CN107988783B - 一种蚕丝无纺布用改性挠曲材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种蚕丝无纺布用改性挠曲材料及其制备方法，属于非织造布材料技术领域。本发明采用纯天然桑蚕丝，通过氯化钙和不同浓度乙酸溶液进行水浴处理，洗涤，再经过快速烘燥，使蚕丝内部应力快速发生变化，制备具有一定弯曲度的改性蚕丝。此处理后得到的改性蚕丝材料与原蚕丝纤维相比极大地提高了自身的弯曲度，而强力并无明显降低，能够解决其它通过涂层、共混、丝胶粘合等方法，单方面提高布料强力而造成布料的透气透湿、柔软度差的缺点。此改性蚕丝材料性能优异，温和不刺激，没有引入其它物质，能够充分发挥丝素纤维的良好性能，可以作为纯蚕丝无纺布的原材料，提高水刺蚕丝无纺布内蚕丝的纠缠率，提高单位面积的摩擦力，从而改善纯蚕丝无纺布产品强力不足的缺点。
Description
技术领域
本发明涉及一种蚕丝无纺布改性挠曲材料及其制备方法，属于非织造布材料技术领域。
背景技术
蚕丝是一种天然蛋白质纤维，含有对人体有益的18中氨基酸，蛋白质含量达97%以上，丝素是主体，丝胶包覆在丝素外面，起到保护的作用。丝素蛋白无毒无害，安全可靠，具有优异的生物相容性，适合开发改性成新材料。其中，含有的丝氨酸、苏氨酸能够延缓衰老，亮氨酸能够加速细胞的新陈代谢。蚕丝的这些优点，使得研究人员加深对其改性材料的研究，比如：浸渍、涂覆、接枝、共混等等，来赋予蚕丝不同的性能。
目前蚕丝作为加工水刺纯蚕丝无纺布原料时，容易造成布料强力不足，布料易撕裂等缺点。因此，研究人员对布料进行改性，目前的方法有：（1）通过涂覆、浸渍强力剂的方法，提高布料的强力性能，但是这样容易导致面料的透气透湿下降；（2）通过熔融法，将未脱胶蚕丝表面丝胶溶解，再进行干燥利用丝胶使蚕丝相互间粘合来提高布料的强力，但是此方法的得到的布料硬度偏大，柔软度很差；（3）通过饱和钙盐制备弯曲蚕丝的方法，提高蚕丝的弯曲程度，增加蚕丝之间的摩擦力，但是此处理后的蚕丝，弯曲程度不够，强力下降较多，限制布料的强力。（4）通过使用涤纶、天丝等纤维和蚕丝进行混纺制备无纺布，虽然布料强力提高，但是其实用价值就会大打折扣。
在本发明作出之前，中国发明专利（CN100379915）“含丝胶的蚕丝变性无纺布及其用途”中，采用戊二醛溶液将丝胶固定在蚕丝纤维上，同时加入表面活性剂使其柔软，虽然能够使蚕丝无纺布提高强力，但是在烘燥和冷却过程中，丝胶的熔融和凝结，将导致布料的手感较差，加入的表面活性剂可能溶出刺激皮肤，加入的戊二醛具有毒性，产生刺激，并引起生物相容性的下降。公开号为CN105671790A的中国发明专利提供了一种蚕丝热风无纺布面料，利用熔点为130℃的ES纤维的熔融粘结作用，将蚕丝无纺布和其相互粘结来起到增加强力的作用，但高温会破坏蚕丝纤维，同时化学纤维ES纤维的加入，可能降低纯蚕丝的亲肤性和生物相容性。
发明内容
本发明针对现有蚕丝无纺布面料存在的不足，提供一种即能充分保持丝素蛋白材料的生物相容性和强力，又具有较高挠曲性的蚕丝无纺布用改性挠曲材料及其制备方法。
实现本发明目的的技术方案是提供一种蚕丝无纺布用改性挠曲材料的制备方法，以家蚕丝为原料，依次经脱胶、洗涤、干燥处理后，再进行以下步骤的加工：
