CN115233459B - 一种白鸭绒脱脂除菌工艺 - Google Patents
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Abstract
Description
技术领域
本发明涉及羽绒加工技术领域,具体涉及一种白鸭绒脱脂除菌工艺。
背景技术
羽绒是一种保暖性极佳的天然材料,与之相比而言,棉花、蚕丝、化纤等纤维都是线性的,长期使用会出现板结,从而影响保暖性能和舒适感;而羽绒是“羽”和“绒”的混合物,绒朵是立体球状,不会有板结的问题。但羽绒直接来源鹅鸭身上,是一种动物性蛋白纤维,并伴有动物性脂肪,因此携带大量的污渍和多种致病微生物,若不能处理干净,则会危及人们的健康。
现有的抗菌羽绒的生产工序一般包括以下步骤:预分-除灰-精分-初洗-洗涤-脱水-烘干-冷却-包装工序;传统的对羽绒进行脱脂抗菌的工序中通过采用三氯异氰尿酸等药剂,在烘干过程中对羽绒进行处理;这种方法虽然能有效除菌,但极强的氧化性会使羽绒的蓬松性能减弱。CN1023525688公开一种抑菌功能羽绒的整理方法,其采用壳聚糖整理到羽绒纤维中,不仅可以获得抗菌防霉、除臭吸湿的效果,同时能保证羽绒的蓬松度较高。但事实上壳聚糖属于溶出型抗菌整理剂,缓慢溶出达到抗菌效果。因此,经壳聚糖整理后的织物在连续使用一段时间后,抗菌性能会逐渐丧失。
发明内容
针对现有技术中的不足之处,本发明基于壳聚糖对其进行改性得到N-双胍壳聚糖和p(AM-co-ALS)接枝壳聚糖,并结合含纳米氧化锌颗粒的有机硅季铵盐,其对羽绒进行整理,能有效杀菌脱脂。
为实现上述目的,本发明提供如下技术方案:
一种白鸭绒脱脂除菌工艺,包括如下步骤:
S1、白鸭绒前处理:预分-除灰-精分-初洗;
S2、配制整理液:壳聚糖衍生物、有机硅季铵盐按照1~3:1的质量比分散在水中,得到5g/L的整理液;
S3、精洗:将前处理后的白鸭绒脱水浸渍于整理液中,浸轧处理后,清水漂洗,脱水烘干;
进一步地,所述p(AM-co-ALS)接枝壳聚糖的制备过程如下:
1)以丙烯酰胺和烯丙基磺酸钠为单体,在4-氰基-4(硫代苯甲酰)戊酸作链转移剂和偶氮二异丁腈作引发剂条件下聚合,得到p(AM-co-ALS);
2)壳聚糖通过苯甲醛与氨基的缩合反应保护氨基,之后与p(AM-co-ALS)进行酯化反应,反应完成后脱除苯甲醛得到p(AM-co-ALS)接枝壳聚糖。
进一步地,所述步骤S1中丙烯酰胺、烯丙基磺酸钠、4-氰基-4(硫代苯甲酰)戊酸和偶氮二异丁腈的摩尔比为10~30:5~15:1:0.02。
进一步地,所述N-双胍壳聚糖和p(AM-co-ALS)接枝壳聚糖的质量比为3~5:7~5。
进一步地,所述有机硅季铵盐的制备过程如下:
1)在无水乙醇中分散纳米氧化锌,超声分散1h,后向其中加入γ-氯丙基三乙氧基硅烷,升温至40~50℃,回流搅拌2h,抽滤,无水乙醇洗涤,烘干得ZnO/KH230;
2)在反应瓶中加入六亚甲基四胺,加入吡啶使其完全溶解;将ZnO/KH230超声分散在甲苯溶液中,之后加到反应瓶中,设置温度110℃,微波加热回流5~10h,反应结束后降温静置,丙酮重结晶,即得有机硅季铵盐。
进一步地,所述纳米氧化锌与γ-氯丙基三乙氧基硅烷的质量比为2:1;六亚甲基四胺与ZnO/KH230的质量比为1:2。
进一步地,所述精洗过程中温度设置为70~80℃,保温30~100min。
本发明的有益效果是:本案通过对常规的羽绒处理工艺中精洗过程的改进,以自制的壳聚糖衍生物以及有机硅季铵盐配制整理液,对羽绒整理后能有效提升抗菌性和脱脂率,处理工艺简单。
具体实施方式
下面将结合实施例对本发明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做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。
