CN117127422A - 一种用于涤纶的基于改性腰果酚的染色增效剂的制备方法 - Google Patents
一种用于涤纶的基于改性腰果酚的染色增效剂的制备方法 Download PDFInfo
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Abstract
本发明涉及纺织助剂领域，公开一种用于涤纶的基于改性腰果酚的染色增效剂的制备方法，先由腰果酚和马来酸酐反应制备得到马来酸双腰果酚酯中间体，再与腰果酚聚氧乙烯醚，聚乙二醇油酸酯复配制得涤纶染色增效剂。本发明所制备的涤纶染色增效剂能提升分散染料的分散性、缓染性和移染性，有效解决实际工艺中因升温过快造成的色花、染色不匀的问题。
Description
技术领域
本发明涉及纺织助剂领域，尤其是涉及一种用于涤纶的基于改性腰果酚的染色增效剂的制备方法。
背景技术
腰果酚是一种从天然腰果壳油中提炼而成的植物多烯酚。作为一种生物基原料，腰果酚可以代替或者部分代替苯酚用于制造环氧固化剂、液体酚醛树脂、液体或者粉末状的热固性酚醛树脂。此外，许多研究者对其进行改性，并广泛应用于表面活性剂领域。已有研究资料显示，采用腰果酚与环氧乙烷反应，可制备非离子型腰果酚聚氧乙烯醚表面活性剂；采用氨基磺酸与腰果酚反应，可制备腰果酚磺酸盐表面活性剂；采用马来酸酐与腰果酚进行反应，可制备腰果酚羧酸盐表面活性剂。这些类型的表面活性剂可作为工业清洗剂、分散剂或织物匀染剂等。
在纺织助剂领域，腰果酚结构中的苯环与长链烯烃均可与涤纶纤维发生吸附，与此同时，该结构对分散染料也具有一定的亲和力。但是，由于结构中缺少酯基，使得其在结构上与涤纶结构仍存在较大的差异。也正是这种差异，使其在涤纶染色中的增效作用受到限制。
现有技术中CN109056371A公开一种分散染料色花防止剂，该方法主要采用分散组分和移染组分来提高涤纶高温染色的染色均匀性，分散组份包括油酸聚氧乙烯酯、椰子油聚氧乙烯酯、蓖麻油聚氧乙烯醚、腰果酚聚氧乙烯醚中的至少一种；所述移染组份包括肉桂酸苄酯、水杨酸苄酯、二乙二醇二水杨酸苄酯、马来酸二苄酯中的至少一种。因此，尚未有腰果酚酯与腰果酚聚氧乙烯醚来改善涤纶染色效果的相关报道。
发明内容
本发明所要解决的技术问题是克服上述现有技术存在的缺陷，提供一种用于涤纶的基于改性腰果酚的染色增效剂的制备方法。
为了实现上述目的，本发明采用以下技术方案：
A: 按质量份进行配比，将600～610份腰果酚、95～105份马来酸酐加入到反应容器中，开启搅拌，升温至90～100℃，在此温度下保温反应3～5小时，然后将5～10份对甲苯磺酸加到反应容器中，开启真空，在真空度-0.08MPa～-0.095MPa和温度90～100℃下保温反应2～4小时，制得马来酸双腰果酚酯，其反应路径如下：
其中n=0，2，4，6。
B: 将5～15份马来酸双腰果酚酯、20～35份腰果酚聚氧乙烯醚、15～35份聚乙二醇油酸酯、10～25份溶剂加入到装有冷凝回流装置的反应容器中，开启搅拌，混合均匀后缓慢加入10～25份去离子水，搅拌均匀后制得染色增效剂。
作为优选，所述腰果酚聚氧乙烯醚结构中的环氧乙烷（EO）链段数量为5～12。作为优选，所述聚乙二醇油酸酯为聚乙二醇单油酸酯、聚乙二醇双油酸酯中的一种。
进一步地，所述聚乙二醇油酸酯中聚乙二醇为PEG400或PEG600。
所述溶剂为异丙醇、乙二醇单丁醚、二乙二醇单丁醚中的一种。
由于上述技术方案的运用，本发明具有如下优点：
本发明采用生物基腰果酚为原料制备马来酸双腰果酚酯，该结构的双酯基、双苯环以及双长链烯烃结构相比于腰果酚，具有更强的亲和力。将其应用于涤纶分散染色中，双酯结构对涤纶具有更强的吸附作用，能提升对分散染料的缓染性，有效解决实际工艺中因升温过快造成的色花问题。与此同时，马来酸双腰果酚酯对涤纶纤维有一定的增塑作用，降低染色时涤纶的玻璃化温度，提高对纤维的溶胀性，使纤维无定型区内的分子链运动加强，促进染料向纤维内部扩散，提高上染率和染色牢度；再者，马来酸双腰果酚酯与腰果酚聚氧乙烯醚、聚乙二醇油酸酯所形成的复配增效体系能够减少分散染料的聚集，对已经聚集的染料进行增溶、分散，并重新上染，达到修色匀染的目的。
附图说明
图1为本发明专利中马来酸双腰果酚酯的红外光谱图。
实施方式
下面通过具体实施方式对本发明做进一步描述。
实施例1
A：按质量份进行配比，将600份腰果酚、100份马来酸酐加入到反应容器中，开启搅拌，升温至95℃，在此温度下保温反应3小时，然后将5份对甲苯磺酸加到反应容器中，开启真空，在真空度-0.095MPa、温度100℃下保温反应4小时，制得马来酸双腰果酚酯。
B：将10份马来酸双腰果酚酯、30份腰果酚聚氧乙烯醚、30份聚乙二醇油酸酯、15份溶剂加入到装有冷凝回流装置的反应容器中，开启搅拌，混合均匀后缓慢加入15份去离子水，搅拌均匀后制得染色增效剂。