（1）将脱胶干燥后的家蚕丝浸泡于含有蚕丝保护剂的氯化钙和乙酸混合溶液中，在温度为60℃～90℃的条件下处理10 min～60min，蚕丝吸收溶液后得到溶胀蚕丝；所述蚕丝保护剂为包括硫酸钠，甘油，糖精和蔗糖的复配物，蚕丝保护剂用量为蚕丝质量的1%～3%；所述氯化钙溶液为6～8 mol/L，乙酸溶液为0.04～0.7 mol/L；
（2）将溶胀蚕丝经压辊轧压，去除多余溶胀液，压辊的压力为0.1 MPa～ 0.4MPa；
（3）将步骤（2）处理后的蚕丝立即用水充分洗涤，至洗出液的pH值大于6；
（4）将洗涤后的蚕丝置于温度为100℃～110℃的烘箱中烘燥至恒重，得到一种蚕丝无纺布用改性挠曲材料。
本发明所述蚕丝保护剂中，按质量计，包括30%～60%的硫酸钠， 20%～50%的蔗糖，5%～10%的甘油，0.1%～5%的糖精。
本发明技术方案还包括按上述制备方法得到的一种蚕丝无纺布用改性挠曲材料。
蚕丝无纺布用改性挠曲材料的蚕丝纤维的弯曲度为10～30%，单丝强力为5～6cN。
本发明的原理是：利用蚕丝具有一定的吸收酸液的特点，使其浸渍于稀醋酸中，吸收稀醋酸后，发生部分溶胀，为了提高其溶胀度，还加入了氯化钙，促使醋酸分子进入蚕丝内部，使蚕丝进一步溶胀，在蚕丝保护剂的保护下，控制蚕丝只发生溶胀而尽量减少蚕丝蛋白的降解。溶胀的蚕丝经过水洗去除醋酸、氯化钙以及蚕丝保护剂，其后快速干燥。由于溶胀的膨胀应力与干燥收缩时应力的不均匀，导致蚕丝弯曲卷绕，形成具有一定绕曲的蚕丝材料。本发明采用提高蚕丝弯曲度方法来制备改性蚕丝改性材料，从产品原料着手进行改性，提高蚕丝的弯曲程度，进而增大产品内部蚕丝之间的纠缠性能，适合于作为生产纯蚕丝无纺布的原料，可以用于生物敷料，蚕丝面膜，蚕丝卫生巾等产品。
与现有纯蚕丝无纺布原料相比，本发明的优势在于：
（1）本发明通过对蚕丝进行氯化钙/乙酸溶液处理，能够大幅度提高蚕丝的弯曲程度，其弯曲度能提高到10～30%，而且不会伤害蚕丝自身的强力。
（2）从蚕丝无纺布原材料本身着手改性，能够解决其它通过涂层、共混、丝胶粘合等方法，只考虑提高强力而造成蚕丝无纺布的透气透湿、柔软度、亲肤性下降的缺点。
（3）本发明制备得到的蚕丝无纺布改性材料，无毒无害，无任何物质的引入，在解决纯蚕丝无纺布强力不足，提高无纺布料的撕裂性能的同时，能够充分保持丝素蛋白材料的生物相容性。
附图说明
图1是未处理样品的蚕丝形态照片；
图2是实施例一样品的蚕丝形态照片；
图3是实施例二样品的蚕丝形态照片；
图4是实施例三样品的蚕丝形态照片；
图5是实施例四样品的蚕丝形态照片；
图6是本发明各实施例提供的样品与未处理蚕丝的弯曲度检测结果对比图；
图7是本发明各实施例提供的样品与未处理蚕丝的强度检测结果对比图。
具体实施方式
下面结合附图和实施例对本发明技术方案作进一步说明。
实施例一：
1.取1公斤脱胶干燥后的家蚕丝，浸泡在5000毫升含有20克蚕丝保护剂的0.04mol/L稀醋酸、6.7 mol/L氯化钙溶液中50 min, 温度60℃，吸收酸液获得溶胀蚕丝；其中蚕丝保护剂为含有58%质量的硫酸钠，含有35%质量的蔗糖，含有6%质量的甘油，含有1%质量的糖精。
2.将溶胀蚕丝通过压辊去除多余酸液，压辊的压力为0.2 MPa；
