CN113527695A - 一种超支化聚合物水性分散剂的制备方法及应用 - Google Patents
一种超支化聚合物水性分散剂的制备方法及应用 Download PDFInfo
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Abstract
本发明涉及一种超支化聚合物水性分散剂的制备方法及其在水性色浆中的应用，为聚(苯乙烯‑co‑马来酸酐)‑g‑(聚乙二醇单甲醚+EO‑PO‑EO+NR3)，可生物降解、不含烷基酚；本发明提供一种超支化聚合物水性分散剂的制备方法，具有阴非离子‑多支链梳状结构，分子结构中含有芳环、羧基、羟基、胺基及聚醚等多个颜料吸附基团，利用空间位阻防止颜料颗粒絮凝沉降，优异的降粘分散性，提高着色力，防止浮色和发花，可制备无树脂/树脂体系的高固低粘颜料浓缩浆分散体，如机红、黄、紫色颜料、无机颜料、消光粉，也可用于有机颜料、防锈颜料及填料的混合分散，适用于水性色浆、水性工业涂料、水性油墨、水性防腐防锈底漆等水性体系。
Description
技术领域
本发明涉及一种水性分散剂，尤其涉及到一种超支化聚合物水性分散剂的制备方法及应用，属于聚合物分散剂技术领域。
背景技术
在涂料油墨生产中，颜料分散是一项至关重要的环节，选择合适的分散剂能够较易获得颜料分散均一、储存稳定的涂料，尽管传统的分散剂在水性分散介质中显示出有效的分散稳定作用，但由于它们在颜料粒子表面的吸附不十分牢固，容易从粒子表面上解吸从而导致被分散的粒子重新聚集或沉淀，体系的长期稳定性欠佳，对漆膜外观、硬度及耐老化等性质也有不利影响，尤其是分散剂针对性强的特点，同一分散剂不能广泛适用于不同有机颜料的分散，导致用户生产成本提高。
分散剂是一种在分子内同时具有亲油性和亲水性两种相反性质的界面活性剂，可均一分散难溶于液体的无机、有机颜料的固体颗粒，同时防止固体颗粒的沉降和凝聚。随着人们对健康环保要求的提高，水性环保涂料成为建筑装饰领域的新宠，在涂料制作工艺中，颜料在研磨剪切力下以微小的颗粒均匀分散于漆料中，由于颜料粒子表面极性低，但水的表面张力要比有机溶剂大很多，就需要添加一些助剂降低水的表面张力，增强对颜料颗粒的润湿作用，使得在配制水性涂料油墨时，分散稳定性问题难于解决，缩小了其使用范围；因此，必须对颜料表面进行改性使颜料粒子表面覆盖某种分散剂，从而达到改善颜料应用性能的目的。
苯乙烯-马来酸酐共聚物(SMA)分子链中既含有疏水性苯乙烯链段，又含有亲水性马来酸酐链段，其水解产物是一种常用的高分子分散剂；同时，SMA分子链中的酸酐单元可进行酰胺化、酯化、阳离子化等改性，苯环单元可进行磺化等改性，从而获得性能优异的高分子分散剂。这类高分子分散剂对具有极大表面积和较高比表面能的超细固体颗粒(如颜料、无机粒子等)能起到良好的分散稳定作用，因此被称为苯乙烯-马来酸系超分散剂。苯乙烯-马来酸系超分散剂在国内外被广泛应用于颜料、染料、涂料、印刷、造纸、建筑等领域。
Zhang.L等使用可逆加成－断裂链转移(RAFT)控制聚合反应，合成了苯乙烯－马来酸酐共聚物，研究了其水解共聚物的分散能力，发现对有机酞菁蓝颜料具有良好分散性能。Xu Y,Liu j等合成了一种超支化苯乙烯-马来酸酐共聚物(BPSMA)，并将该产物应用于水性体系中炭黑分散，结果表明，相比于线性苯乙烯-马来酸酐共聚物(LPSMA)，BPSMA对炭黑颜料分散体具有较小的粒径、更窄的粒度分布和更高的稳定性。
王平等采用研磨分散法制备了超细分散红60，并研究了聚苯乙烯-马来酸酯化物PSMA和脂肪醇聚氧乙烯醚(AE)协同作用对分散染料分散稳定性能的影响。关有俊等则以苯乙烯、部分酯化的马来酸酐和马来酸酐为单体，合成了一种水溶性高分子超分散剂—部分酯化的SMA，并探讨了各种工艺参数对共聚物分散性能的影响。周家达等则利用2、3-环氧丙基三甲基氯化铵对进行阳离子化改性，制备了部分酯化接枝季铵盐的阳离子表面活性剂，研究发现该聚合物对颜料黄14的分散稳定性较好。
