CN107082887B - 一种超分散剂的制备方法及其应用 - Google Patents
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Abstract
本发明提供一种超分散剂的制备方法,以苯乙烯‑马来酸酐共聚物为主链,聚乙烯亚胺和多乙烯多胺为支链,其主链在多种树脂中具有优异的相容性,支链可与各种涂料用的色粉的表面相结合,起到良好的锚定作用,其梳妆结构可以有很好的空间效应,用于制备分散液,使得色粉能很好的分散在体系中,具有很好的展色性。
Description
技术领域
本发明涉及一种超分散剂的制备方法及其应用,尤其涉及一种改性的苯乙烯-马来酸酐共聚物分散剂的制备方法及其应用,属于分散剂加工技术领域。
背景技术
苯乙烯-马来酸酐共聚物(SMA)分子链中既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产物。为了获得性能优异的高分子分散剂,可以对苯乙烯-马来酸酐共聚物进行改性。现有的改性苯乙烯-马来酸酐共聚物一般只能用于特定的树脂中,其酰胺化产物很少用作分散剂,原因是其没有好的锚定基团,可以很好的锚定到颜料表面。且现有产品对颜料的润湿、分散性不够强,只能分散特定种类的颜料,且现有产品大多含有有机溶剂,不利用环保。
发明内容
本发明的目的在于提供一种超分散剂的制备方法,以苯乙烯-马来酸酐为主链,聚乙烯亚胺和多乙烯多胺为支链,合成一种具有宽广的树脂相容性、良好分散性和展色性的超分散剂。
本发明的技术方案如下:
一种超分散剂的制备方法,具体包括以下步骤:
步骤(1):利用苯乙烯和马来酸酐共聚,获得苯乙烯-马来酸酐共聚物产品;
步骤(2):在氮气的保护下,加入苯乙烯-马来酸酐共聚物和多乙烯多胺,在50-70℃条件下反应4h以上;
步骤(3):在氮气的保护下,向步骤(2)反应物中加入聚乙烯亚胺,继续反应4h以上,降温,得到黄色液体。
所述超分散剂的制备方法,其中,所述步骤(1)可以利用现有方法制备苯乙烯-马来酸酐共聚物。优选按照以下步骤进行:
步骤a:称取苯乙烯、马来酸酐,用甲苯在反应瓶内加热溶解马来酸酐,在搅拌下先后将BPO(过氧化苯甲酰)及1/3的苯乙烯加入反应瓶;
步骤b:在60-90℃条件下,反应20-60分钟,有白色混浊出现时,用甲苯溶解余下的苯乙烯,慢慢滴入反应瓶中,1-5小时加完,再反应半小时,升温至80-100℃,反应0.5-2小时;
步骤c:反应完全后,即刻减压过滤,用少量甲苯洗沉淀三次,抽干,80℃烘干,得白色细粉状的苯乙烯-马来酸酐共聚物产品。
所述超分散剂的制备方法,步骤(1)所的苯乙烯-马来酸酐共聚物的分子量为1000-20000,马来酸酐的含量为10%-50%(摩尔比)。
所述超分散剂的制备方法,步骤(2)中,多乙烯多胺与马来酸酐的摩尔比为1:1,多乙烯多胺的分子量为100-1000。
所述超分散剂的制备方法,步骤(3)中,聚乙烯亚胺与马来酸酐的摩尔比为1:1,聚乙烯亚胺为非线性结构,其分子量为1000-10000。
按照上述制备方法制得的超分散剂,其结构式如下:
其中,x、y、m、n、p均为1-50之间的整数。
一种上述超分散剂在制备分散液中的应用,所述分散液中含有涂料、无机颜料、有机颜料、油墨或成膜树脂。
