CN104769050A - 含有dcoit的控制释放组合物 - Google Patents

含有dcoit的控制释放组合物 Download PDF

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CN104769050A
CN104769050A CN201380057480.9A CN201380057480A CN104769050A CN 104769050 A CN104769050 A CN 104769050A CN 201380057480 A CN201380057480 A CN 201380057480A CN 104769050 A CN104769050 A CN 104769050A
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dcoit
activated carbon
coating
microns
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J·阿什莫
D·拉根艾拉
B·普拉努耶尔
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Nutrition and biotechnology USA second Ltd.
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Abstract

一种组合物,其含有4,5-二氯-2-正辛基异噻唑啉-3-酮和表面积为至少700m2/g的活性碳。

Description

含有DCOIT的控制释放组合物
技术领域
本发明涉及含有4,5-二氯-2-正辛基异噻唑啉-3-酮(4,5-dichloro-2-n-octylisothiazolin-3-one,DCOIT)的控制释放组合物。
背景技术
含有DCOIT的控制释放组合物公开于美国专利第6,676,954号中。然而,需要以较低速率释放DCOIT的控制释放组合物。
本发明所解决的问题是提供一种改进的控制释放调配物,其提供DCOIT的长期控制释放。
发明内容
本发明涉及包含4,5-二氯-2-正辛基异噻唑啉-3-酮和表面积为至少700m2/g的活性碳的组合物。
具体实施方式
除非另外规定,否则温度以摄氏度(℃)计,百分比的提及是重量百分比(wt%),并且DCOIT的量和比率是按活性成分计。如本文所使用,当粒子集具有某一值的D50时,那么50体积百分比的粒子具有小于或等于所述值的直径。对于非球形粒子来说,直径是最大尺寸。船舶涂料组合物是能够在船舶物件的表面上形成干燥涂层的涂料组合物。在形成干燥涂层之后,即使当一些或全部经涂布的表面保持在水下大量的时间(即每天至少一个小时)时,干燥涂层也将粘着于表面持续有用地长的时间。船舶物件是在其中一些或全部物件在水下持续大量的时间的环境中投入使用的那些物件。船舶物件的实例包括船、码头、船坞、桩、鱼网、热交换器、水坝以及管道结构,如进口滤网。优选地,衬底是船舶物件。
海水是来自大海或海洋的水。平均来说,世界海洋中的海水具有约3.5wt%的盐度和1.025g/ml的海洋表面平均密度。人工海水是水与溶解的矿物质盐的混合物,其模拟海水。人工海水的实例是可购自RICCA(ASTM D1141)的合成海水。
优选地,DCOIT和活性碳存在于船舶涂料中,即涂布于船舶物件上。优选地,在涂布于船舶物件表面上之前,将DCOIT和活性碳添加到液体船舶涂料调配物中。在本发明的一个优选实施例中,将DCOIT和活性碳分别添加到液体船舶涂料组合物中。在本发明的一个优选实施例中,DCOIT和活性碳在添加到液体船舶涂料组合物中之前组合。通过将呈熔融物或溶液形式的DCOIT与活性碳混合,DCOIT可以吸附在活性碳上。对于DCOIT来说适合的溶剂是溶解DCOIT、不使其去稳定化并且不与活性碳反应的任何溶剂。适合的溶剂包括醇,如甲醇、乙醇以及丙醇;酯,如乙酸乙酯和乙酸丁酯;酮,如丙酮、甲基异丁基酮以及甲基异戊基酮;二甲苯;矿油精;以及腈,如乙腈。优选的溶剂是(C1-C4)醇、二甲苯以及矿油精。优选地,使DCOIT在与活性碳或液体船舶涂料混合之前在溶剂中溶解或成浆液。
用于船舶涂料的衬底可以是未经涂布的表面,例如船舶物件或船舶物件表面上的另一种涂层,例如表面上的底涂剂或涂料的底层。优选地,船舶涂层是环氧树脂涂层、自抛光涂层(例如金属丙烯酸酯共聚物涂料,典型地并有锌或铜羧酸盐基团,或硅烷基丙烯酸酯共聚物涂料)或污损释放涂层(例如硅酮涂料)。船舶涂料组合物包含粘合剂和溶剂以及任选地其它成分。所述溶剂可以是有机溶剂或水。其它成分可以包括无机颜料、有机颜料或染料以及天然树脂。水基涂料还可以含有聚结剂、分散剂、表面活性剂、流变改性剂或粘着促进剂。溶剂基涂料还可以包括增量剂、塑化剂或流变改性剂。典型的船舶涂料组合物包含5%到30%的粘合剂,至多15%的松香/改性松香,0.5%到5%的塑化剂,0.1%到2%的防沉剂,5%到60%的溶剂,至多65%的氧化亚铜,至多30%的颜料(不同于氧化亚铜)以及至多15%的船舶防污剂(包括DCOIT)。优选地,船舶涂料含有至少0.5wt%的DCOIT,优选是至少0.8wt%,优选是至少1wt%,优选是至少1.2wt%,优选是至少1.4wt%,优选是至少1.6wt%,优选是至少1.8wt%,优选是至少2wt%;优选地,船舶涂料含有不超过5wt%的DCOIT,优选是不超过4.5wt%,优选是不超过4wt%,优选是不超过3.5wt%,优选是不超过3wt%,优选是不超过2.5wt%,优选是不超过2wt%,优选是不超过1.8wt%。优选地,船舶涂料含有至少1wt%的活性碳,优选是至少1.5wt%,优选是至少2wt%,优选是至少2.5wt%,优选是至少3wt%,优选是至少3.5wt%;优选地,船舶涂料含有不超过20wt%的活性碳,优选是不超过16wt%,优选是不超过14wt%,优选是不超过12wt%,优选是不超过10wt%,优选是不超过8wt%。