林圣森等制备了3种梳型两亲聚合物，聚(苯乙烯-co-马来酸酐)-g-(聚乙二醇单甲醚)(A)、聚(苯乙烯-co-马来酸酐)-g-C12H25OH)(B)和聚(苯乙烯-co-马来酸酐)-co-(聚乙二醇单甲醚+C12H25OH)(C)。发现3种梳型两亲聚合物用作做炭黑的分散剂时，在相同条件下，3种样品对炭黑的分散性能依次为B＞C＞A。
本发明制备一种结构为聚(苯乙烯-co-马来酸酐)-g-(聚乙二醇单甲醚+EO-PO-EO+NR3)超支化水性分散剂，对有机颜料红、黄、紫具有很好的分散作用。
发明内容
苯乙烯-马来酸超支化结构具有降粘作用，其分子结构中的锚固基团，如羧基、羧酸根、多元醇、多元胺及聚醚等，通过离子键、共价键、氢键及范德华力等相互作用，紧紧地结合在极性超细粒子表面上，另外一部分非极性苯环或则缠绕在粒子外表面。非极性苯环或聚醚链与分散介质相容性良好，呈现舒展构象，在粒子表面形成“厚厚的”保护层。由于占用空间和构象所引起的空间阻碍作用，即产生空间位阻效应，当两个吸附有超分散剂分子的粒子相互“靠拢”时，粒子之间会产生排斥力而使固体粒子弹开，因而不会絮凝。另外聚链上含有PO支链，具有消泡抑泡作用。
本发明目的旨在提供一种超支化聚合物水性分散剂及其制备方法。
为了解决水性分散剂在水性体系中的分散和稳定性能，本发明采用苯乙烯-马来酸酐共聚物(SMA)，其分子结构式如下：
其中，分子式中的x:y＝1:1～2:1；z＝8～10。
本发明采用聚乙二醇单甲醚MPEG和环氧乙烷-环氧丙烷嵌段共聚物EO-PO-EO封端，然后用叔胺中和水性化。所述的超支化聚合物水性分散剂，为结构为SMA-g-MPEG+EO-PO-EO+NR3；其分子结构式如下所示：
其中，分子式中的x:y＝1:1～2:1；z＝8～10；
R为-CH2CH3或-CH2CH2OH；R＇为
q＝22～28；
EO-PO-EO为
m＝40～45；n＝2～5。
所述的超支化聚合物水性分散剂，其数均分子量为20000～22000。
为了解决上面所述的技术问题，本发明采取以下技术方案：本发明涉及一种超支化聚合物水性分散剂，按重量百分比计，其成分为：苯乙烯-马来酸酐共聚物12.0～18.0％、聚乙二醇单甲醚15.0～20.0％、环氧乙烷-环氧丙烷嵌段共聚物5.0～10.0％、叔胺0.2～0.5％、去离子水45.0～60.0％。
其中，所述的苯乙烯-马来酸酐共聚物为数均分子量为1000～2000。
所述的聚乙二醇单甲醚为数均分子量为1000～1200。
所述的环氧乙烷-环氧丙烷嵌段共聚物为数均分子量为2000～2200，EO的含量占8.0～10.0％。
所述的叔胺为三乙胺或三乙醇胺中的一种。
本发明提供一种超支化聚合物水性分散剂的制备方法，其制备步骤如下：
按重量百分比，称取苯乙烯-马来酸酐共聚物、聚乙二醇单甲醚、环氧乙烷-环氧丙烷嵌段共聚物加入到反应釜中，升温到120℃开始熔化，开起真空，控制真空度为0.09MPa下脱水1h；待完全溶化后开动搅拌，继续升温170～175℃、并控制真空度为0.07～0.08MPa下反应3～4h，每0.5h取样检测酸值，当含酸值达到规定的值时停止反应；降温至120℃，关闭N2，搅拌下加入叔胺，同时加入去离子水，当pH值为7.0～8.5时降温至60℃，过滤包装，得所述的超支化聚合物水性分散剂。
本发明所述的超支化聚合物水性分散剂采用一釜法生产，工艺简单，没有用到危险品原材料，无三废排放，属于绿色生产工艺。
本发明制备的超支化聚合物水性分散剂JW在水性色浆的应用，按重量百分比计，其组成如下表1、2所示：
表1：水性色浆组成
| 名称 | 铁红 | 铁黄 | 钛白 | PY74 | PY154 | PY83 | PY93 |
| 去离子水 | 13.9-14.9 | 19.2-20.2 | 17.9-18.9 | 29.3-30.3 | 34.2-35.2 | 39.0-40.0 | 39.2-40.2 |
| 丙二醇 | 5.0 | 5.0 | 5.0 | 6.0 | 6.0 | 6.0 | 6.0 |
