CN107059431A - 一种栀子果中蓝色色素的提取及其对纺织品染色的方法 - Google Patents
一种栀子果中蓝色色素的提取及其对纺织品染色的方法 Download PDFInfo
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Abstract
本发明公开一种栀子果中蓝色色素的提取及其对纺织品染色的方法,属于纺织印染技术领域,本发明中所使用的可食用色素是从栀子果中提取的一种蓝色色素,所述方法包括如下步骤:栀子果中蓝色色素的提取、纺织品前处理、改性纺织品、染色、烘干定型。本发明采用可食用天然色素进行染色,可以保证纺织品在较长时间内不褪色,同时染色牢固度高,色彩鲜亮,对纺织品品质无影响,具有环保、健康等优点。
Description
技术领域
本发明属于纺织印染领域,具体涉及一种栀子果中蓝色色素的提取及其对纺织品染色的方法。
背景技术
目前纺织印染行业上所应用的染料主要以化工染料为主,主要有酸性染料、活性染料、分散染料、阳离子染料等。酸性染料主要用来染羊毛、丝绸,活性染料主要用来染棉麻制品、竹炭、莫代尔等,分散染料主要用来染涤纶产品,阳离子染料主要用来染腈纶产品。目前还没有发现有一种化工染料能够同时对羊毛、丝绸、棉麻制品、竹炭以及莫代尔进行染色。
化工染料中有相当一部分本身或者是其生产原料或者在生产过程中产生的中间体属于难以降解,甚至是致癌物质,不仅对环境造成污染,甚至对生产工人和消费者也造成健康。
随着人们生活水平的提高,追求生活品味,回归自然的愿望越来越强烈,纺织品作为人们不可或缺的生活的必须品,其品质和色彩一直是广大消费者消费和关注的焦点,如何能够满足消费者既环保健康又不失高端大气的品质追求,一直是所有纺织品生产厂家努力实现的目标,特别是对纺织品工艺绿色环保的需求越来越强烈。但因各种原因,目前市场上出现的产品很少能够达到绝对回归自然的终级需求,终究不能满足主流消费者所追求高端、时尚、廉价的综合要求。
可食用天然色素无毒、对环境无害以及其特殊有的药用价值等众多优点使它成为近年来染料领域的新宠儿。随着生物技术的大力发展,充分利用可食用染料来开发一些高附加值、多功能的纺织品具有广阔的发展前景。
从栀子果中提取的蓝色素是由经食品酶处理过的从栀子的果实中提取出蓝色色素而制得,其在PH=3-10条件下稳定,色泽鲜艳,着色力强,抗光、耐热性好。
查阅文献资料,了解到从栀子果中获得的蓝色色素的化学性质比较稳定。经对现有的文献进行检索,发现采用该可食用天然色素对纺织品进行染色的研究少之又少。
发明内容
为了克服现有技术的不足,本发明提供了一种栀子果中蓝色色素的提取及其对纺织品染色的方法,该方法为减少化工染料的使用,开发新的天然染料提供技术依据。
本发明解决其技术问题所采用的技术方案是:
一种栀子果中蓝色色素的提取及其对纺织品染色的方法,所述的方法包括以下步骤:
1)栀子果中蓝色色素的提取:栀子苷的提取、栀子苷转化为栀子蓝粗品、栀子蓝粗品浓缩纯化,最后得到蓝色色素成品;
2)纺织品前处理:使用天然可降解非离子表面活性剂茶皂素分散液对纺织品进行去杂、脱浆处理,之后进行蒸煮,结束后水洗,再用醋酸洗;
3)改性纺织品:将步骤2)前处理后的纺织品采用稀土化合物进行改性处理;
4)染色:将步骤1)中提取的蓝色色素溶解于水中,对步骤3)中改性后的纺织品进行染色;
5)烘干定型:将步骤4)染色后得到纺织品进行烘干定型。
