Search Images Maps Play Gmail Drive Calendar Translate More »
Sign in
Screen reader users: click this link for accessible mode. Accessible mode has the same essential features but works better with your reader.

Patents

  1. Advanced Patent Search
Publication numberCN101024743 A
Publication typeApplication
Application numberCN 200710090028
Publication date29 Aug 2007
Filing date26 Mar 2007
Priority date26 Mar 2007
Also published asCN100567233C
Publication number200710090028.9, CN 101024743 A, CN 101024743A, CN 200710090028, CN-A-101024743, CN101024743 A, CN101024743A, CN200710090028, CN200710090028.9
Inventors王贤明, 杨凯, 张燕, 卢伟, 阎永江
Applicant海洋化工研究院
Export CitationBiBTeX, EndNote, RefMan
External Links: SIPO, Espacenet
Preparing for all-fluoroalkyl compound containing active end group and use thereof
CN 101024743 A
Abstract
The invention relates to a perfluoroalkyl group compound that is compounded from perfluoroalkyl group monomer A with hydroxyl and diisocyanate B under the existing of solvent and catalyst. It could be used on the hull of ship and submarine to have anti-drag and antifouling effect, used on the engine of craft to have waterproofing and anti-icing effect, etc.
Claims(9)  translated from Chinese
1.一种含活性端基的全氟烷基化合物,其特征在于,由含有羟基的全氟烷基单体A与二异氰酸酯β在溶剂和催化剂存在下合成;所述的A:是具有下面结构的含羟基的全氟烷基单体:CnF2n+1CH2CH2OH式中n=6,8,10;所述的B:是具有下面通式结构的二异氰酸酯:OCN-R-NCO式中R为脂肪、脂环或芳香族的二价基团,包括不少于两个碳的脂肪基团、脂环族基团、单环芳香族基团、稠环芳香族基团以及其他链接基团所连接的非稠环芳香族基团;所述的A和B满足:羟基与异氰酸根比为1∶4;A和B占总投料量的75~90%重量百分比。 A perfluoroalkyl end groups containing an active compound, wherein the perfluoroalkyl group and a hydroxyl group-containing monomer A diisocyanate β in the presence of a solvent and a catalyst under synthesis; wherein the A: having the following hydroxyl group-containing structure of a perfluoroalkyl group-containing monomers: CnF2n + 1CH2CH2OH where n = 6,8,10; said B: having the following general structure diisocyanate: OCN-R-NCO wherein R is a fatty alicyclic or aromatic divalent group, including at least two carbon aliphatic group, an alicyclic group, a monocyclic aromatic group, polycyclic aromatic groups and other groups of the connected links non-condensed polycyclic aromatic group; wherein the A and B satisfy: hydroxyl isocyanate ratio 1:4; A and B from 75 to 90% of the total weight percent of feeding amount.
2.根据权利要求1的含活性端基的全氟烷基化合物,其特征在于,所述的二异氰酸酯是一种或几种组合。 The perfluoroalkyl end groups containing an active compound as claimed in claim 1, characterized in that said diisocyanate is one or more combinations.
