CN115387118A - 一种有机磷改性的丙烯酸浆料及其制备方法和应用 - Google Patents
一种有机磷改性的丙烯酸浆料及其制备方法和应用 Download PDFInfo
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Abstract
本发明提供一种有机磷改性的丙烯酸浆料及其制备方法和应用,涉及纺织技术领域。所述有机磷改性的丙烯酸浆料为有机磷单体、丙烯酸酯单体、疏水改性单体、亲水单体、蜡、链转移剂等通过自由基聚合,在水中分散而得到。本发明克服了现有技术的不足,通过有机磷单体赋予浆料良好的附着力、耐磨性和抗静电性;通过疏水改性单体赋予浆料良好的柔韧性,且耐磨性好、不吸湿发粘、抗静电效果持久,可不添加或者少添加助剂即可满足严苛环境中的使用。
Description
技术领域
本发明涉及纺织技术领域,具体涉及一种有机磷改性的丙烯酸浆料及其制备方法和应用。
背景技术
经纱上浆是织造工程的关键环节,纤维经过上浆后,提高复丝的集束性和强力,可以提高纱线的耐磨性,减少毛羽、适当地增加纱线的强度,减少伸度,以承受经纱在织造过程中受到的机械作用力,提高纱线的可织造性。
目前经纱上浆的浆料主要有淀粉、聚乙烯醇(PVA)和聚丙烯酸酯类三大浆料。其中,丙烯酸酯浆料是其中应用最为广泛的一种。在严苛的环境中,丙烯酸酯浆料易出现吸湿再粘、耐磨性能不足等问题。因此,有大量的研究人员提出了解决丙烯酸酯浆料现有问题的方案。
常规的改善浆膜的耐磨性的方法有物理添加硅油、蜡、蜡乳液、纳米粉体等,例如专利CN114316722A将丙烯酸酯乳液与蜡乳液混合,得到高耐磨的水性光油。专利CN105908503B通过将丙烯酸酯和纳米SiO2复合变性淀粉混合,提升浆料的耐磨性和抗吸湿再粘效果。
专利CN103898753B将纳米二氧化硅改性淀粉、蛋白浆料、聚丙烯酸酯乳液、改性硅油消泡剂倒入搅拌器内进行搅拌混合,即可得到高枝棉织物浆料。所制备的浆料中各组分主要依靠物理混合。
这些采用物理混合方法,在存储和使用的过程中,会出现分层或上浆不均匀等问题,同时也会导致一定吸湿发粘,影响实际使用的便捷性,同时降低布料的品质。
发明内容
针对现有技术不足,本发明提供一种有机磷改性的丙烯酸浆料及其制备方法和应用,本发明制得的纺织浆料,柔韧性好、耐磨性好、不吸湿发粘、抗静电效果持久,可不添加或者少添加助剂即可满足严苛环境中的使用。
为实现以上目的,本发明的技术方案通过以下技术方案予以实现:
一种有机磷改性的丙烯酸浆料,所述丙烯酸浆料由以下质量份物质组成:蜡0.57-1.9份、磷酸丙烯酸酯单体0.095-0.475份、含烯键的单体19-23.75份、引发剂0.095-0.665份、链转移剂0.019-0.225份、助溶剂7-15份、中和剂2.47-10份、去离子水46-73份;其中所述含烯键单体为普通烯键单体、亲水性单体、疏水性单体按照质量比67.6-80.1∶17.9-25.2∶3.1-7.2组成。
优选的,所述亲水性单体选自丙烯酸、甲基丙烯酸、丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟丙酯、丙烯酰胺、丙烯酰胺基异丙基磺酸钠、含烯丙烯的特种醇醚硫酸盐、烯丙基醚羟丙基磺酸盐的中至少一种;所述疏水性单体选自丙烯酸十八烷基酯、叔碳酸乙烯酯、丙烯酸酯硅油、乙烯基聚硅氧烷、硅烷偶联剂KH570之中的至少一种。
优选的,所述磷酸丙烯酸酯单体为甲基丙烯酰氧乙基磷酸酯、乙二醇甲基丙烯酸酯磷酸酯、烷基丙烯酸酯磷酸酯至少一种,且所述烷基丙烯酸酯磷酸酯的结构式如下所示:
其中R为H或者烷基中的一种;X为烷基链。