优选的,步骤1)中,所述的栀子苷的提取过程中,首先将鲜栀子果在45-60℃烘干至恒重,粉碎并过筛得到栀子果粉末;在栀子果粉末中加入体积分数为50-95%的乙醇溶液进行浸提,栀子果粉末与乙醇溶液的料液比为(1:6)-(1:12)g/mL;浸提后浓缩至近无醇;加水溶解后用等体积正丁醇萃取2次,浓缩回收正丁醇至干;含有栀子苷的组分浓缩后再用体积比为(1:2)-(1:4)的石油醚与乙酸乙酯混合溶剂重结晶,即可得到白色栀子苷晶体。
优选的,步骤1)中,所述的栀子苷转化为栀子蓝粗品过程中,将栀子苷溶解于水中,栀子苷与水的质量比为(1:10)-(1:15),再添加米曲霉发酵液,米曲霉发酵液与栀子苷的质量比为(1:1)-(1:1.8),在温度为45-85℃下搅拌8-16h,搅拌速率为140-220r/min;搅拌结束后在溶液中添加谷氨酸钠反应36-48h,谷氨酸钠的添加量为溶液质量的2-6%,谷氨酸钠为发酵液的氮源;搅拌结束后,在40-60℃保温1-4h,得栀子蓝粗品。
优选的,步骤1)中,所述的浓缩纯化过程中,采用70%的乙醇浸泡溶胀的大孔树脂,蒸馏水洗至无醇味,采用静态吸附,流速为60-100滴/min,收集洗脱液,旋蒸干燥,干燥温度为40-60℃,得到蓝色色素成品。
优选的,步骤2)中,所述的纺织品包括羊毛、丝绸、棉麻制品、竹炭或莫代尔中的一种,该染料可以同时对这些布料进行染色。
优选的,步骤2)中,所述的天然可降解非离子表面活性剂茶皂素的浓度为0.1-0.3g/L,茶皂素可以去除纺织品纤维素在织造过程中添加的浆料,去除纤维本身生长采摘过程中未去除的杂质等;蒸煮时间在30-60min之间,蒸煮的温度在70-98℃之间,蒸煮可以很好的去除影响织物上色的浆料、杂质等物质;采用醋酸洗后直至纺织品表面的pH为6-8,调节pH值使得织物处于中性状态,为织物上色提供条件。
优选的,步骤3)中,所述的稀土化合物包括氧化镧、氧化铈或氧化镨中的一种,稀土化合物分散液的浓度为0.1-2g/L,控制纺织品和稀土化合物分散液的重量比,即控制其浴比为(1:6)-(1:30),采用稀土化合物对前处理好的纤维进行改性处理,使其纤维结构发生改变,不仅可以增加染料对纺织品的上染率,还可以增加颜色的鲜艳度,提高日晒及耐洗色牢度;如果不对纤维进行改性,纤维中有大量的羟基,氨基酸等,对色素虽然有较好的直接性,但是很少有对纤维共价键,离子键,或者范德华力等的结合,色素和纤维之间如果没有很好的结合,上染的牢度会很差,各项指标不符合纺织品基本指标的要求,因此,改性也是必须要进行的步骤。
优选的,步骤3)中,改性起始温度为常温,之后开始升温,升温速度为1-5℃/min,升温至70-95℃,保温20-60min,降温至50-60℃,开始水洗,先用冷水洗一道,再用热水洗一道,最后再用冷水洗至布面干净为止,降至室温,待染色。
优选的,步骤4)中,将步骤1)得到的蓝色色素溶解于水中得到浓度为0.1-10g/L的染料,之后加醋酸将染料的pH调至6-8,室温条件下依次加入染料助剂,开始染色,染色过程中纺织品和染液的重量比即浴比为(1:6)-(1:30),然后开始升温,升温速率1-5℃/min,温度升至70-95℃,保温30-60min,开始降温至60-70℃,降温速率为1-3℃/min,开始水洗,先冷水洗一次,再用90℃热水和皂洗剂进行皂洗10-30min,采用浓度为1-2g/L的皂洗剂,洗至干净,整个染色流程结束。
优选的,步骤5)中,烘干的温度为110-150℃。
本发明的优点是:
(1)本发明所使用的染料是从栀子果中提取的一种蓝色色素,具有可食用的特点,对人体和环境无毒、无害。经该工艺染色后的产品具有染色均一性好,日晒牢度高,可用于纺织行业清洁生产;
(2)本发明所使用的从栀子果中提取的蓝色色素能够同时对羊毛、丝绸、棉麻制品、竹炭、以及莫代尔等进行染色,具有应用领域广泛,操作简单的优点。
具体实施方式