3.根据权利要求2的含活性端基的全氟烷基化合物,其特征在于,所述的二异氰酸酯包括:己二异氰酸酯、二甲苯撑二异氰酸酯、异佛尔酮二异氰酸酯、2,2,4-三甲基己烷撑二异氰酸酯、苯二甲撑二异氰酸酯、甲苯环己撑二异氰酸酯、4,4`-双(异氰酸酯环己基)甲烷、2,4`-甲苯二异氰酸酯、4,4`-二苯甲烷二异氰酸酯、3,3`-二甲基二苯基甲烷-4,4`-二异氰酸酯、1,5-萘二异氰酸酯、多次甲基多苯基多异氰酸酯。 3. The perfluoroalkyl group-containing compound reactive end groups according to claim 2, characterized in that said diisocyanate comprises: hexamethylene diisocyanate, xylylene diisocyanate, isophorone diisocyanate, 2,2, 4- trimethyl hexane diisocyanate support, xylylene diisocyanate, toluene cyclohexylene diisocyanate, 4,4'-bis (isocyanate cyclohexyl) methane, 2,4`- toluene diisocyanate, 4,4 `- diphenyl methane diisocyanate, diphenyl dimethyl methane 3,3`- -4,4`- diisocyanate, 1,5-naphthalene diisocyanate, polymethine polyphenyl polyisocyanate.
4.根据权利要求1的含活性端基的全氟烷基化合物,其特征在于,所述的溶剂是酯类或强极性溶剂。 4. The perfluoroalkyl end groups containing an active compound of claim 1, wherein said solvent are esters or strongly polar solvents.
5.根据权利要求4的含活性端基的全氟烷基化合物,其特征在于,所述的溶剂是乙酸乙酯、乙酸丁酯或N-甲基吡咯烷酮、N,N`-二甲基甲酰胺或N,N`-二甲基乙酰胺,选择其中一种或几种;用量是总投料量的10-25%重量百分比。 5. perfluoroalkyl end groups containing an active compound according to claim 4, characterized in that said solvent is ethyl acetate, butyl acetate or N- methylpyrrolidone, N, N`- dimethylformamide amide or N, N`- dimethylacetamide, choose one or more; the amount is 10-25% by weight of the total feeding amount.
6.根据权利要求1的含活性端基的全氟烷基化合物,其特征在于,所述的催化剂是二月桂酸二丁基锡或辛酸亚锡中任选一种,用量是总投料量的0.1-3%重量百分比。 The perfluoroalkyl end groups containing an active compound of claim 1, wherein said catalyst is dibutyl tin dilaurate or stannous octoate optionally an amount of the total feeding amount of 0.1 the percentage of 3% by weight.
7.根据权利要求1的含活性端基的全氟烷基化合物,其特征在于,制备方法是:在惰性气体保护下,将二异氰酸酯在搅拌下溶于有机溶剂体系中,溶解后加入催化剂,分批加入含羟基的全氟烷基单体,反应2-10小时,冷却至室温,得到透明的低粘度溶液。 7. perfluoroalkyl end groups containing an active compound according to claim 1, characterized in that the preparation method is: under the protection of inert gas, the diisocyanate with stirring dissolved in an organic solvent system, the catalyst was added and dissolved, was added portionwise hydroxyl-containing perfluoroalkyl monomer, reaction 2-10 hours, cooled to room temperature, to give a clear solution of low viscosity.
8.一种低表面能涂料组合物,其特征在于,包括如权利要求1的含活性端基的全氟烷基化合物、至少一种含羟基的丙烯酸树脂、适量的稀释剂、颜填料。 A low surface energy coating composition comprising a perfluoroalkyl group-containing compound reactive end groups as claimed in claim 1, at least one hydroxyl group-containing acrylic resin, an appropriate amount of diluents, pigments and fillers.
9.根据权利要求8的低表面能涂料组合物,其特征在于,所述的含活性端基的全氟烷基化合物与含羟基的丙烯酸树脂的比例是1∶5~1∶15。 9. The low surface energy according to claim 8 coating composition, characterized in that the proportion of the perfluoroalkyl group-containing compound reactive with the end groups of the hydroxyl group-containing acrylic resin is 1:5 1:15.
Description  translated from Chinese
含活性端基的全氟烷基化合物的制备及其应用 Preparation and application of perfluoroalkyl compounds containing reactive end groups