上述超分散剂在制备分散液中的应用,其中,所述成膜树脂为丙烯酸树脂、醇酸树脂、环氧树脂或聚氨树脂。
本发明的有益效果是:
1、以苯乙烯-马来酸酐共聚物为主链,聚乙烯亚胺和多乙烯多胺为支链,合成一种改性的超分散剂,其主链在多种树脂中具有优异的相容性,支链可与各种涂料用的色粉的表面相结合,起到良好的锚定作用。其梳妆结构可以有很好的空间效应,使得色粉能很好的分散在体系中,具有很好的展色性;
2、与现有产品相比,本发明所得超分散剂具有宽广的树脂相容性,在丙烯酸树脂、醇酸树脂、环氧树脂及聚氨树脂中对无机颜料和有机颜料有良好的分散效果;
3、制备方法简单,条件温和,所得产物中无有机溶剂,没有VOC排放,节是一种绿色环保的溶剂型分散剂。
附图说明
图1为本发明实施例1所得产物的红外光谱图。
具体实施方式
为使本发明的目的、技术方案及效果更加清楚、明确,以下举实例对本发明进一步详细说明。应当理解,此处所描述的具体实施例仅用于解释本发明,并不用于限定本发明。
实施例1
按照以下步骤合成超分散剂:
步骤(1):利用苯乙烯和马来酸酐共聚,获得苯乙烯-马来酸酐共聚物产品;
步骤(2):在氮气的保护下,按照马来酸酐与多乙烯多胺为1:1的摩尔比加入苯乙烯-马来酸酐共聚物和多乙烯多胺(重均分子量约为400),在60℃条件下反应;
步骤(3):在氮气的保护下,按照马来酸酐与聚乙烯亚胺为1:1的摩尔比向步骤(2)反应物中加入非线性聚乙烯亚胺(重均分子量约为1800),继续反应4h,降温,得到黄色液体即为本发明所述超分散剂。
本实施例中,所述超分散剂的制备方法,其中,所述步骤(1)所得苯乙烯-马来酸酐共聚物的重均分子量约为2000,其中,且步骤(1)优选按照以下步骤进行:
步骤a:按照1:1的摩尔比称取苯乙烯和马来酸酐,用甲苯在反应瓶内加热溶解马来酸酐,在搅拌下先后将BPO(过氧化苯甲酰)及1/3的苯乙烯加入反应瓶;
步骤b:在80℃条件下,反应30分钟,有白色混浊出现时,用甲苯溶解余下的苯乙烯,慢慢滴入反应瓶中,3小时加完,再反应半小时,升温至90℃,反应1.5小时;
步骤c:反应完全后,即刻减压过滤,用少量甲苯洗沉淀三次,抽干,80℃烘干,得白色细粉状的苯乙烯-马来酸酐共聚物产品。
本实施例所得超分散剂的红外光谱图如图1所示,其中,1602.86cm-1、1454.33cm-1处的吸收峰为芳烃的特征吸收峰,证明苯乙烯在主链上;1697.36cm-1为酰胺键的特征吸收峰,1768cm-1处为C=O的特征吸收峰,3000cm-1-3100cm-1处为仲胺的特征吸收峰,3500cm-1-3600cm-1处为伯胺的特征吸收峰,从图中可看出,本产品的胺通过形成酰胺的形式连接在含有芳烃的主链上。其反应方程式如下:
其中,x、y、m、n、p均为1-50之间的整数。
实施例2
按照以下步骤合成超分散剂:
步骤(1):利用苯乙烯和马来酸酐共聚,获得苯乙烯-马来酸酐共聚物产品;
步骤(2):在氮气的保护下,按照马来酸酐与多乙烯多胺为1:1的摩尔比加入苯乙烯-马来酸酐共聚物和多乙烯多胺(重均分子量约为900),在60℃条件下反应;
步骤(3):在氮气的保护下,按照马来酸酐与聚乙烯亚胺为1:1的摩尔比向步骤(2)反应物中加入非线性聚乙烯亚胺(重均分子量约为6000),继续反应4h,降温,得到黄色液体即为本发明所述超分散剂。