| 杀菌剂 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| 消泡剂 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| 润湿剂 | 1.0 | 1.0 | 1.0 | 2.0 | 2.0 | 2.0 | 2.0 |
| JW分散剂 | 6.0-7.0 | 5.5-6.5 | 4.0-5.0 | 11.0-12.0 | 11.0-12.0 | 11.0-12.0 | 11.0-12.0 |
| 颜料 | 72.0 | 67.0 | 70.0 | 50.0 | 45.0 | 40.0 | 40.0 |
| pH调节剂 | 0.2 | 0.5 | 0.2 | 0.2 | 0.2 | 0.3 | 0.2 |
| 防沉剂 | 0.5 | 0.4 | 0.5 | 0.1 | 0.2 | 0.3 | 0.2 |
表2：水性色浆组成
本发明制备的超支化聚合物水性分散剂，具有阴非离子-多支链梳状结构，分子结构中含有芳环、羧基、羟基、胺基及聚醚等多个颜料吸附基团，利用空间位阻防止颜料颗粒絮凝沉降，优异的降粘分散性，提高着色力，防止絮凝、浮色和发花，可制备无树脂/树脂体系的高固低粘颜料浓缩浆分散体，如机红、黄、紫色颜料、无机颜料、消光粉，也可用于有机颜料、防锈颜料及填料的混合分散，适用于水性色浆、水性工业涂料、水性油墨、水性防腐防锈底漆等水性体系。
具体实施方式
本发明结合以下实施例对超支化聚合物水性分散剂的制备做进一步描述。可以理解的是，此处所描述的具体实施例仅仅用于解释相关发明，而非对该发明的限定。
实施例1
一种超支化聚合物水性分散剂，其制备步骤如下：
按重量百分比，称取125.0份SMA1200、155.0份MPEG1000、65.0份EO-PO-EO嵌段共聚物加入到反应釜中，升温到120℃开始熔化，开起真空，控制真空度为0.09MPa下脱水1h；待完全溶化后开动搅拌，继续升温170～175℃、并控制真空度为0.07～0.08MPa下反应4h，每0.5h取样检测酸值，当含酸值达到规定的值时停止反应；降温至120℃，关闭N2，搅拌下加入2.6份三乙胺，同时加入去离子水520.0份，当pH值为7.5～7.8时降温至60℃，过滤包装，制得固含为40.6％的超支化聚合物水性分散剂。
实施例2
一种超支化聚合物水性分散剂，其制备步骤如下：
按重量百分比，称取126.0份SMA1000、165.0份MPEG1000、55.0份EO-PO-EO嵌段共聚物加入到反应釜中，升温到120℃开始熔化，开起真空，控制真空度为0.09MPa下脱水1h；待完全溶化后开动搅拌，继续升温170～172℃、并控制真空度为0.07～0.08MPa下反应4h，每0.5h取样检测酸值，当含酸值达到规定的值时停止反应；降温至120℃，关闭N2，搅拌下加入2.8份三乙胺，同时加入去离子水500.0份，当pH值为7.0～7.2时降温至60℃，过滤包装，制得固含为41.5％的超支化聚合物水性分散剂。
实施例3
一种超支化聚合物水性分散剂，其制备步骤如下：
按重量百分比，称取125.0份SMA1000、160.0份MPEG1200、60.0份EO-PO-EO嵌段共聚物加入到反应釜中，升温到120℃开始熔化，开起真空，控制真空度为0.09MPa下脱水1h；待完全溶化后开动搅拌，继续升温170～172℃、并控制真空度为0.07～0.08MPa下反应4h，每0.5h取样检测酸值，当含酸值达到规定的值时停止反应；降温至120℃，关闭N2，搅拌下加入3.0份三乙醇胺，同时加入去离子水500.0份，当pH值为7.2～7.5时降温至60℃，过滤包装，制得固含为41.2％的超支化聚合物水性分散剂。
实施例4
一种超支化聚合物水性分散剂，其制备步骤如下：