技术领域 FIELD

本发明涉及含氟化合物或组合物,其含有至少一个含氟可重复单元和至少一个含氟端基。 The present invention relates to a fluorine-containing compound or composition, which contains at least one fluorine-containing repeatable unit and at least one fluorine-containing terminal group. 本发明同时涉及涂料等方面,其含氟化物组合物可作为涂料组分使用或作为其他活性添加剂使用。 The present invention relates to coatings, etc. Meanwhile, the fluoride-containing composition can be used as a coating or as a component of other reactive additives. 添加或使用该氟化物组合物的制品可具有较低的表面能。 Adding or the fluorochemical composition of the article may have a lower surface energy.

背景技术 BACKGROUND

涂料或活性添加剂主要作用于各种物体表面,起装饰或保护作用。 Paint or active additive major role in a variety of surfaces, decorative or protective effect. 由于长期暴露在外非常容易受到水、灰尘、油污等的污染。 Due to the long exposed very easily contaminated water, dust, oil and the like. 减少污物在物体表面存留或使物体表面更易清洁,就需要涂层表面具有较低的表面张力,提高物体表面的自洁性。 Decrease dirt retention on surfaces or make the surface easier to clean, it is necessary coating surface has low surface tension, improve self-cleaning surface of an object.

在高分子及高分子基材上使用某些氟化物或含氟的组合物,使其具有疏水疏油性等性能,已有广泛的应用。 The use of certain fluoride or fluorine-containing polymer and a polymer on a substrate composition, so as to have a hydrophobic oleophobic properties, has been widely used. 如Banks主编的《有机氟化学品及其工业应用》中所提到的。 Banks such as the editor of the "organic fluorine chemicals and industrial application" as mentioned. Philips,RW和Dettre,RH在1976年就已公开了氟化物片段(J.Col.and Interface Sci.,56(2),1976),根据所公开的资料显示,基本上任何含有CnF2n+1(n≥6)的聚合物、化合物和低聚物都拥有疏水疏油性能。 Philips, RW and Dettre, RH in 1976 already discloses a fluoride fragment (J.Col.and Interface Sci., 56 (2), 1976), based on the information disclosed in the display, basically any material that contains CnF2n + 1 ( n≥6) polymers, compounds and oligomers have hydrophobic and oleophobic properties. 但当n≥8时,某些氟化物或含氟单体呈现固体蜡状性质,较难溶解,利用困难。 But n≥8, some fluoride or a fluorine-containing monomer exhibit solid waxy nature, difficult to dissolve, the use of difficulty.

发明内容 SUMMARY

本发明的目的之一是提供一种含活性端基的全氟烷基化合物,以及制备方法。 One object of the present invention is to provide a perfluoroalkyl compound containing reactive end groups, and the preparation method.

本发明的目的之二是提供包含所述的含活性端基的全氟烷基化合物的低表面能涂料组合物。 Second object of the present invention to provide a low surface comprises a perfluoroalkyl group containing an active compound of the end groups can coating compositions.

本发明的含活性端基的全氟烷基化合物,是含有羟基的全氟烷基单体A与二异氰酸酯B在溶剂和催化剂存在下合成的。 Perfluoroalkyl end groups containing an active compound of the present invention, monomer A is a perfluoroalkyl group with a diisocyanate B having a hydroxy group in the presence of a solvent and a catalyst synthesis.

所述的A:是具有下面结构的含羟基的全氟烷基单体:CnF2n+1CH2CH2OH式中n=6,8,10;所述的B:是具有下面通式结构的二异氰酸酯:OCN-R-NCO式中R为脂肪、脂环或芳香族的二价基团,包括不少于两个碳的脂肪基团、脂环族基团、单环芳香族基团、稠环芳香族基团以及其他连接基团所连接的非稠环芳香族基团。 Said A: having the following structure is a hydroxyl-containing perfluoroalkyl monomers: CnF2n + 1CH2CH2OH where n = 6,8,10; said B: having the following general structure diisocyanate: OCN- R-NCO wherein R is aliphatic, alicyclic or aromatic divalent radical, including not less than two carbons aliphatic group, an alicyclic group, a monocyclic aromatic group, fused ring aromatic group group and other groups connected connected non-condensed polycyclic aromatic groups.

所述的A和B满足:羟基与异氰酸根比为1∶4;A和B占总投料量的75~90%重量百分比。 Said A and B satisfy: hydroxyl isocyanate ratio 1:4; A and B from 75 to 90% of the total weight percent of feeding amount.

