CN113667082A - 一种软触感羟基聚氨酯分散体及其制备方法 - Google Patents
一种软触感羟基聚氨酯分散体及其制备方法 Download PDFInfo
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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
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- C08G18/3212—Polyhydroxy compounds containing cycloaliphatic groups
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G2150/00—Compositions for coatings
Abstract
本发明公开了一种软触感羟基聚氨酯分散体,包括以下组分:a)一端亲水一端疏水的聚氨酯预聚体;b)直链型分子量在1000~5000的聚酯多元醇;c)流变助剂;d)水。其中,组分a)通过以下重量组分反应获得:至少一种二异氰酸酯;具有可离子化亲水基团的羟基化合物;至少一种分子量为500至5000的二元醇;胺或无机碱;至少一种分子量小于400的二元醇或多元醇;上述各组分的重量总和为100%。本发明采用外乳化工艺合成水性聚氨酯分散体,提高了该水性聚氨酯储存稳定性,同时可通过调整a)和b)组份来获得不同羟基含量和软触感的分散体,从而实现兼顾软触感和耐化性。
Description
技术领域
本发明属于树脂涂料技术领域,尤其涉及一种具有软触感的羟基聚氨酯分散体及其制备得到的软触感涂料组合物。
背景技术
随着人们对环境与健康意识的不断增强,水性涂料日益受到重视。现阶段涂料领域的水性化主要集中在木器涂料、汽车原厂涂料、建筑涂料、集装箱涂料等领域。软触感涂料由于其表面特殊的触觉感受,漆膜会带给消费者天鹅绒一般丝滑、橡胶一般Q弹或温暖的感受,因此在3C(包括电脑产品、通信产品和消费类电子产品)领域非常受欢迎并且经久不衰。而在3C领域,由于对涂料产品的综合性能、装饰效果以及长期使用的可靠性要求非常高,因此,涂料水性化率非常低。目前的软触感涂料绝大部分均为油性产品,配方中溶剂含量在600~800g/L,远超国家涂料消费税免征点420g/L。所以在3C领域对低VOC含量的水性软触感涂料需求迫切。近年来已经确立了基于聚氨酯结构的水性软触感涂料体系。
专利CN 1572849A、CN 1910214A、CN101061153A、CN 1884408A、CN101153192A及CN104736582A公开的制备具有软触感水性聚氨酯树脂的方法均为传统的预聚体法和丙酮法。这两种方法各有缺陷,预聚体法难以制备高固含聚氨酯分散体。而丙酮法虽然可以制备高固含聚氨酯分散体,但其制备工艺相对复杂,不可控因素更多,缺点更明显。首先丙酮作为易制毒原料,需要到公安部门备案后才能进行采购;其次,丙酮作为低闪点易燃物料,生产操作过程中存在较大安全风险;最后,丙酮法生产的聚氨酯,加水分散完后需要抽真空将丙酮脱除,增加工时和能耗,同时脱丙酮过程中,脱低釜中容易产生结皮,而结皮随着搅拌被打碎成碎末混在树脂中,出料过滤包装容易堵滤网,又会增加生产工时。
发明内容
针对现有技术存在的问题,本发明提供了一种软触感羟基聚氨酯分散体及其制备方法。
为解决上述技术问题,本发明采用了以下技术方案:
一种软触感羟基聚氨酯分散体,包括以下组分:
a)一端亲水一端疏水的聚氨酯预聚体;
b)直链型分子量在1000~5000的聚酯多元醇;
c)流变助剂;
d)水;
其中,组分a)通过以下重量组分反应获得:
ⅰ)5至30重量%的至少一种二异氰酸酯;
ⅱ)1至20重量%的具有可离子化亲水基团的羟基化合物;
ⅲ)40至90重量%的至少一种分子量为500至5000的二元醇;
ⅳ)0至5重量%的胺或无机碱;
ⅴ)0至10重量%的至少一种分子量小于400的二元醇或多元醇;
上述各组分的重量总和为100%。
作为优选,所述组分a)的反应组分中异氰酸酯基于羟基的摩尔比范围为0.3~5:1。优选0.3:1至3:1、更优选0.3:1至1.5:1、甚至更优选0.5:1至1.5:1。