3.取出干燥过的蚕丝，用水充分洗涤，直到洗出液中的pH值升高到6.5；
4.将清洗过的蚕丝，放入100℃烘箱中快速烘燥至恒重，获得具有一定弯曲度的蚕丝，可用于蚕丝无纺布的制造。
处理前后的蚕丝形态参见附图1和附图2。
弯曲度的检测：将处理后的蚕丝放在黑绒版上，一端固定，将蚕丝悬垂，测量获得处理后的长度。再将蚕丝另一端施加一定的应力，使其伸直测量其原有长度，计算得出弯曲度=（原有长度-处理后长度）/原有长度*100%。通过检测，本实施例获得的蚕丝材料的弯曲度为14%，参见附图6。单丝的强力检测结果参见附图7。
实施例二：
1.取2公斤脱胶干燥后的家蚕丝，浸泡在10升含有40克蚕丝保护剂的0.21mol/L稀醋酸、7.0mol/L氯化钙溶液中30 min, 温度70℃，吸收酸液获得溶胀蚕丝；其中蚕丝保护剂为含有45%质量的硫酸钠，含有45%质量的蔗糖，含有8%质量的甘油，含有2%质量的糖精。
2.将溶胀蚕丝通过压辊去除多余酸液，压辊的压力为0.25 MPa；
3.取出干燥过的蚕丝，用水充分洗涤，直到洗出液中的pH值升高到6.2；
4.将清洗过的蚕丝，放入101℃烘箱中快速烘燥至恒重，获得具有一定弯曲度的蚕丝，可用于蚕丝无纺布的制造。
处理前后的蚕丝形态参见附图1和附图3。
弯曲度的检测：将处理后的蚕丝放在黑绒版上，一端固定，将蚕丝悬垂，测量获得处理后的长度。再将蚕丝另一端施加一定的应力，使其伸直测量其原有长度，计算得出弯曲度=（原有长度-处理后长度）/原有长度*100%。通过检测，本实施例获得的蚕丝材料的弯曲度为18%，参见附图6。单丝的强力检测结果参见附图7。
实施例三：
1.取2公斤脱胶干燥后的家蚕丝，浸泡在10升含有40克蚕丝保护剂的0.42mol/L稀醋酸、7.2mol/L氯化钙溶液中40 min, 温度65℃，吸收酸液获得溶胀蚕丝；其中蚕丝保护剂为含有42%质量的硫酸钠，含有50%质量的蔗糖，含有7%质量的甘油，含有1%质量的糖精。
2.将溶胀蚕丝通过压辊去除多余酸液，压辊的压力为0.25 MPa；
3.取出干燥过的蚕丝，用水充分洗涤，直到洗出液中的pH值升高到6.1；
4.将清洗过的蚕丝，放入101℃烘箱中快速烘燥至恒重，获得具有一定弯曲度的蚕丝，可用于蚕丝无纺布的制造。
处理前后的蚕丝形态参见附图1和附图4。
弯曲度的检测：将处理后的蚕丝放在黑绒版上，一端固定，将蚕丝悬垂，测量获得处理后的长度。再将蚕丝另一端施加一定的应力，使其伸直测量其原有长度，计算得出弯曲度=（原有长度-处理后长度）/原有长度*100%。通过检测，本实施例获得的蚕丝材料的弯曲度为20%，参见附图6。单丝的强力检测结果参见附图7。
实施例四：
1.取2公斤脱胶干燥后的家蚕丝，浸泡在10升含有40克蚕丝保护剂的0.62mol/L稀醋酸、7.4mol/L氯化钙溶液中35 min, 温度76℃，吸收酸液获得溶胀蚕丝；其中蚕丝保护剂为含有40%质量的硫酸钠，含有51%质量的蔗糖，含有8.1%质量的甘油，含有0.9%质量的糖精。
2.将溶胀蚕丝通过压辊去除多余酸液，压辊的压力为0.25 MPa；
3.取出干燥过的蚕丝，用水充分洗涤，直到洗出液中的pH值升高到6.4；
4.将清洗过的蚕丝，放入101℃烘箱中快速烘燥至恒重，获得具有一定弯曲度的蚕丝，可用于蚕丝无纺布的制造。