此外,下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
实施例
本案中所用原材料如无特殊说明,均可从市场直接购得。
1)在反应瓶中加入20mmol丙烯酰胺、10mmol烯丙基磺酸钠、1mmol4-氰基-4(硫代苯甲酰)戊酸和0.2mmol偶氮二异丁腈,冷冻-抽气-充氮重复三次,60℃下反应2h;得到p(AM-co-ALS)1,Mn=3100g/mol,m=17,n=6;
改变反应投料比,得到:
p(AM-co-ALS)2,Mn=2200g/mol,m=6,n=15;
p(AM-co-ALS)3,Mn=2700g/mol,m=13,n=8;
p(AM-co-ALS)4,Mn=4400g/mol,m=25,n=7;
2)壳聚糖(脱乙酰度91.5%,平均分子量3000)通过苯甲醛与氨基的缩合反应保护氨基,将4g壳聚糖分散于甲醇水溶液中,滴加含15ml的苯甲醛甲醇溶液,升温至50℃,回流反应4h,乙醇索提得到氨基保护壳聚糖;取2g分散于DMF中,加入DCC,氮气保护,加入等质量的p(AM-co-ALS),低速搅拌,滴加溶解有DMAP的DMF溶液,常温搅拌48h进行酯化反应,反应完成后脱除苯甲醛得到p(AM-co-ALS)接枝壳聚糖,对应p(AM-co-ALS)1~4,将最终产物编号为p(AM-co-ALS)/CS-1、p(AM-co-ALS)/CS-2、p(AM-co-ALS)/CS-3、p(AM-co-ALS)/CS-4。
本案中对壳聚糖进行改性,首先制备了N-双胍壳聚糖,相较于壳聚糖具备更高的抗菌性,使之能在较大的pH值范围内保持正电性,提高分子的稳定性;此外,以烯丙基磺酸钠和丙烯酰胺的聚合物接枝改性壳聚糖,同样可以提高抗菌性,并且磺酸基的负电性与N-双胍壳聚糖通过静电吸附,结合度高,提高耐久性。引入有磺酸基的壳聚糖在一定程度上具有表面活性功能,在精洗过程中进一步起到去除羽绒中油脂含量的作用,降低羽绒中的残脂率。
有机硅季铵盐的制备过程如下:
1)在50ml无水乙醇中分散2g纳米氧化锌,超声分散1h,后向其中加入1gγ-氯丙基三乙氧基硅烷,升温至40~50℃,回流搅拌2h,抽滤,无水乙醇洗涤,烘干得ZnO/KH230;
2)在反应瓶中加入1.5g六亚甲基四胺,加入30ml吡啶使其完全溶解;将3g ZnO/KH230超声分散在甲苯溶液中,之后加到反应瓶中,设置温度110℃,微波加热回流5~10h,反应结束后降温静置,丙酮重结晶,即得有机硅季铵盐。
有机硅季铵盐类抗菌剂属于非溶出型抗菌剂,耐久性好,能有效弥补壳聚糖耐久性差的问题,进而避免抗菌失效的问题;本案中以六亚甲基四胺和硅烷偶联剂合成一种多头有机硅季铵盐,抑菌效果好,且反应过程中γ-氯丙基三乙氧基硅烷偶联剂起到架桥作用将纳米氧化锌颗粒包裹在有机硅当中,无机和有机的复配,更进一步提高了抗菌性,使羽绒有更加持久的抗菌效果。复配的抗菌剂形成的整理液对羽绒的除菌效果好,使用量少,更加经济高效。
一种白鸭绒脱脂除菌工艺,包括如下步骤:
S1、白鸭绒前处理:预分-除灰-精分-初洗;
S2、配制整理液:壳聚糖衍生物、有机硅季铵盐按照1~3:1的质量比分散在水中,得到5g/L的整理液;
S3、精洗:将前处理后的白鸭绒脱水浸渍于整理液中,设置温度为70~80℃,保温30~100min,清水漂洗,脱水烘干;
实施例1:
按照上述白鸭绒脱脂除菌工艺,其中所述整理液中N-双胍壳聚糖与p(AM-co-ALS)/CS-1的质量比为3:7,二者质量与有机硅季铵盐的质量比为1:1。
实施例2:
按照上述白鸭绒脱脂除菌工艺,其中所述整理液中N-双胍壳聚糖与p(AM-co-ALS)/CS-1的质量比为5:5,二者质量与有机硅季铵盐的质量比为2:1。