按重量百分比，称取125.0份SMA1000、160.0份MPEG1000、60.0份EO-PO-EO嵌段共聚物加入到反应釜中，升温到120℃开始熔化，开起真空，控制真空度为0.09MPa下脱水1h；待完全溶化后开动搅拌，继续升温170～172℃、并控制真空度为0.07～0.08MPa下反应4h，每0.5h取样检测酸值，当含酸值达到规定的值时停止反应；降温至120℃，关闭N2，搅拌下加入3.2份三乙醇胺，同时加入去离子水500.0份，当pH值为7.0～7.2时降温至60℃，过滤包装，制得固含为42.2％的超支化聚合物水性分散剂。
实施例5
一种灰色水性丙烯酸防锈底漆，其组成为：水性丙烯酸树脂42.0份、乙二醇丁醚3.0份、分散剂2.5份、抗闪锈剂1.0份、磷酸锌6.0份、滑石粉6.0份、三聚磷酸铝3.0份、云母粉6.0份、高岭土10.0份、重钙粉5.0份、钛白粉2.0份、碳黑0.5份、消泡剂0.2份、流平剂0.1份、pH调节剂0.1份、二丙二醇甲醚2.0份、防沉剂1.0份、去离子水11.6份。
其中，所述分散剂为实施例中的超支化聚合物水性分散剂和对比例BYK-190W。
按照相关标准，其检测的性能指标如表3所示。
表3：水性丙烯酸防锈底漆性能技术指标
尽管本发明已作了详细说明并引证了实施例，但对于本领域的普通技术人员，显然可以按照上述说明而做出的各种方案、修改和改动，都应该包括在权利要求的范围之内。
Claims (6)
1.一种超支化聚合物水性分散剂，其特征在于，为超支化梳状阴非离子型，成分为SMA-g-MPEG+EO-PO-EO+NR3，其分子结构式如下所示：
其中，分子式中的x:y＝1:1～2:1；z＝8～10；
R为-CH2CH3或-CH2CH2OH；R＇为
q＝22～28；
EO-PO-EO为
m＝40～45；n＝2～5；
所述的超支化聚合物水性分散剂，其数均分子量为20000～22000。
2.一种如权利1所述的超支化聚合物水性分散剂的制备方法，其特征在于，所述的制备方法，其步骤如下：
按重量百分比，称取苯乙烯-马来酸酐共聚物、聚乙二醇单甲醚、环氧乙烷-环氧丙烷嵌段共聚物加入到反应釜中，升温到120℃开始熔化，开起真空，控制真空度为0.09MPa下脱水1h；待完全溶化后开动搅拌，继续升温170～175℃、并控制真空度为0.07～0.08MPa下反应3～4h，每0.5h取样检测酸值，当含酸值达到规定的值时停止反应；降温至120℃，关闭N2，搅拌下加入叔胺，同时加入去离子水，当pH值为7.0～8.5时降温至60℃，过滤包装，得所述的超支化聚合物水性分散剂；
其中，按重量百分比计，各原料成分如下：
所述的环氧乙烷-环氧丙烷嵌段共聚物为数均分子量为2000～2200，EO的含量占8.0～10.0％。
3.根据权利要求2所述的超支化聚合物水性分散剂，其特征在于，所述的苯乙烯-马来酸酐共聚物为数均分子量为1000～2000；所述的苯乙烯与马来酸酐的摩尔比为1:1～2:1。
4.根据权利要求2所述的超支化聚合物水性分散剂，其特征在于，所述的聚乙二醇单甲醚为数均分子量为1000～1200。
5.根据权利要求2所述的超支化聚合物水性分散剂，其特征在于，所述的叔胺为三乙胺或三乙醇胺中的一种。
6.一种如权利要求2所述的超支化聚合物水性分散剂在水性色浆中的应用，其特征在于，所述的水性色浆，按重量百分比计，其组成如表1、表2：
表1：水性色浆组成
表2：水性色浆组成
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| CN114736381A (zh) * | 2022-04-20 | 2022-07-12 | 无锡颐景丰科技有限公司 | 一种梳状高分子表面活性剂及其合成方法 |
| CN115057952A (zh) * | 2022-07-29 | 2022-09-16 | 岳阳凯门水性助剂有限公司 | 改性聚苯乙烯马来酸酐聚合物及其制备方法、水性分散剂和色浆 |
| CN115057952B (zh) * | 2022-07-29 | 2023-09-15 | 岳阳凯门水性助剂有限公司 | 改性聚苯乙烯马来酸酐聚合物及其制备方法、水性分散剂和色浆 |
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