处理前后的蚕丝形态参见附图1和附图5。
弯曲度的检测：将处理后的蚕丝放在黑绒版上，一端固定，将蚕丝悬垂，测量获得处理后的长度。再将蚕丝另一端施加一定的应力，使其伸直测量其原有长度，计算得出弯曲度=（原有长度-处理后长度）/原有长度*100%。通过检测，该实施例获得的蚕丝材料的弯曲度为26%，参见附图6。单丝的强力检测结果参见附图7。
参见附图1至附图5，是本发明各实施例中处理前后蚕丝形态的对比照片；其中，A为未处理样品，B为实施例一样品，C 为实施例二样品，D为实施例三样品，E为实施例四样品，由图可以看到，处理后蚕丝弯曲度大大提高。
参见附图6，是本发明各实施例提供的样品与未处理蚕丝的弯曲度检测结果对比图。由图6可以看到，未处理蚕丝的弯曲度仅为5%左右，处理后蚕丝的弯曲度大大提高。
参见附图7，是本发明各实施例提供的样品与未处理蚕丝的强度检测结果对比图。由图7可以看出，蚕丝经过处理后强度下降不明显。
Claims (4)
1.一种蚕丝无纺布用改性挠曲材料的制备方法，以家蚕丝为原料，依次经脱胶、洗涤、干燥处理后，其特征在于再进行以下步骤的加工：
（1）将脱胶干燥后的家蚕丝浸泡于含有蚕丝保护剂的氯化钙和乙酸混合溶液中，在温度为60℃～90℃的条件下处理10 min～60min，蚕丝吸收溶液后得到溶胀蚕丝；所述蚕丝保护剂为包括硫酸钠，甘油，糖精和蔗糖的复配物，蚕丝保护剂用量为蚕丝质量的1%～3%；所述氯化钙溶液为6～8 mol/L，乙酸溶液为0.04～0.7 mol/L；
（2）将溶胀蚕丝经压辊轧压，去除多余溶胀液，压辊的压力为0.1 MPa～ 0.4MPa；
（3）将步骤（2）处理后的蚕丝立即用水充分洗涤，至洗出液的pH值大于6；
（4）将洗涤后的蚕丝置于温度为100℃～110℃的烘箱中烘燥至恒重，得到一种蚕丝无纺布用改性挠曲材料。
2.根据权利要求1所述的一种蚕丝无纺布用改性挠曲材料的制备方法，其特征在于：所述蚕丝保护剂中，按质量计，包括30%～60%的硫酸钠， 20%～50%的蔗糖，5%～10%的甘油，0.1%～5%的糖精。
3.按权利要求1制备方法得到的一种蚕丝无纺布用改性挠曲材料。
4.根据权利要求3所述的一种蚕丝无纺布用改性挠曲材料，其特征在于：蚕丝纤维的弯曲度为10～30%，单丝强力为5～6cN。
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| CN104233778A (zh) * | 2014-09-11 | 2014-12-24 | 苏州印丝特纺织数码科技有限公司 | 一种蚕丝织物的盐缩整理方法 |
| CN105256544A (zh) * | 2015-10-28 | 2016-01-20 | 南通纺织丝绸产业技术研究院 | 一种高性能天然蚕丝纤维及其制备方法 |
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| CN104233778A (zh) * | 2014-09-11 | 2014-12-24 | 苏州印丝特纺织数码科技有限公司 | 一种蚕丝织物的盐缩整理方法 |
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