作为优选,组分ⅰ)是一种二异氰酸酯,相对于用于制备聚氨酯预聚体的重量占比优选5~15%,其采用亚乙基二异氰酸酯、1,6-六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)、环己烷-1,4-二异氰酸酯、4,4′-二环己基甲烷二异氰酸酯(H12MDI)、对四甲基二甲苯二异氰酸酯(p-TMXDI)(及其间位异构体m-TMXDI)、1,4-亚苯基二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、4,4′-二苯基甲烷二异氰酸酯(MDI)、多亚甲基多苯基多异氰酸酯中的一种或多种的混合。
更优选,所述组分ⅰ)为IPDI和/或H12MDI的混合。
作为优选,所述组分ⅱ)为具有可离子化亲水基团的羟基化合物。相对于用于制备聚氨酯的组分的总量,组分(B)的量为1至20重量%,优选2至10重量%,甚至更优选2至7重量%。可离子化亲水基团是指在相关条件下可以通过形成盐(即通过碱使基团进行去质子化)而被转化为带负电荷的阴离子基团。组分(B)包含任何合适的多元醇,优选二醇,其含有可离子化的亲水基团。优选的离子性亲水基团是阴离子性水亲水基团。优选的阴离子性亲水基团是羧酸、磷酸和/或磺酸基团。这些化合物的实例包括含羧基的二醇,例如二羟基烷酸如2,2-二羟甲基丙酸(DMPA)或2,2-二羟甲基丁酸(DMBA)。或者磺酸盐基团可用作潜在阴离子性水分散基团。阴离子性水分散基团优选完全或部分为盐形式。
作为优选,所述组分ⅲ)采用分子量为500至5000g/mol的二醇,相对于用于制备聚氨酯的组分的总量,其添加量为40-90重量%,优选为50-90重量%,甚至更优选55至85重量%。这种多元醇可以选自可用于聚氨酯合成的任何化学类型的多元醇。特别地,多元醇可以是聚酯多元醇、聚醚多元醇、聚碳酸酯多元醇、聚乙烯基多元醇和/或聚硅氧烷多元醇。组分(c)的玻璃化转变温度Tg优选为-110℃至+110℃,更优选为-100℃至+40℃,最优选为-100℃和-35℃。优选的二醇(C)是聚醚二醇,优选包括聚亚烷基二醇(例如聚丙二醇(PPG);聚乙二醇(PEG);聚四氢呋喃(PTMEG)。优选的聚醚多元醇选自由PPG、PEG、PTMEG及其混合物,更优选的是PPG和/或PTMEG,最有用的是PTMEG。
作为优选,所述组分ⅳ)任选地通过用碱(优选在制备聚氨酯预聚物期间和/或在制备本发明的水性组合物期间)中和聚氨酯预聚物来转化成盐形式。如果阴离子性水分散基团被中和,则用于中和基团的碱优选为氨、胺或无机碱。合适的胺包括叔胺,例如三乙胺或N,N-二甲基乙醇胺。合适的无机碱包括碱金属氢氧化物和碳酸盐,例如氢氧化锂、氢氧化钠或氢氧化钾。还可以使用季铵氢氧化物,例如N+(CH3)4(OH)。通常使用可以为组合物提供所需的抗衡离子的碱。例如,优选的抗衡离子包括Li+、Na+、K+、NH4+和取代的铵盐。也可以使用阳离子性水分散性基团,但不太优选。实例包括吡啶基、咪唑基和/或季铵基团,其是可被中和或永久电离的(例如与硫酸二甲酯)。非常合适的组分(b)是二羟甲基丙酸(DMPA)。
作为优选,所述组分ⅴ)选用分子量低于500g/mol、优选在40至250g/mol范围内的二醇。其相对于用于制备聚氨酯的组分的总量,组分ⅴ)的量为0至10重量%,优选0.5至5重量%。进一步的,优选采用乙二醇、新戊二醇、丁二醇、己二醇或1,4-环己烷二甲醇。
作为优选,所述组分b)直链型分子量在1000~5000的聚酯多元醇的玻璃化转变温度为-100℃~100℃。其通过小分子二元醇与小分子二元酸反应获得,其中:
所述小分子二元醇为乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,4-环己烷二甲醇、1,6-己二醇、新戊二醇、二甘醇等,优选乙二醇、1,4-丁二醇和1,6-己二醇;
所述小分子二元酸为对苯二甲酸、间苯二甲酸、邻苯二甲酸、1,4-环己烷二甲酸、己二酸、富马酸、葵二酸、月桂二酸以及它们的可能酸酐。
作为优选,所述组分c)流变助剂根据本发明的要求优选包含0.5-20重量%的流变添加剂(相对于组份(1)-(3)的总量而言)。优选有机增稠剂,包括纤维素醚及其衍生物、缔合型碱溶胀型增稠剂(HASE)、非缔合型碱溶胀增稠剂(ASE)、缔合型聚氨酯增稠剂(HEUR)等,优选缔合型增稠剂,更优选缔合型聚氨酯增稠剂(HEUR)。缔合型增稠剂可以通过增加体系的粘度来提高分散体的储存稳定性。