所述的二异氰酸酯可以是单一的,也可以是由二种或多种二异氰酸酯组成的混合物。 Said diisocyanate may be a single, or a mixture from two or more diisocyanates thereof.

所述的二异氰酸酯包括:己二异氰酸酯、二甲苯撑二异氰酸酯、异佛尔酮二异氰酸酯、2,2,4-三甲基己烷撑二异氰酸酯、苯二甲撑二异氰酸酯、甲苯环己撑二异氰酸酯、4,4`-双(异氰酸酯环己基)甲烷、2,4`-甲苯二异氰酸酯、4,4`-二苯甲烷二异氰酸酯、3,3`-二甲基二苯基甲烷-4,4`-二异氰酸酯、1,5-萘二异氰酸酯、多次甲基多苯基多异氰酸酯。 Said diisocyanate comprising: hexamethylene diisocyanate, xylylene diisocyanate, isophorone diisocyanate, 2,2,4-trimethyl hexane stays diisocyanate, xylylene diisocyanate, toluene cyclohexylene diisocyanate, 4,4'-bis (isocyanate cyclohexyl) methane, 2,4`- toluene diisocyanate, 4,4'-diphenyl methane diisocyanate, diphenyl dimethyl methane 3,3`- -4 , 4`- diisocyanate, 1,5-naphthalene diisocyanate, polymethine polyphenyl polyisocyanate.

所述的溶剂可以是酯类或强极性溶剂,例如乙酸乙酯、乙酸丁酯或N-甲基吡咯烷酮、N,N`-二甲基甲酰胺或N,N`-二甲基乙酰胺。 The solvent may be an ester or strongly polar solvents, such as ethyl acetate, butyl acetate or N- methylpyrrolidone, N, N`- dimethylformamide or N, N`- dimethylacetamide . 最优选是乙酸乙酯或乙酸丁酯中任选一种或两种混合组成的溶剂。 Most preferably ethyl acetate or butyl acetate, optionally, one or a mixture of two solvents. 用量是总投料量的10-25%重量百分比。 The amount of 10-25% by weight of the total feeding amount.

所述的催化剂是二月桂酸二丁基锡或辛酸亚锡中任选一种。 Said catalyst is dibutyl tin dilaurate or stannous octoate optionally one. 用量是总投料量的0.1-3%重量百分比。 The amount is 0.1-3% by weight of the total feeding amount.

所述的含活性端基的全氟烷基化合物按下述方法制备:在氮气或氩气保护下,将本发明所述的二异氰酸酯在搅拌下溶于有机溶剂体系中。 Perfluoroalkyl-containing compound of the active end groups was prepared as follows: Under a nitrogen or argon atmosphere, the diisocyanate according to the present invention under stirring dissolved in an organic solvent system. 待完全溶解后,加入催化剂。 After the complete dissolution of the catalyst. 在0~25℃下,分批加入含羟基的全氟烷基单体。 At 0 ~ 25 ℃, was added portionwise perfluoroalkyl hydroxyl group-containing monomer. 反应2-8小时,最佳时间为2-6小时;再在60-80℃下,反应2-10小时,最佳时间为4-8小时。 The reaction 2-8 hours, the optimal time is 2-6 hours; then at 60-80 ℃, reaction 2-10 hours, the optimum time is 4-8 hours. 冷却至室温,得到透明的低粘度溶液。 Cooled to room temperature to give a clear solution of low viscosity.

所述的低表面能涂料组合物包括:含活性端基的全氟烷基化合物、至少一种含羟基的丙烯酸树脂(市售产品)、适量的稀释剂、颜填料等。 Low surface energy coating composition comprising: a perfluoroalkyl group-containing compound reactive end groups, at least an acrylic resin hydroxyl group (commercially available product) containing an appropriate amount of diluents, fillers and the like.

所述的含活性端基的全氟烷基化合物与含羟基的丙烯酸树脂的比例是1∶5~1∶15。 Hydroxyl group-containing compound and the ratio of the acrylic resin-containing perfluoroalkyl end groups are active 1:5 ~ 1:15.