实施例2
A：按质量份进行配比，将610份腰果酚、95份马来酸酐加入到反应容器中，开启搅拌，升温至100℃，在此温度下保温反应3小时，然后将5份对甲苯磺酸加到反应容器中，开启真空，在真空度-0.095MPa、温度100℃下保温反应4小时，制得马来酸双腰果酚酯。
B：将15份马来酸双腰果酚酯、25份腰果酚聚氧乙烯醚、30份聚乙二醇油酸酯、20份溶剂加入到装有冷凝回流装置的反应容器中，开启搅拌，混合均匀后缓慢加入10份去离子水，搅拌均匀后制得染色增效剂。
实施例3
A：按质量份进行配比，将600份腰果酚、95份马来酸酐加入到反应容器中，开启搅拌，升温至90℃，在此温度下保温反应3小时，然后将5份对甲苯磺酸加到反应容器中，开启真空，在真空度-0.095MPa、温度100℃下保温反应4小时，制得马来酸双腰果酚酯。
B：将15份马来酸双腰果酚酯、30份腰果酚聚氧乙烯醚、25份聚乙二醇油酸酯、15份溶剂加入到装有冷凝回流装置的反应容器中，开启搅拌，混合均匀后缓慢加入15份去离子水，搅拌均匀后制得染色增效剂。
对比例1
将35份腰果酚聚氧乙烯醚、35份聚乙二醇油酸酯、15份溶剂加入到装有冷凝回流装置的反应容器中，开启搅拌，混合均匀后缓慢加入15份去离子水，搅拌均匀后即可。
应用评价工艺：
低温染色性
分散红F3BS 2.0%
染浴pH 4.5~5
染色增效剂用量 0.25g/L
浴比 1:10
升温速率 2.0℃/min
染色温度 100~130℃
染色时间 30min
采用上述染色工艺，测试在100℃，110℃，120℃，130℃时的颜色深度（K/S值），空白对照为不加增效剂，实验结果见表1。
表1 低温染色性结果对比
移染性
移染性测试依照行业标准HG/T4263-2011《纺织染整助剂 涤用匀染剂移染性能的测定》进行，空白对照为不加增效剂，结果见表2。
表2 移染性测试结果对比
3、缓染性
缓染性依照行业标准HG/T4262-2011《纺织染整助剂 涤用匀染剂缓染性能的测定》进行测试，空白对照为不加增效剂，结果如表3所示。
表3 缓染性测试结果对比
结合表1到表的3结果可知，本发明实施例的染色增效剂具有较好的低温染色效果。并且相比较对比例，缓染性和移染性均有提升。
4、染色牢度
用于涤纶的基于改性腰果酚的染色增效剂对染色牢度的影响见表4
表4 涤纶染色增效剂对染色牢度的影响
从表4结果可知，本发明实施例的染色增效剂加入染浴中后，对织物染色的摩擦牢度、皂洗牢度影响不大，说明该增效剂对染料牢度无不良影响。
5、 红外光谱分析
图1中3008cm-1和1408cm-1处为不饱和烯烃的特征吸收峰，2923cm-1和2853cm-1处为甲基和亚甲基的特征吸收峰。对比两条曲线可知，马来酸双腰果酚酯在1730cm-1处出现的新的吸收峰为酯键的特征峰，同时3334cm-1处羟基的特征峰消失，说明腰果酚的酚羟基与马来酸酐反应较完全，目标产物成功获得。
本发明的技术范围不仅仅局限于上述说明中的内容，本领域技术人员可以在不脱离本发明技术思想的前提下，对上述实施例进行多种变形和修改，而这些变形和修改均应当属于本发明的范围内。
Claims (4)
1.一种用于涤纶的基于改性腰果酚的染色增效剂的制备方法，其特征在于包括如下步骤：
A: 按质量份进行配比，将600～610份腰果酚、95～105份马来酸酐加入到反应容器中，开启搅拌，升温至90～100℃，在此温度下保温反应3～5小时，然后将5～10份对甲苯磺酸加到反应容器中，开启真空，在真空度-0.08MPa～-0.095MPa和温度90～100℃下，保温反应2～4小时，制得马来酸双腰果酚酯，其结构通式如下所示：
其中n=0，2，4，6
B: 将5～15份马来酸双腰果酚酯、20～35份腰果酚聚氧乙烯醚、15～35份聚乙二醇油酸酯、10～25份溶剂加入到装有冷凝回流装置的反应容器中，开启搅拌，混合均匀后缓慢加入10～25份去离子水，搅拌均匀后制得染色增效剂。
2.根据权利要求1所述的一种用于涤纶的基于改性腰果酚的染色增效剂的制备方法，其特征在于：所述腰果酚聚氧乙烯醚结构中的环氧乙烷（EO）链段数量为5～12，所述聚乙二醇油酸酯为聚乙二醇单油酸酯、聚乙二醇双油酸酯中的一种，所述溶剂为异丙醇、乙二醇单丁醚、二乙二醇单丁醚中的一种。
3.根据权利要求2所述的一种用于涤纶的基于改性腰果酚的染色增效剂的制备方法，其特征在于：所述聚乙二醇油酸酯中的聚乙二醇为PEG400或PEG600。
4.一种用于涤纶的基于改性腰果酚的染色增效剂，其特征在于：通过权利要求1-3中所述的制备方法获得。
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