优选地,活性碳与DCOIT的重量比是至少1∶1,优选是至少1.5∶1,优选是至少2∶1,优选是至少2.5∶1,优选是至少3∶1;优选地,所述重量比不超过12∶1,优选是不超过10∶1,优选是不超过8∶1,优选是不超过6∶1,优选是不超过5∶1,优选是不超过4.5∶1。优选地,自抛光涂层中活性碳与DCOIT的重量比是1.5∶1到5∶1,优选是2∶1到4∶1。优选地,污损释放涂层中活性碳与DCOIT的重量比是2∶1到10∶1,优选是2∶1到8∶1,优选是3∶1到8∶1。
优选地,船舶涂层的湿膜厚度是至少25微米,优选是至少50微米,优选是至少100微米,优选是至少200微米;优选是不超过500微米,优选是不超过400微米,优选是不超过300微米。预期湿涂层固化后所形成的干膜的厚度将比湿厚度小对应于湿涂层材料的溶剂含量的量。优选地,船舶涂层的干(固化)膜厚度是至少20微米,优选是至少40微米,优选是至少80微米,优选是至少160微米;优选是不超过400微米,优选是不超过320微米,优选是不超过240微米。
适合的活性碳包括例如碳,如衍生自煤、木材、椰子壳、木质素或动物骨的碳。活性碳可以通过物理处理或化学处理产生。物理处理需要以下过程的组合:在600℃到900℃范围内的温度下在缺氧条件下使碳碳化、热解;以及在高于250℃的温度下用氧化气氛(二氧化碳、氧气或蒸汽)暴露碳化的碳。化学活化需要在碳化之前用以下特定化学物质浸渍原材料:酸、强碱或盐(例如磷酸、氢氧化钾、氢氧化钠、氯化钙以及氯化锌25%);继而在较低温度(450℃到900℃)下进行碳化。特别优选的是高表面积“活性”碳,如通过直接化学活化制备的碳。关于这些活性碳和其制备方法的其它一般和具体细节可以查询石油衍生碳(Petroleum Derived Carbons)(T.M.奥格雷迪(T.M.O′Grady)和A.N.温涅伯格(A.N.Wennerberg)著),《美国化学学会讨论会丛刊》(AmericanChemical Society Symposium Series),第303卷,J.D.巴夏(J.D.Bacha)等人编,美国化学学会出版物(American Chemical Society Publications),华盛顿哥伦比亚特区(Washington,D.C.),(1986)。优选地,活性碳的表面积是至少750m2/g(通过BET方法测量),优选是至少800m2/g,优选是至少900m2/g,优选是至少1000m2/g,优选是至少1200m2/g;优选是不超过2500m2/g,优选是不超过2200m2/g。
优选地,仅在与DCOIT或船舶涂料调配物组合之前,活性碳的平均粒度(例如D50)是不超过100微米(0.1mm),优选是不超过50微米,优选是不超过40微米,优选是不超过35微米,优选是不超过30微米,优选是不超过25微米,优选是不超过20微米;优选是至少5微米,优选是至少10微米。
实例
经GERSTEL TWISTER聚二甲基硅氧烷(polydimethylsiloxane,PDMS)涂布的搅拌棒购自格斯特尔股份有限公司(Gerstel Gmbh)。所用的涂料是商购获得的InterluxMICRON 66涂料(“M66”)、INTERSLEEK 970涂料(“P970”)以及INTERSLEEK 731(“P731”),并且除了添加如下文所描述的DCOIT之外,根据制造商的说明将其混合。
使用定轨振荡器(美国红魔鬼公司(Red Devil Inc,USA))将涂料与DCOIT和吸附剂混合并且使用不锈钢量规将其涂覆在莱尼塔纸(Leneta paper)或铝箔上(湿膜厚度500微米)。使涂料干燥过夜。
将适当载体上的纸(20sq.cm到40sq.cm的涂料表面)浸没到含有100ml人工海水的120ml玻璃瓶中,插入Twister搅拌棒,并且将瓶子放置在搅拌混合器上。搅拌速率是600rpm。在第1天、第4天、第7天、第14天以及第21天,将TWISTER棒从瓶子中移出,用纸巾擦拭并且放置到含有1ml乙腈的HPLC小瓶中。在35℃下萃取吸附的杀生物剂30min。在萃取之后,再次擦拭棒并且将其放回具有海水/MAF涂料的瓶子中。通过HPLC测量杀生物剂的浓度。通过化学工作站(Chemstation)软件控制装备有自动进样器、柱加热器以及二极管阵列检测器的安捷伦(Agilent)1200 HPLC。使用UltraC18柱150×4.6cm(瑞斯泰克公司(Restek Inc))分析DCOIT。使用相同的等度条件(70%乙腈,2.3ml/min)。在280nm下检测到DCOIT。使用外部标准技术来对所释放的杀生物剂进行定量。基于先前校准,估计Twister搅拌棒容量是400微克。以涂料组合物中的DCOIT的重量计,报告以重量百分比计的DCOIT的累积释放。
DCOIT的累积释放(截止指定天释放的总DCOIT%)
注释:
DCOIT来自SEANINE 211N杀生物剂(陶氏化学公司(Dow Chem.Co.)),30%DCOIT于二甲苯中
“SPC”涂料是MICRON 66涂料(国际涂料(International Paints)),湿厚度254微米
“I970”是INTERSLEEK 970FRC涂料(国际涂料),湿厚度127微米
“I731”是INTERSLEEK 731FRC涂料(国际涂料),湿厚度127微米
活性碳
缩写 全称 表面积,m2/g
HD 纽恰尔(Nuchar)HD 1500-1900
SN-20 纽恰尔SN-20 1400-1800
RG-C 纽恰尔RG-C 1400-1800
CGP SUPER 诺芮特(Norit)CGP SUPER 1500-1700
KB-G 达寇(Darco)KB-G 1700
KB-WJ 达寇KB-WJ 1800
G-60 达寇G-60 600
S-51 达寇S-51 650
PAC 200 诺芮特PAC 200 1000-1150
数据表明,当DCOIT与表面积大于650m2/g的活性碳组合时,获得好得多的控制释放。