优选的,所述的蜡为微晶蜡、蜂蜡、石蜡、沙索蜡、巴西棕榈蜡、氧化乙烯蜡等中的至少一种,且各种蜡的熔点为40~130℃。
优选的,所述引发剂为偶氮二异丁腈、偶氮二异庚腈、过氧化苯甲酰、过氧化2-乙基己基酸叔丁酯、过氧化2-乙基己基酸叔戊酯、过氧化苯甲酸叔丁酯等中的至少一种。
优选的,所述链转移剂为十二烷基硫醇、2,4-二苯基-4-甲基-1-戊烯、正辛硫醇、巯基乙酸、巯基乙醇、2-巯基丙酸异辛酯等中的至少一种。
优选的,所述中和剂为氨水、三乙胺、氢氧化钠、氢氧化钾、二甲基乙醇胺、三乙醇胺、二乙醇胺、AMP-95、氨基乙醇胺中的至少一种。
优选的,有机磷改性的丙烯酸浆料的制备方法包括以下步骤:
(1)混合处理:将蜡、磷酸丙烯酸酯单体、含烯键的单体、引发剂,链转移剂、助溶剂等充分混合均匀,制备成为反应混合液A;
(2)升温反应:将向有回流、温度计、搅拌、加料口的反应器内加入(1)中配制的反应混合液A质量份的5-50%,并升温引发反应,获得反应液备用;
(3)滴加反应:将剩余的混合液A滴加到上述反应液中,且滴加时间为2~5h,继续保温反应,得备用液;
(4)中和稀释:将上述备用液反应结束后加入中和剂进行中和反应,后加入去离子水进行稀释,得到有机磷改性的丙烯酸浆料
优选的,所述步骤(2)和步骤(3)中的升温引发反应和保温反应的温度为70~85℃。
有机磷改性的丙烯酸浆料可直接用于纺织纤维类的上浆,特别是用于锦纶、涤纶等合成纤维。
本发明提供一种有机磷改性的丙烯酸浆料及其制备方法和应用,与现有技术相比优点在于:
(1)本发明所制备的浆料,选用磷酸酯丙烯酸酯类功能单体,赋予浆料优异的附着力、耐磨性和抗静电性;
(2)本发明所制备的浆料,以含有烯键的单体和有机磷单体形成一种大分子乳化剂,将蜡结构包袱于其中,不需要额外的引入乳化蜡的乳化剂,因此有效提升了浆料的抗吸湿发粘效果;
(3)本发明所制备的浆料,引入具有滑爽结构的单体,如(甲基)丙烯酸十八烷基酯、硅烷丙烯酸酯单体等引入到聚合物主链上,有效的提升浆膜的柔韧性、耐磨性、抗吸湿再粘效果;
(4)本发明所制备的浆料采用聚合的方式将具备有不同功能的组分引入到分子结构链上,相较于复配型浆料,可有效提升浆料的稳定性,防止浆料分层,便于保存。
附图说明:
图1为本发明浆料对比的红外谱图
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面结合本发明实施例对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:
有机磷改性的丙烯酸浆料的制备:
(1)将3g聚乙烯蜡和1.8g微晶蜡、3g乙二醇甲基丙烯酸酯磷酸酯、27g甲基丙烯酸、20g丙烯酸丁酯、43g丙烯酸甲酯、28.2g甲基丙烯酸甲酯、15g丙烯酸乙酯、5.4g甲基丙烯酸十八烷基酯、3.6g过氧化苯甲酰,0.18g正十二烷基硫醇、72g异丙醇进行充分混合均匀,形成反应混合液A;
(2)向有回流、温度计、搅拌、加料口的反应器内加入步骤一配制的反应混合液A25.3g;逐渐升温至78℃,进行引发反应;
(3)待引发反应结束后,开始滴加步骤一剩余的反应混合液A,滴加时间为4h;控制反应温度为80℃;
(4)待滴加反应结束后,将31.2g三乙胺加入到反应器中,进行中和反应;
(5)向反应瓶中加入360g去离子水进行稀释,即可得到固含量为28.9%的有机磷改性的丙烯酸酯浆料。
实施例2:
有机磷改性的丙烯酸浆料的制备:
(1)将2.4g棕榈蜡、0.6g甲基丙烯酰氧乙基磷酸酯、9.5g丙烯酸、0.5g甲基丙烯酸羟乙酯、6g丙烯酸丁酯、10g丙烯酸甲酯、8.5g甲基丙烯酸甲酯、10g丙烯酸乙酯、2g甲基丙烯酸十八烷基酯和0.4g硅烷偶联剂KH570、0.8g偶氮二异丁腈,0.16g正十二烷基硫醇、15g异丙醇和15g乙醇混合溶剂进行充分混合均匀,形成反应混合液A;