作为优选,所组分b)与a)的重量比为0.5~10:1,组分c)的占组分a)、b)和c)的总重量的0.5-20%。
本发明另一目的,是还提供了一种上述软触感羟基聚氨酯分散体的制备方法,包括以下步骤:
步骤S1,按比例将组分ⅰ)~ⅴ)进行混合反应,得到一端亲水一端疏水的聚氨酯预聚体a);
步骤S2,继续加入直链型分子量在1000~5000的聚酯多元醇混合均匀;
步骤S3,继续加入组分c)流变助剂并混合均匀后,最后加入去离子水,完毕。
有益效果,与现有技术相比,本发明具有以下优点:
(1)本发明发明不需要采用传统的丙酮法工艺即可获得高固含量水性聚氨酯分散体。可带来两方面好处,首先是由于丙酮属于低闪点甲类易燃品,常规丙酮法工艺中加丙酮和脱丙酮这一步存在很大的安全风险,因此本工艺过程中不使用丙酮,生产方面的安全性大大增加;另外,传统的丙酮法在6吨以上水性聚氨酯生产过程中,后期脱除丙酮这一步至少需要8小时才能达到指标要求,因此本发明可以大大降低生产工时,节约生产成本。
(2)本发明的羟基聚氨酯分散体,树脂配方调整空间大,可通过调整a)和b)组份来获得不同羟基含量和软触感的分散体,从而实现兼顾软触感和耐化性。
具体实施方式
下面结合具体实施例,进一步阐明本发明。应理解这些实施例仅用于说明本发明而不用于限制本发明的范围,在阅读了本发明之后,本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定的范围。
本发明使用到物质组分的英文缩写与中文注释:
BYK333:流平剂,毕克化学
TEGO810:消泡剂,迪高
TEGO280:润湿剂,迪高
BYK192:分散剂,毕克化学
BORCHERS LH-10:催化剂,OMG
Acematt OK 520:消光粉,德固赛
Bayhydur XP 2655:水性异氰酸酯固化剂,科思创
实施例1 聚酯多元醇(组分b)
向装有搅拌、冷凝、加热和分水装置的反应容器中加入1340克的己二酸、355克的1,4-丁二醇、274克的1,6-己二醇和239克的乙二醇,将该物料在1小时内加热到140℃,然后在6小时内将温度升至220℃,直到酸值小于5mgKOH/g为止。这样得到的聚酯多元醇OH值为56mgKOH/g。
实施例2 聚酯多元醇(组分b)
向装有搅拌、冷凝、加热和分水装置的反应容器中加入1220克的己二酸、345克的1,4-丁二醇、262克的1,6-己二醇和223克的乙二醇,将该物料在1小时内加热到140℃,然后在6小时内将温度升至220℃,直到酸值小于5mgKOH/g为止。这样得到的聚酯多元醇OH值为110mgKOH/g。
实施例3 软触感羟基分散体
向装有搅拌、冷凝、加热装置的反应容器中加入308克数均分子量2000的聚四氢呋喃PTMEG,6克1,4-环己烷二甲醇,17克二羟甲基丙酸DMPA,在110℃下真空脱水2小时,然后破真空冷却降温至70℃,32克1,6-六亚甲基二异氰酸酯HDI,在90℃下反应4小时至NCO降为0。加入11克N,N-二甲基乙醇胺后搅拌30分钟,得到一端亲水一端疏水的聚氨酯预聚体(作为高分子乳化剂)。
然后加入374克来自实施例1的聚酯多元醇和7.48克Borchi Gel 0620流变助剂,搅拌2小时。降温至80℃,滴加500克去离子水2小时。这样得到的羟基聚氨酯分散体OH含量为1.45%(对固体分),固含60%,粘度500mPa.s。
实施例4 软触感羟基分散体
向装有搅拌、冷凝、加热装置的反应容器中加入308克数均分子量2000的聚四氢呋喃PTMEG,6克1,4-环己烷二甲醇,17克二羟甲基丙酸DMPA,在110℃下真空脱水2小时,然后破真空冷却降温至70℃,32克1,6-六亚甲基二异氰酸酯HDI,在90℃下反应4小时至NCO降为0。加入11克N,N-二甲基乙醇胺后搅拌30分钟,得到聚氨酯预聚体。
然后加入748克来自实施例1的聚酯多元醇和11.22克Borchi Gel 0620流变助剂,搅拌2小时。降温至80℃,滴加748克去离子水2小时。这样得到的羟基聚氨酯分散体OH含量为1.53%(对固体分),固含60%,粘度1200mPa.s。
实施例5 软触感羟基分散体
向装有搅拌、冷凝、加热装置的反应容器中加入308克数均分子量2000的聚丙二醇PPG,6克1,4-环己烷二甲醇,17克二羟甲基丙酸DMPA,在110℃下真空脱水2小时,然后破真空冷却降温至70℃,32克1,6-六亚甲基二异氰酸酯HDI,在90℃下反应4小时至NCO降为0。加入11克N,N-二甲基乙醇胺后搅拌30分钟,得到聚氨酯预聚体。