所述的稀释剂包括甲苯、二甲苯、丙酮、丁酮中任选一种或两种混合组成的溶剂。 The diluents include toluene, xylene, acetone, butanone optionally mixing one or both of the composition of solvent. 用量是总投料量的10-50%重量百分比。 The amount is 10-50% by weight of the total feeding amount.

所述的颜填料是金红石型钛白粉、滑石粉、云母、漂珠、重质碳酸钙、氧化铁红、氧化锌中任选一种或两种,以及两种以上混合组成。 The pigments and fillers are rutile titanium dioxide, talc, mica, floating beads, heavy calcium carbonate, iron oxide red, zinc oxide, optionally, one or two, as well as a mixture of two or more.

所述的低表面能涂料组合物制备方法:上述物质按照常规制漆方法混合配制,采用刷涂或喷涂等工艺,得到光滑平整的低表面能涂层。 The preparation of low surface energy coating composition: The above material is mixed according to a conventional method of preparation of paints, by brush or spraying techniques, to obtain smooth, low surface energy coating.

所得到的含活性端基的全氟烷基化合物具有下列综合性能:(1)优良的溶解性能,可溶于常见的有机溶剂和极性溶剂。 Perfluoroalkyl end groups containing an active compound obtained has the following overall performance: (1) excellent solubility, soluble in common organic solvents and a polar solvent.

(2)优良的反应性能,化合物一端为全氟烷基结构,另一端为异氰酸酯结构,可保证化合物具有一个活性反应端基。 (2) excellent reactivity, the compound is a perfluoroalkyl group structure at one end, the other end of the isocyanate structure, guarantees a compound having an activated reactive end group.

(3)优越的低表面能,本化合物一端基为全氟链段,该产物与树脂配合后,形成微观“梳”状结构,全氟链段为“梳齿”,可提供优异的疏水性能,水接触角在100以上。 (3) the superior low surface energy, this end of perfluorinated compounds segment, after the product with the resin with the formation of microscopic "comb" -like structure, perfluorinated segments as "comb", can provide excellent hydrophobic properties , water contact angle above 100 .

(4)优越的持久性,该产物与树脂固化后,全氟链段以化学键形式接入树脂,形成支链,可经溶剂擦拭600次后,水接触角基本不变。 (4) excellent durability, the product with the resin after curing, after perfluoro segment access chemically form resin to form a branched, may be solvent wiped 600 times, the water contact angle substantially constant.

本发明得到的含活性端基的全氟烷基化合物与含羟基的丙烯酸树脂配合,可得到具有自清洁、减阻等性能涂层。 Perfluoroalkyl end groups containing an active compound of the present invention is obtained with a hydroxyl-containing acrylic resin complexes, can be obtained having a self-cleaning, and other drag reduction properties of the coating. 在国防、工农业生产和日常生活中有着广泛的应用前景。 Has a broad application prospects in defense, industrial and agricultural production and daily life. 如建筑外墙涂料、减阻防污涂料、防雾防冰涂料等方面有重要的潜在应用。 Such as exterior house paint, drag reduction antifouling paints, coatings and other aspects of anti-fog anti-ice has important potential applications. 此技术用于室外天线上,可防止积雪沉积从而保证通信质量;用在船、潜艇的外壳上,不但减少水的阻力,提高航行速度,还能达到防污的功效;用在石油输送管道内壁能防止黏附、堵塞,减少损耗;用于航空飞行器发动机上,起到防水防冰效果;用在纺织品上,还能制成防水、防污的服装等。 This technique is used for outdoor antenna to prevent snow deposited in order to ensure communication quality; used on boats, submarines shell, not only reduce water resistance, improve navigation speed, but also to achieve the effect of anti-fouling; used in oil pipeline the inner wall to prevent adhesion, congestion, reduce losses; for the aviation aircraft engines, played ice waterproof effect; used in textiles, but also made of waterproof, stain-resistant clothing.

