 |
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| CN100532478C (en) * | 2007-09-29 | 2009-08-26 | 中国科学院广州化学研究所 | Composite coating containing fluorine-containing acrylic ester block copolymer and producing method thereof |
| CN101215364B (en) * | 2008-01-08 | 2010-06-30 | 厦门大学 | Fluorine silicon tri-block copolymers and preparation method thereof |
| CN101215362B (en) * | 2008-01-08 | 2010-08-25 | 厦门大学 | Silicon-acrylic tri-block copolymer with low surface energy and preparing method thereof |
| KR101406645B1 (en) * | 2009-10-13 | 2014-06-11 | 닛뽄 페인트 마린 가부시키가이샤 | Antifouling coating composition, antifouling film, composite film, and in-water structure |
| CN101710112B (en) * | 2009-12-01 | 2014-02-05 | 大连海洋大学 | Device for testing marine anti-pollution materials |
| CN102040900B (en) * | 2010-11-11 | 2014-04-30 | 常州大学 | Fluorocoating resin and preparation method thereof |
| CN102220080B (en) * | 2011-05-31 | 2013-10-16 | 浙江大学 | Quaternary ammonium salt modified organosilicon polyurethane ocean antifouling paint and preparation method and application thereof |
| CN102212306B (en) * | 2011-05-31 | 2013-05-08 | 浙江大学 | Organosilicon type marine antifouling paint binder and preparation method and application thereof |
| CN103483966B (en) * | 2013-09-17 | 2016-11-16 | 三棵树涂料股份有限公司 | The preparation method of antifouling automatically cleaning building external paint based on fluorine silicon block polymer |
| CN103694839B (en) * | 2013-12-16 | 2015-09-16 | 浙江大学 | The preparation method of a kind of antimicrobial form low surface energy modified polyurethane antifouling coating agent |
| CN104513340B (en) * | 2015-02-06 | 2016-08-17 | 中国船舶重工集团公司第七二五研究所 | A kind of fluorine silica acrylic acid is from polishing antifouling resin and preparation method thereof |
| CN105061770B (en) * | 2015-08-10 | 2017-08-04 | 广东博兴新材料科技有限公司 | A kind of organic fluorinated silicone light-cured resin and its preparation method and application |
| CN111234694B (en) * | 2020-03-16 | 2021-07-27 | 中国船舶重工集团公司第七二五研究所 | Antifouling material and preparation method thereof |
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