然后加入374克来自实施例1的聚酯多元醇和7.48克Borchi Gel 0620流变助剂,搅拌2小时。降温至80℃,滴加500克去离子水2小时。分散体外观无蓝相,放置过夜后分层。
实施例6 软触感羟基分散体
向装有搅拌、冷凝、加热装置的反应容器中加入308克数均分子量2000的聚四氢呋喃PTMEG,6克1,4-环己烷二甲醇,17克二羟甲基丙酸DMPA,在110℃下真空脱水2小时,然后破真空冷却降温至70℃,32克1,6-六亚甲基二异氰酸酯HDI,在90℃下反应4小时至NCO降为0。加入11克N,N-二甲基乙醇胺后搅拌30分钟,得到聚氨酯预聚体。
然后加入374克来自实施例2的聚酯多元醇和7.48克Borchi Gel 0620流变助剂,搅拌2小时。降温至80℃,滴加500克去离子水2小时。这样得到的羟基聚氨酯分散体OH含量为2.30%(对固体分),固含60%,粘度1800mPa.s。
实施例7 软触感羟基分散体
向装有搅拌、冷凝、加热装置的反应容器中加入308克数均分子量2000的聚四氢呋喃PTMEG,6克1,4-环己烷二甲醇,17克二羟甲基丙酸DMPA,在110℃下真空脱水2小时,然后破真空冷却降温至70℃,32克1,6-六亚甲基二异氰酸酯HDI,在90℃下反应4小时至NCO降为0。加入11克N,N-二甲基乙醇胺后搅拌30分钟,得到聚氨酯预聚体。
然后加入748克来自实施例2的聚酯多元醇和7.48克Borchi Gel 0620流变助剂,搅拌2小时。降温至80℃,滴加748克去离子水2小时。这样得到的羟基聚氨酯分散体OH含量为2.66%(对固体分),固含60%,粘度2000mPa.s。
应用实施例
软触感弹性涂料的配方组成
软触感弹性涂料的制备工艺
1)将树脂液加入烧杯中,开启分散机搅拌至500rpm
2)将助剂混合均匀,然后缓慢加入树脂液中,500rpm转速下分散5分钟
3)将转速提升至800rpm,加入消光粉Acematt OK520,800rpm下分散30min
4)加入固化剂Bayhydrol XP 2655,500rpm转速下搅拌5min,加入适量去离子水兑稀后,200目滤布过滤待用。
通过喷涂将上述工艺制备得到的水性涂料喷涂到ABS+PC塑胶基材上,在室温下闪干10分钟,然后70℃下干燥8小时。这样得到具有突出软触感弹性效果的均匀涂层。
干燥后涂层的性能测试结果:
耐溶剂测试方法:
将浸泡了溶剂的棉垫放置到涂层上,并用表面皿盖住棉垫,一分钟后移走棉垫,用棉布擦去多余的溶剂,观察涂层是否起泡和涂层颜色是否变化。
耐油酸测试方法:
将浸泡了油酸的棉垫放置到涂层上,然后放入40℃×95%湿度的高温高湿相中,8小时后取出,移走棉垫并用棉布擦去剩余的油酸,观察涂层是否起泡和涂层颜色是否变化。
本发明的技术创新点在于:
1、区别于传统水性聚氨酯自乳化工艺,本发明采用外乳化工艺合成水性聚氨酯分散体,提高了该水性聚氨酯储存稳定性。
2、本发明不需要采用传统的丙酮法工艺即可获得高固含量水性聚氨酯分散体
3、本发明的羟基聚氨酯分散体,树脂配方调整空间大,可通过调整a)和b)组份来获得不同羟基含量和软触感的分散体,从而实现兼顾软触感和耐化性。
Claims (18)
1.一种软触感羟基聚氨酯分散体,其特征在于包括以下组分:
a)一端亲水一端疏水的聚氨酯预聚体;
b)直链型分子量在1000~5000的聚酯多元醇;
c)流变助剂;
d)水;
其中,组分a)通过以下重量组分反应获得:
ⅰ)5至30重量%的至少一种二异氰酸酯;
ⅱ)1至20重量%的具有可离子化亲水基团的羟基化合物;
ⅲ)40至90重量%的至少一种分子量为500至5000的二元醇;
ⅳ)0至5重量%的胺或无机碱;
ⅴ)0至10重量%的至少一种分子量小于400的二元醇或多元醇;
上述各组分的重量总和为100%。
2.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分a)的反应组分中异氰酸酯基于羟基的摩尔比范围为0.3~5:1。