(2)向有回流、温度计、搅拌、加料口的反应器内加入步骤一配制的反应混合液A10g;逐渐升温至80℃,进行引发反应;
(3)待引发反应结束后,开始滴加步骤一剩余的反应混合液A,滴加时间为2h;控制反应温度为82℃;
(4)待滴加反应结束后,将11g氨水(质量分数为20%)加入到反应器中,进行中和反应;
(5)向反应瓶中加入150g去离子水进行稀释,即可得到固含量为25.6%的有机磷改性的丙烯酸酯浆料。
实施例3:
有机磷改性的丙烯酸浆料的制备:
(1)将4.5g沙索蜡、0.6g甲基丙烯酸乙基磷酸酯(索尔维的RPM2060)、10g丙烯酸、4g甲基丙烯酸、1.6g甲基丙烯酸羟乙酯、15g丙烯酸甲酯、6.4g丙烯酸乙酯、6g丙烯酸丁酯、4.8g甲基丙烯酸甲酯、3g苯乙烯、4.8g甲基丙烯酸丁酯、4.2g丙烯酸酯硅油、0.9g偶氮二异庚腈,1.5g2,4-二苯基-4-甲基-1-戊烯、20g异丙醇和34g环己烷混合溶剂进行充分混合均匀,形成反应混合液A;
(2)向有回流、温度计、搅拌、加料口的反应器内加入步骤一配制的反应混合液A10.9g;逐渐升温至82℃,进行引发反应;
(3)待引发反应结束后,开始滴加步骤一剩余的反应混合液A,滴加时间为3h;控制反应温度为75℃;
(4)待滴加反应结束后,将3.48g氨水(质量分数为20%)和5.94g氢氧化钠加入到反应器中,进行中和反应;
(5)向反应瓶中加入240g去离子水进行稀释,即可得到固含量为20.56%的有机磷改性的丙烯酸酯浆料。
实施例4:
有机磷改性的丙烯酸浆料的制备:
(1)将1g蜂蜡、0.6g石蜡、0.35g甲基丙烯酰氧乙基磷酸酯、5g甲基丙烯酸、0.45g丙烯酰胺基异丙基磺酸钠、2g丙烯酸丁酯、9g丙烯酸甲酯、4g甲基丙烯酸丁酯、1.6g乙烯基聚硅氧烷、0.2g过氧化2-乙基己基酸叔戊酯,0.3g巯基乙酸、9.8g甲醇进行充分混合均匀,形成反应混合液A;
(2)向有回流、温度计、搅拌、加料口的反应器内加入步骤一配制的反应混合液A29.3g;逐渐升温至85℃,进行引发反应;
(3)待引发反应结束后,开始滴加步骤一剩余的反应混合液A,滴加时间为4h;控制反应温度为85℃;
(4)待滴加反应结束后,将3.09g氨基乙醇胺和1.6g二乙醇胺加入到反应器中,进行中和反应;
(5)向反应瓶中加入102g去离子水进行稀释,即可得到固含量为21.98%的有机磷改性的丙烯酸酯浆料。
实施例5:
(1)将0.9Kg棕榈蜡、0.4kg乙二醇甲基丙烯酸酯磷酸酯、5kg丙烯酸、0.8Kg甲基丙烯酸、2Kg丙烯酸丁酯、10Kg丙烯酸甲酯、5.9Kg甲基丙烯酸正丁酯、1.3KG甲基丙烯酸十八烷基酯、0.15kg过氧化苯甲酸叔丁酯,0.2Kg正十二烷基硫醇、20Kg乙醇混合溶剂进行充分混合均匀,形成反应混合液A;
(2)向有回流、温度计、搅拌、加料口的反应器内加入步骤一配制的反应混合液A27.6g;逐渐升温至75℃,进行引发反应;
(3)待引发反应结束后,开始滴加步骤一剩余的反应混合液A,滴加时间为4h;控制反应温度为85℃;
(4)待滴加反应结束后,将12.36gAMP-95和0.78g氢氧化钾加入到反应器中,进行中和反应;
(5)向反应瓶中加入176.6g去离子水进行稀释,即可得到固含量为21.9%的有机磷改性的丙烯酸酯浆料。
实施例6:
(1)将0.9Kg棕榈蜡、0.4kg乙二醇甲基丙烯酸酯磷酸酯、5kg丙烯酸、0.8Kg甲基丙烯酸、2Kg丙烯酸丁酯、10Kg丙烯酸甲酯、5.9Kg甲基丙烯酸正丁酯、1.3KG甲基丙烯酸十八烷基酯、0.15kg过氧化苯甲酸叔丁酯,0.2Kg正十二烷基硫醇、20Kg乙醇混合溶剂进行充分混合均匀,形成反应混合液A;