Claims (10)

1.一种组合物,其包含4,5-二氯-2-正辛基异噻唑啉-3-酮和表面积为至少700m2/g的活性碳。
2.根据权利要求1所述的组合物,其中活性碳与4,5-二氯-2-正辛基异噻唑啉-3-酮的重量比是1.5∶1到10∶1。
3.根据权利要求2所述的组合物,其中所述4,5-二氯-2-正辛基异噻唑啉-3-酮和所述活性碳存在于船舶涂料中。
4.根据权利要求3所述的组合物,其中所述船舶涂料包含0.5wt%到4wt%的4,5-二氯-2-正辛基异噻唑啉-3-酮和1.5wt%到16wt%的活性碳。
5.根据权利要求4所述的组合物,其中所述活性碳的表面积是800m2/g到2500m2/g。
6.根据权利要求5所述的组合物,其中所述船舶涂料是污损释放涂料。
7.根据权利要求5所述的组合物,其中所述船舶涂料是自抛光涂料。
8.根据权利要求7所述的组合物,其中所述自抛光涂料是金属丙烯酸酯共聚物涂料。
9.根据权利要求5所述的组合物,其中活性碳与4,5-二氯-2-正辛基异噻唑啉-3-酮的所述重量比是2∶1到8∶1。
10.根据权利要求9所述的组合物,其中所述船舶涂料包含1wt%到3.5wt%的4,5-二氯-2-正辛基异噻唑啉-3-酮和2wt%到12wt%的活性碳。
CN201380057480.9A 2012-11-06 2013-10-31 含有dcoit的控制释放组合物 Pending CN104769050A (zh)

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CL2015001115A1 (es) 2015-09-25
EP2898026A1 (en) 2015-07-29
JP2015535018A (ja) 2015-12-07
US9410046B2 (en) 2016-08-09
KR102299631B1 (ko) 2021-09-07
US20150284572A1 (en) 2015-10-08
BR112015007506A2 (pt) 2017-07-04
WO2014074376A1 (en) 2014-05-15
JP7089560B2 (ja) 2022-06-22

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