3.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅰ)为亚乙基二异氰酸酯、1,6-六亚甲基二异氰酸酯(HDI)、异佛尔酮二异氰酸酯(IPDI)、环己烷-1,4-二异氰酸酯、4,4′-二环己基甲烷二异氰酸酯(H12MDI)、对四甲基二甲苯二异氰酸酯(p-TMXDI)(及其间位异构体m-TMXDI)、1,4-亚苯基二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、4,4′-二苯基甲烷二异氰酸酯(MDI)、多亚甲基多苯基多异氰酸酯中的一种或多种的混合。
4.根据权利要求3所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅰ)为IPDI和/或H12MDI的混合。
5.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅱ)为可离子化为带负电荷的阴离子亲水基团的多元醇。
6.根据权利要求5所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅱ)为可离子化为带负电荷的阴离子亲水基团的二元醇。
7.根据权利要求5所述软触感羟基聚氨酯分散体,其特征在于:所述可离子化为带负电荷的阴离子亲水基团为羧酸基团、磷酸基团和/或磺酸基团。
8.根据权利要求5所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅱ)为二羟基烷酸如2,2-二羟甲基丙酸(DMPA)或2,2-二羟甲基丁酸(DMBA)。
9.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅲ)为聚酯多元醇、聚醚多元醇、聚碳酸酯多元醇、聚乙烯基多元醇和/或聚硅氧烷多元醇。
10.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅲ)的玻璃化转变温度Tg优选为-110℃至+110℃。
11.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅲ)为聚亚烷基二醇(例如聚丙二醇(PPG)、聚乙二醇(PEG)、聚四氢呋喃(PTMEG)。
12.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅳ)为三乙胺、N,N-二甲基乙醇胺、金属氢氧化物、碳酸盐或季铵氢氧化物。
13.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分ⅴ)为乙二醇、新戊二醇、丁二醇、己二醇或1,4-环己烷二甲醇。
14.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分b)直链型分子量在1000~5000的聚酯多元醇的玻璃化转变温度为-100℃~100℃。
15.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分b)聚酯多元醇通过小分子二元醇与小分子二元酸反应获得,其中:
所述小分子二元醇为乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、1,4-环己烷二甲醇、1,6-己二醇、新戊二醇、二甘醇等,优选乙二醇、1,4-丁二醇和1,6-己二醇;
所述小分子二元酸为对苯二甲酸、间苯二甲酸、邻苯二甲酸、1,4-环己烷二甲酸、己二酸、富马酸、葵二酸、月桂二酸以及它们的可能酸酐。
16.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所述组分c)流变助剂为纤维素醚及其衍生物、缔合型碱溶胀型增稠剂(HASE)、非缔合型碱溶胀增稠剂(ASE)、缔合型聚氨酯增稠剂(HEUR)。
17.根据权利要求1所述软触感羟基聚氨酯分散体,其特征在于:所组分b)与a)的重量比为0.5~10:1,组分c)的占组分a)、b)和c)的总重量的0.5-20%。
18.一种权利要求1~17任一所述软触感羟基聚氨酯分散体的制备方法,其特征在于包括以下步骤:
步骤S1,按比例将组分ⅰ)~ⅴ)进行混合反应,得到一端亲水一端疏水的聚氨酯预聚体a);
步骤S2,继续加入直链型分子量在1000~5000的聚酯多元醇混合均匀;
步骤S3,继续加入组分c)流变助剂并混合均匀后,最后加入去离子水,完毕。
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