本实施例中,所述超分散剂的制备方法,其中,所述步骤(1)所得苯乙烯-马来酸酐共聚物的重均分子量约为10000,其中,且步骤(1)优选按照以下步骤进行:
步骤a:按照3:1的摩尔比称取苯乙烯和马来酸酐,用甲苯在反应瓶内加热溶解马来酸酐,在搅拌下先后将BPO(过氧化苯甲酰)及1/3的苯乙烯加入反应瓶;
步骤b:在60℃条件下,反应60分钟,有白色混浊出现时,用甲苯溶解余下的苯乙烯,慢慢滴入反应瓶中,1.1小时加完,再反应半小时,升温至100℃,反应0.5小时;
步骤c:反应完全后,即刻减压过滤,用少量甲苯洗沉淀三次,抽干,80℃烘干,得白色细粉状的苯乙烯-马来酸酐共聚物产品。其化学反应方程式及所得产物的红外光谱图与实施例1基本相同。
实施例3
按照以下步骤合成超分散剂:
步骤(1):利用苯乙烯和马来酸酐共聚,获得苯乙烯-马来酸酐共聚物产品;
步骤(2):在氮气的保护下,按照马来酸酐与多乙烯多胺为1:1的摩尔比加入苯乙烯-马来酸酐共聚物和多乙烯多胺(重均分子量约为400),在60℃条件下反应;
步骤(3):在氮气的保护下,按照马来酸酐与聚乙烯亚胺为1:1的摩尔比向步骤(2)反应物中加入非线性聚乙烯亚胺(重均分子量约为10000),继续反应4h,降温,得到黄色液体即为本发明所述超分散剂。
本实施例中,所述超分散剂的制备方法,其中,所述步骤(1)所得苯乙烯-马来酸酐共聚物的重均分子量约为20000,其中,且步骤(1)优选按照以下步骤进行:
步骤a:按照9:1的摩尔比称取苯乙烯和马来酸酐,用甲苯在反应瓶内加热溶解马来酸酐,在搅拌下先后将BPO(过氧化苯甲酰)及1/3的苯乙烯加入反应瓶;
步骤b:在90℃条件下,反应20分钟,有白色混浊出现时,用甲苯溶解余下的苯乙烯,慢慢滴入反应瓶中,5小时加完,再反应半小时,升温至80℃,反应2小时;
步骤c:反应完全后,即刻减压过滤,用少量甲苯洗沉淀三次,抽干,80℃烘干,得白色细粉状的苯乙烯-马来酸酐共聚物产品。其化学反应方程式及所得产物的红外光谱图与实施例1基本相同。
实施例4相容性、分散性、稳定性、着色力、展色性和颜色性能测试
为了证明本发明所得超分散剂的有益效果,本实施例采用正十六烷基胺将苯乙烯-马来酸酐共聚物酰胺化(酰胺化过程与本发明上述方法基本相同,区别仅在于用正十六烷基胺替代多乙烯多胺和聚乙烯亚胺)后制得的超分散剂作为对照品,进行对比试验,测试方法如下:
相容性:将实施例1-3制得的超分散剂以及对照品与多种成膜物质按1:10的比例混合均匀,同时利用隔夜观察分散体系是否清澈透明,结果见表1。
分散性:按先按配方研磨黑浆和黄浆,研磨介质:φ1-1.2mm玻璃珠10000rpm*60min。测量色浆细度、粒径分布、粘度。
配方:醇酸树脂46%
二甲苯13%
PMA 9%
分散剂14%
黑浆或黄浆18%
着色力和颜色数据:研磨得到的色浆分别在深色测试基础漆里按照10%和浅色测试基础漆里按照2%的比例加入各只色浆,静置消泡后用100μ涂布器在黑白卡上刮板。测量样板光泽,以国外竞品4310样板为标准,对比色差。
展色性:分别用热贮存前后的色浆按照上一试验的方法配成色漆,分散均匀后静置过夜,观察湿样浮色情况,在白色铜版纸上200μ刮板指研,测试色差。
稳定性:色浆和配好的色漆50℃贮存30天,检测有无返粗、增稠、分层、沉淀等问题。