附图说明 Brief Description

图1是实施例3低表面能涂层的表面能水接触角测量效果图。 Figure 1 is 3 patients with low surface energy coating surface water contact angle measurements can implement renderings.

图2是实施例4低表面能涂层的表面能水接触角测量效果图。 Figure 2 is an example 4 low surface energy coating the surface of the water contact angle measurements can implement renderings.

图3是实施例5低表面能涂层的表面能水接触角测量效果图。 Example 5 Figure 3 is a low surface energy surface coating embodiment can effect the water contact angle measurements FIG.

图4是实施例6低表面能涂层的表面能水接触角测量效果图。 Figure 4 is a 6 cases of low surface energy coating the surface of the water contact angle measurements can implement renderings.

具体实施方式 DETAILED DESCRIPTION

下面列举的实施例对本发明进一步说明,但本发明不只限于这些实施例。 The following examples are exemplified for the present invention is further illustrated, but the present invention is not limited to these examples.

实施例1:含活性端基的全氟烷基化合物的制备将60份甲苯二异氰酸脂溶解于140份的乙酸乙酯中,加入0.5份二月桂酸二丁基锡,然后加入800份全氟烷基乙醇。 Example 1: Preparation of perfluoroalkyl compounds containing reactive end groups of the 60 parts of toluene diisocyanate were dissolved in 140 parts of ethyl acetate was added 0.5 parts of dibutyl tin dilaurate, followed by addition of 800 parts of perfluoro alkyl alcohol. 反应在0-25℃下搅拌反应4小时,再在60-80℃下搅拌8小时。 The reaction was stirred at 0-25 ℃ for 4 hours, then stirred at 60-80 ℃ 8 hours. 反应物冷却至室温后,得到1000份均相液体。 After the reaction was cooled to room temperature to obtain 1000 parts of a homogeneous liquid.

实施例2:含活性端基的全氟烷基化合物的制备将40份二苯甲烷二异氰酸脂溶解于200份的乙酸乙酯中,加入0.5份二月桂酸二丁基锡,然后加入700份全氟烷基乙醇。 Example 2: Preparation of perfluoroalkyl compounds containing reactive end groups of the 40 parts of diphenylmethane diisocyanate were dissolved in 200 parts of ethyl acetate, was added 0.5 parts of dibutyl tin dilaurate, followed by addition of 700 parts of perfluoroalkyl ethanol. 反应在0-25℃下搅拌反应2小时,再在60-80℃下搅拌6小时。 The reaction was stirred at 0-25 ℃ for 2 hours, then stirred at 60-80 ℃ 6 hours. 反应物冷却至室温后,得到1000份均相液体。 After the reaction was cooled to room temperature to obtain 1000 parts of a homogeneous liquid.

实施例3:低表面能涂层的制备将实施例1产物与丙烯酸树脂(牌号BS2150)配合,按下述步骤制备:A组分:将100份BS2150丙烯酸树脂、60份颜填料(30份氧化铁红、20份氧化锌和10份重质碳酸钙)和60份稀释剂(50份二甲苯和10份丙酮混合)加入到容器中,在2000rpm转速下高速分散2小时,当细度为30~50μm时,用100目滤网过滤,计量包装;B组分为实施例1的产物;将A、B组分按重量比为5∶1均匀混合后,采用喷涂工艺施工,室温固化,固化时间10小时以上,得到光滑平整的低表面能涂层。 Example 3: Preparation of low surface energy coatings to the product of Example 1 and acrylic resin (Grade BS2150) complex, prepared by the following steps: A component: 100 parts of BS2150 acrylic resin, 60 parts of pigment (30 parts by oxidation iron oxide red, 20 parts of zinc oxide and 10 parts of heavy calcium carbonate) and 60 parts of a diluent (50 parts of xylene and 10 parts of acetone) were added to the vessel, a high speed disperser at 2000rpm speed two hours, when a fineness of 30 ~ When 50μm, with a 100 mesh filter, weighing and packaging; group B is divided into the product of Example 1; the A, B component weight ratio 5:1 After uniformly mixing, spraying construction process, room temperature curing, curing more than 10 hours, to obtain smooth, low surface energy coating. 对涂层表面能水接触角测量达到109。 Coating the surface of the water contact angle measurements can reach 109 . 效果见图1。 Results shown in Figure 1. 该涂料可应用于船舶减阻防污的需要,具有良好的效果。 The coating can be applied to the needs of the ship antifouling drag, with good results.