(2)向有回流、温度计、搅拌、加料口的反应器内加入步骤一配制的反应混合液A9.28Kg;逐渐升温至84℃,进行引发反应;
(3)待引发反应结束后,开始滴加步骤一剩余的反应混合液A,滴加时间为5h;控制反应温度为78℃;
(4)待滴加反应结束后,将10.5Kg三乙醇胺加入到反应器中,进行中和反应;
(5)向反应瓶中加入140KG去离子水进行稀释,即可得到固含量为20.3%的有机磷改性的丙烯酸酯浆料。
检测:
设置对比样:选择市售普通聚丙烯酸类浆料。
设置无磷对比样:即不添加有机磷单体,其余成分的添加和加工方式与实施例1均相同;
对上述实施例1-6和对比例1-2按照以下方式检测:
1、固含量:按照GB/T 1175-2002合成树脂乳液试验方法。
2、玻璃化转变温度Tg:采用差示扫描量热分析(DSC)测量浆膜的玻璃化转变温度,称取样品8~10mg,温度范围-100~100℃,升温速率10℃/min,氮气为保护气。
3、浆膜的制备:取15g浆料在60℃下4h,然后60℃下烘12h,然后在110℃下烘1h,取出后放置1h。
4、吸湿发粘:制备厚度为0.5mm的浆膜,裁成2*2cm尺寸,将裁好的浆膜放置在锡纸上,然后,置于相对湿度为90%,温度为70℃的恒温恒湿箱中,放置一周后,如果浆膜粘附在锡纸上视为吸湿发粘等级为1级;如果浆膜可从锡纸上取下,但是取下的过程比较困难,视为吸湿发粘等级为3级;如果浆膜可直接从锡纸盘中拿出,视为吸湿发粘等级为5级。
5、膨润率:取一块重量为W1的浆膜放入到50℃的恒温水浴中,泡30min后,用滤纸吸干表面水分,称重为W2;再放入到110℃的烘箱中烘3~4h,完全烘干后称重为W3;
膨润率=(W2-W1)/W1*100%;
水解率=(W1-W3)/W1*100%。
6、退浆:取一块制备好的浆膜,放入到0.5%NaOH沸腾溶液中,开始计时,直到浆膜消失,停止计时;超过10min浆膜未消失的,视为不合格。
7、消泡:在100mL的量筒中,加入40mL浆液,在1min内摇晃100次,记下此时的泡沫高度,1min后再次记下泡沫的高度,超过50ml为不合格。
8、抱合力:将上浆后的丝线,在抱合力测试仪上测试。
上述检测结果见下表:
由上表可知,本发明所制备的浆料具备有退浆快,不吸湿发粘,抱合力高等特点。
9、实施例1、对比样和无磷对比样的浆料进行红外检测:
红外谱图(FTIR):设备为Themo scientific Nicolet IS5,光谱范围为4000~400cm-1,扫描次数为32次;将浆料直接涂覆在KBr晶片上,利用红外灯照射挥发水分后测得,具体结果见图1:
由图1可知实施例1的谱图为最上端的线条,无磷对比样的谱图为最下端的线条,对比样的谱图为中间的线条,且实施例1的谱图中,1723cm-1为C=O的特征吸收峰;在1062cm-1处有明显的吸收峰,它是为P-O-C的伸缩振动特征吸收峰;1291cm-1为P=O的特征吸收峰,从红外谱图上说明了有机磷改性的丙烯酸浆料的合成。
需要说明的是,在本文中,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。
以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种有机磷改性的丙烯酸浆料,其特征在于,所述丙烯酸浆料由以下质量份物质组成:蜡0.57-1.9份、磷酸丙烯酸酯单体0.095-0.475份、含烯键的单体19-23.75份、引发剂0.095-0.665份、链转移剂0.019-0.225份、助溶剂7-15份、中和剂2.47-10份、去离子水46-73份;