实施例3:
按照上述白鸭绒脱脂除菌工艺,其中所述整理液中N-双胍壳聚糖与p(AM-co-ALS)/CS-2的质量比为3:7,二者质量与有机硅季铵盐的质量比为1:1。
实施例4:
按照上述白鸭绒脱脂除菌工艺,其中所述整理液中N-双胍壳聚糖与p(AM-co-ALS)/CS-3的质量比为3:7,二者质量与有机硅季铵盐的质量比为1:1。
实施例5:
按照上述白鸭绒脱脂除菌工艺,其中所述整理液中N-双胍壳聚糖与p(AM-co-ALS)/CS-4的质量比为3:7,二者质量与有机硅季铵盐的质量比为1:1。
实施例6:
按照上述白鸭绒脱脂除菌工艺,其中所述整理液中N-双胍壳聚糖与p(AM-co-ALS)/CS-1的质量比为3:7,且不含有机硅季铵盐。
实施例7:
按照上述白鸭绒脱脂除菌工艺,其中所述整理液中N-双胍壳聚糖与有机硅季铵盐的质量比为1:1,不含p(AM-co-ALS)/CS。
按照GB/T14272-2011测试羽绒的残脂率,按照FZ/T 73023-2006测试抗菌性,记录在表1中。
表1
从上表中可以看出本案对白鸭绒的处理工艺可以有效对羽绒脱脂除菌,整理液中p(AM-co-ALS)/CS-4对脱脂的影响起到决定性作用,并且结构式中烯丙基磺酸钠的重复单元数在10~20以内效果最佳,低于10抗菌性较低,脱脂效果减弱;但高于20的时候,磺酸基富余,负电性增加,排斥作用增加,导致抗菌性下降。
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节。
Claims (6)
1.一种白鸭绒脱脂除菌工艺,其特征在于,包括如下步骤:
S1、白鸭绒前处理:预分-除灰-精分-初洗;
S2、配制整理液:壳聚糖衍生物、有机硅季铵盐按照1~3:1的质量比分散在水中,得到5g/L的整理液;
S3、精洗:将前处理后的白鸭绒脱水浸渍于整理液中,浸轧处理后,清水漂洗,脱水烘干;
所述有机硅季铵盐的制备过程如下:
1)在无水乙醇中分散纳米氧化锌,超声分散1h,后向其中加入γ-氯丙基三乙氧基硅烷,升温至40~50℃,回流搅拌2h,抽滤,无水乙醇洗涤,烘干得ZnO/KH230;
2)在反应瓶中加入六亚甲基四胺,加入吡啶使其完全溶解;将ZnO/KH230超声分散在甲苯溶液中,之后加到反应瓶中,设置温度110℃,微波加热回流5~10h,反应结束后降温静置,丙酮重结晶,即得有机硅季铵盐。
2.如权利要求1所述的白鸭绒脱脂除菌工艺,其特征在于,所述p(AM-co-ALS)接枝壳聚糖的制备过程如下:
1)以丙烯酰胺和烯丙基磺酸钠为单体,在4-氰基-4(硫代苯甲酰)戊酸作链转移剂和偶氮二异丁腈作引发剂条件下聚合,得到p(AM-co-ALS);
2)壳聚糖通过苯甲醛与氨基的缩合反应保护氨基,之后与p(AM-co-ALS)进行酯化反应,反应完成后脱除苯甲醛得到p(AM-co-ALS)接枝壳聚糖。
3.如权利要求2所述的白鸭绒脱脂除菌工艺,其特征在于,所述步骤S1中丙烯酰胺、烯丙基磺酸钠、4-氰基-4(硫代苯甲酰)戊酸和偶氮二异丁腈的摩尔比为10~30:5~15:1:0.02。
4.如权利要求1所述的白鸭绒脱脂除菌工艺,其特征在于,所述N-双胍壳聚糖和p(AM-co-ALS)接枝壳聚糖的质量比为3~5:7~5。
5.如权利要求1所述的白鸭绒脱脂除菌工艺,其特征在于,所述纳米氧化锌与γ-氯丙基三乙氧基硅烷的质量比为2:1;六亚甲基四胺与ZnO/KH230的质量比为1:2。
6.如权利要求1所述的白鸭绒脱脂除菌工艺,其特征在于,所述精洗过程中温度设置为70~80℃,保温30~100min。
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