实施例4:低表面能涂层的制备将实施例1产物与丙烯酸树脂(牌号BS9960)配合,按下述步骤制备:A组分:将100份BS9960丙烯酸树脂、70份颜填料(金红石型钛白粉10份氧化铁红、50份漂珠和10份云母)和60份稀释剂(50份甲苯和10份丁酮混合)加入到容器中,在2000rpm转速下高速分散3小时,当细度为30~50μm时,用100目滤网过滤,计量包装;B组分为实施例1产物; Example 4: Preparation of low surface energy coatings to the product of Example 1 and acrylic resin (Grade BS9960) complex, prepared as follows: A component: 100 parts of BS9960 acrylic resin, 70 parts of pigment (rutile-type titanium white powder 10 parts of red iron oxide, 50 parts and 10 parts mica floating beads) and 60 parts of a diluent (50 parts of toluene and 10 parts of methyl ethyl ketone mixed) was added to the vessel, a high speed disperser at 2000rpm speed 3 hours, when the fineness When 30 to 50μm, with a 100 mesh filter, weighing and packaging; component B product of Example 1;

将A、B组分按重量比8∶1均匀混合后,采用喷涂工艺施工,室温固化,固化时间10小时以上,得到光滑平整的低表面能涂层,对涂层表面能水接触角测量达到107;效果见图2。 The A, B components were uniformly mixed at a weight ratio 8:1 After spraying construction process, room temperature curing, the curing time is more than 10 hours to obtain a smooth and flat lower surface energy coating, the coating surface can reach a water contact angle measurements 107 ; effect shown in Figure 2. 该涂料可应用于航空飞行器上,起到防水防冰的效果。 The coating can be applied to the aviation aircraft, played ice waterproof effect.

实施例5:低表面能涂层的制备将实施例2产物与丙烯酸树脂(牌号BS960)配合,按下述步骤制备:A组分:将100份BS960丙烯酸树脂、70份颜填料(10份金红石型钛白粉、25份滑石粉、25份云母和10份重质碳酸钙)和60份稀释剂(50份二甲苯和10份丙酮混合)加入到容器中,在2000rpm转速下高速分散3小时,当细度为30~50μm时,用100目滤网过滤,计量包装;B组分为实施例2的产物;将A、B组分按重量比11∶1均匀混合后,采用刷涂工艺施工,室温固化,固化时间12小时以上,得到光滑平整的低表面能涂层,对涂层表面能水接触角测量达到105。 Example 5: Preparation of low surface energy coatings to the product of Example 2 and the acrylic resin (Grade BS960) complex, prepared by the following steps: A component: 100 parts of BS960 acrylic resin, 70 parts of pigment (10 parts rutile type titanium dioxide, 25 parts of talc, 25 parts of mica and 10 parts by weight of calcium carbonate) and 60 parts of a diluent (50 parts of xylene and 10 parts of acetone) were added to the vessel, a high speed disperser at 2000rpm rpm for 3 hours, When the fineness of 30 to time 50μm, with a 100 mesh filter, weighing and packaging; group B is divided into the product of Example 2; the A, B components were uniformly mixed at a weight ratio 11:1 After brushing process Construction , room temperature curing, the curing time is more than 12 hours to obtain a smooth coating of low surface energy, the surface energy of the coating to reach a water contact angle measurements 105 . 效果见图3。 Results shown in Figure 3. 该涂料可应用于室外天线罩上,可防止积雪堆积,从而保证通信质量。 The coating can be applied to an outdoor antenna cover to prevent snow accumulation, thus ensuring the quality of communication.