其中所述含烯键单体为普通烯键单体、亲水性单体、疏水性单体按照质量比67.6-80.1∶17.9-25.2∶3.1-7.2组成。
2.根据权利要求1所述的一种有机磷改性的丙烯酸浆料,其特征在于:所述亲水性单体选自丙烯酸、甲基丙烯酸、丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯、甲基丙烯酸羟丙酯、丙烯酰胺、丙烯酰胺基异丙基磺酸钠、含烯丙烯的特种醇醚硫酸盐、烯丙基醚羟丙基磺酸盐的中至少一种;所述疏水性单体选自丙烯酸十八烷基酯、叔碳酸乙烯酯、丙烯酸酯硅油、乙烯基聚硅氧烷、硅烷偶联剂KH570之中的至少一种。
4.根据权利要求1所述的一种有机磷改性的丙烯酸浆料,其特征在于:所述的蜡为微晶蜡、蜂蜡、石蜡、沙索蜡、巴西棕榈蜡、氧化乙烯蜡等中的至少一种,且各种蜡的熔点为40~130℃。
5.根据权利要求1所述的一种有机磷改性的丙烯酸浆料,其特征在于:所述引发剂为偶氮二异丁腈、偶氮二异庚腈、过氧化苯甲酰、过氧化2-乙基己基酸叔丁酯、过氧化2-乙基己基酸叔戊酯、过氧化苯甲酸叔丁酯等中的至少一种。
6.根据权利要求1所述的一种有机磷改性的丙烯酸浆料,其特征在于:所述链转移剂为十二烷基硫醇、2,4-二苯基-4-甲基-1-戊烯、正辛硫醇、巯基乙酸、巯基乙醇、2-巯基丙酸异辛酯等中的至少一种。
7.根据权利要求1所述的一种有机磷改性的丙烯酸浆料,其特征在于:所述中和剂为氨水、三乙胺、氢氧化钠、氢氧化钾、二甲基乙醇胺、三乙醇胺、二乙醇胺、AMP-95、氨基乙醇胺中的至少一种。
8.一种如权利要求1-7任意所述有机磷改性的丙烯酸浆料的制备方法,其特征在于:所述制备方法包括以下步骤:
(1)混合处理:将蜡、磷酸丙烯酸酯单体、含烯键的单体、引发剂,链转移剂、助溶剂等充分混合均匀,制备成为反应混合液A;
(2)升温反应:将向有回流、温度计、搅拌、加料口的反应器内加入(1)中配制的反应混合液A质量份的5-50%,并升温引发反应,获得反应液备用;
(3)滴加反应:将剩余的混合液A滴加到上述反应液中,且滴加时间为2~5h,继续保温反应,得备用液;
(4)中和稀释:将上述备用液反应结束后加入中和剂进行中和反应,后加入去离子水进行稀释,得到有机磷改性的丙烯酸浆料。
9.根据权利要求5所述的一种有机磷改性的丙烯酸浆料的制备方法,其特征在于:所述步骤(2)和步骤(3)中的升温引发反应和保温反应的温度为70~85℃。
10.一种如权利要求1-7任意所述有机磷改性的丙烯酸浆料在纺织纤维类的上浆上的应用,其特征在于,所述有机磷改性的丙烯酸浆料用于锦纶、涤纶等合成纤维的上浆。
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CN111348883A (zh) * | 2020-03-13 | 2020-06-30 | 重庆中科建设(集团)有限公司 | 一种高抗裂、低吸水率的蒸压加气混凝土及其制备方法 |
CN114621385A (zh) * | 2020-12-11 | 2022-06-14 | 株洲飞鹿高新材料技术股份有限公司 | 一种高鲜映性的水性丙烯酸树脂及其制备方法 |
CN114292588A (zh) * | 2021-12-28 | 2022-04-08 | 东莞市贝特利新材料有限公司 | 一种高磨耗性有机硅涂料及其制备方法和应用 |
CN114940724A (zh) * | 2022-06-28 | 2022-08-26 | 扬州绿邦化工有限公司 | 一种改性羟基丙烯酸分散体及其制备方法 |
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