实验结果如下:
表1:各组分散剂相容性测试结果
成膜物质 | 实施例1 | 实施例2 | 实施例3 | 对照品 |
丙烯酸树脂 | 清澈 | 清澈 | 清澈 | 清澈 |
醇酸树脂 | 清澈 | 清澈 | 清澈 | 轻微浑浊 |
聚酰胺 | 清澈 | 清澈 | 清澈 | 轻微浑浊 |
聚氨树脂 | 清澈 | 清澈 | 轻微浑浊 | 清澈 |
环氧树脂 | 轻微浑浊 | 清澈 | 清澈 | 清澈 |
纤维素 | 清澈 | 清澈 | 清澈 | 清澈 |
由表1可知,按照本发明所述方法制得的分别以多乙烯多胺、聚乙烯亚胺为支链的超分散剂,其与丙烯酸树脂、醇酸树脂、聚酰胺、聚氨树脂、环氧树脂、纤维素等成膜物质具有良好的相容性,优于以正十六烷基胺为支链的苯乙烯-马来酸酐共聚物。
表2:分散性、稳定性,着色力和颜色数据
由表2可知,按照本发明所述方法制得的分别以多乙烯多胺、聚乙烯亚胺为支链的超分散剂,其分散性、着色能力及稳定性与4310相当,而以正十六烷基胺为支链的超分散剂对照品的性能欠佳。
表3展色性测试结果
由表2可知,按照本发明所述方法制得的分别以多乙烯多胺、聚乙烯亚胺为支链的超分散剂,其展色性显著优于4310和以正十六烷基胺为支链的超分散剂对照品。
以上对本发明进行了详细的介绍,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,而所有这些改进和变换都应属于本发明所附权利要求的保护范围。
Claims (5)
1.一种超分散剂的制备方法,其特征在于,具体包括以下步骤:
步骤(1):称取苯乙烯、马来酸酐,用甲苯在反应瓶内加热溶解马来酸酐,在搅拌下先后将过氧化苯甲酰及1/3的苯乙烯加入反应瓶;
在60-90℃条件下,反应20-60分钟,有白色混浊出现时,用甲苯溶解余下的苯乙烯,慢慢滴入反应瓶中,1-5小时加完,再反应半小时,升温至80-100℃,反应0.5-2小时;
反应完全后,即刻减压过滤,用少量甲苯洗沉淀三次,抽干,80℃烘干,得白色细粉状的苯乙烯-马来酸酐共聚物产品;
步骤(2):在氮气的保护下,加入苯乙烯-马来酸酐共聚物和多乙烯多胺,在50-70℃条件下反应4h以上,其中,所述的多乙烯多胺与马来酸酐的摩尔比为1:1,多乙烯多胺的分子量为100-1000;
步骤(3):在氮气的保护下,向步骤(2)反应物中加入聚乙烯亚胺,继续反应4h以上,降温,得到黄色液体,其中,所述的聚乙烯亚胺与马来酸酐的摩尔比为1:1,聚乙烯亚胺为非线性结构,其分子量为1000-10000。
2.根据权利要求1所述的超分散剂的制备方法,其特征在于,步骤(1)所述的苯乙烯-马来酸酐共聚物的分子量为1000-20000,马来酸酐的含量为10%-50%。
3.按照权利要求1-2中任一项所述的制备方法制得的超分散剂,其结构式如下:
其中,x、y、m、n、p均为1-50之间的整数。
4.一种权利要求3所述的超分散剂在制备分散液中的应用,其特征在于,所述分散液中含有涂料、无机颜料、有机颜料、油墨或成膜树脂。
5.根据权利要求4所述的超分散剂在制备分散液中的应用,其特征在于,所述成膜树脂为丙烯酸树脂、醇酸树脂或环氧树脂。
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