实施例6:低表面能涂层的制备将实施例2的产物与丙烯酸树脂(牌号BS985)配合,按下述步骤制备: Example 6: Preparation of low surface energy coating product of Example and an acrylic resin (Grade BS985) 2 complex, prepared according to the following steps:

A组分:将100份BS985丙烯酸树脂、75份颜填料(25份滑石粉、25份云母和25份重质碳酸钙)和60份稀释剂(50份甲苯和10份丁酮混合)加入到容器中,在2000rpm转速下高速分散4小时,当细度为30~50μm时,用100目滤网过滤,计量包装;B组分:为实施例2的产物;将A、B组分按重量比10∶1均匀混合后,采用刷涂工艺施工,室温固化,固化时间24小时以上,得到光滑平整的低表面能涂层。 A component: 100 parts BS985 acrylic resin, 75 parts of fillers (25 parts of talc, mica, 25 parts and 25 parts by weight of calcium carbonate) and 60 parts of diluent (50 parts of toluene and methyl ethyl ketone mixing 10 parts) was added to container, at a high speed disperser speed 2000rpm 4 hours, when a fineness of 30 ~ When 50μm, with 100 mesh filter, weighing and packaging; B component: the product from Example 2; the A, B component by weight 10:1 uniform mixing ratio after brushing construction process, room temperature curing, curing time of 24 hours or more to obtain a smooth, low surface energy coatings. 对涂层表面能水接触角测量达到100;效果见图4。 Coating the surface of the water contact angle measurements can reach 100 ; effect shown in Figure 4. 该涂料可应用于建筑外墙涂料上,防涂鸦、保持建筑的清洁和美观。 The coating can be applied to the exterior house paint, anti-graffiti, clean, and beautiful architecture.

实施例7:对实施例4、5中的涂层进行耐擦拭实验,经有机溶剂600次擦拭后,水接触角不变。 Example 7: 4, 5 in Example scratch coating experiment, the organic solvent after wiping 600 times, the water contact angle unchanged.

Referenced by
Citing PatentFiling datePublication dateApplicantTitle
CN102099615B *27 May 200914 Jan 2015缠绕机公司Ice-phobic coating and use thereof
CN102352558A *10 Jun 201115 Feb 2012上海汇宇精细化工有限公司Stain-resistant leather treatment agent and preparation method
CN102352558B10 Jun 20115 Jun 2013上海汇宇精细化工有限公司Stain-resistant leather treatment agent and preparation method
CN102676034A *24 Apr 201219 Sep 2012三元控股集团有限公司Anti-doodling coating for outdoor facility and preparation method of anti-doodling coating
CN102676034B *24 Apr 201219 Aug 2015三元控股集团有限公司一种适用于户外设施的抗涂鸦涂料及其制备方法
CN102876150A *14 Jul 201116 Jan 2013上海大通高科技材料有限责任公司High weather resistant anti-pasting and doodling-proof water-based paint and preparing method thereof
CN103483974A *10 Oct 20131 Jan 2014常熟市方塔涂料化工有限公司Environment-friendly grease proofing paint
CN104736583B *16 Aug 201315 Mar 2017巴斯夫涂料有限公司含氟非水性涂料组合物、涂覆方法和涂料组合物的用途
US957408916 Aug 201321 Feb 2017Basf Coatings GmbhFluorine-containing nonaqueous coating material composition, coating methods, and the use of the coating material composition
WO2016095128A1 *17 Dec 201423 Jun 2016Dow Global Technologies LlcSurfactants for polyurethane foams
Classifications
International ClassificationC09D133/14, C09D7/12
Legal Events
DateCodeEventDescription
29 Aug 2007C06Publication
24 Oct 2007C10Entry into substantive examination
9 Dec 2009C14Grant of patent or utility model
2 Jul 2014C56Change in the name or address of the patentee
Owner name: MARINE CHEMICAL RESEARCH INSTITUTE
Free format text: FORMER NAME: RESEARCH INST OF OCEAN CHEMISTRY
11 May 2016EXPYTermination of patent right or utility model