下面对本发明作进一步的说明:
实施例1
鲜栀子果50℃烘干至恒重,粉碎并过筛;准确称量粉碎处理过的栀子果,按照料液比1:10g/mL加入体积分数为70%乙醇溶液浸提后,浓缩至近无醇,加水溶解后用等体积正丁醇萃取2次,浓缩回收正丁醇至干。含有栀子苷的组分浓缩后再用体积比为1:2的石油醚与乙酸乙酯混合溶剂重结晶,得到白色晶体栀子苷。
栀子苷与水按质量比1:12混合溶解后,按照米曲霉发酵液与栀子苷的质量比为1:1的量加入米曲霉发酵液,温度为60℃,搅拌速率为200r/min反应10h后,在溶液中添加溶液质量2%的谷氨酸钠反应48h,85℃保温1.5h,得栀子蓝粗品。
采用70%的乙醇浸泡溶胀的AB-8大孔树脂,蒸馏水洗至无醇味,采用静态吸附,流速控制在90滴/min,收集洗脱液,旋蒸干燥,干燥温度为45℃,得色素成品。
首先对棉纤维32S精梳针织单面布进行前处理,加入浓度为0.3g/L茶皂素分散液,温度升至95℃,保温40min,然后进行冷水洗,热水醋酸酸洗,至布面为中性。
对前处理好的布料进行改性处理,加入浓度为0.1g/L氧化镧分散液,控制布料与氧化镧分散液的重量比即浴比1:10,常温升温,升温速率为3℃/min,升至90℃,保温50min,降温至60℃,开始水洗,先用冷水洗一道,再热水洗一道,最后再用冷水洗至布面干净为止,降至室温,待染色。
进行染色,将提取的色素粉末制备得到浓度为2g/L的染液,之后加醋酸将染料的pH调至7,室温条件下依次加入染料助剂,控制布料和染液的重量比即浴比为1:10,常温升温,升温速度为2℃/min,升温至95℃,保温40min,降温至50℃,降温速率为1℃/min,开始水洗,先冷水洗,接着用弱酸性皂洗剂(BM-2)水洗,冷水洗一道,加固色剂(CF-3),最后水洗。
在140℃条件下烘干,定型、打包。
实施例2
鲜栀子果45℃烘干至恒重,粉碎并过筛;准确称量粉碎处理过的栀子果,按照料液比1:8g/mL加入体积分数为60%乙醇溶液浸提后,浓缩至近无醇,加水溶解后用等体积正丁醇萃取2次,浓缩回收正丁醇至干。含有栀子苷的组分浓缩后再用体积比为1:3的石油醚与乙酸乙酯混合溶剂重结晶,得到白色晶体栀子苷;
栀子苷与水按质量比1:10混合溶解后,按照米曲霉发酵液与栀子苷的质量比为1:1.5的量加入米曲霉发酵液,温度为50℃,搅拌速率为150r/min反应8h后,在溶液中添加溶液质量4%的谷氨酸钠反应55h,85℃保温2.5h,得栀子蓝粗品。
采用70%的乙醇浸泡溶胀的AB-8大孔树脂,蒸馏水洗至无醇味,采用静态吸附,流速控制在80滴/min,收集洗脱液,旋蒸干燥,干燥温度为40℃,得色素成品。
首先对丝绸36S平纹布进行前处理,加入浓度为3g/L茶皂素分散液,温度升至90℃,保温30min,然后进行冷水洗,热水醋酸酸洗,至布面的pH为6。
对前处理好的面料进行改性处理,加入浓度为0.5g/L氧化铈分散液,控制布料与氧化铈分散液的重量比即浴比1:6,常温升温,升温速率为3℃/min,升至80℃,保温30min,降温至50℃,开始水洗,先用冷水洗一道,再热水洗一道,最后再用冷水洗至布面干净为止,降至室温,待染色。
进行染色,将提取的色素粉末制备得到浓度为1g/L的染液,之后加醋酸将染料的pH调至6,室温条件下依次加入染料助剂,控制布料和染液的重量比即浴比为1:8,常温升温,升温速度为1℃/min,升温至90℃,保温30min,降温至50℃,降温速率为2℃/min开始水洗,先冷水洗,接着用弱酸性皂洗剂(BM-2)水洗,冷水洗一道,加固色剂(CF-3),最后水洗。
在120℃条件下烘干,定型、打包。
实施例3
鲜栀子果60℃烘干至恒重,粉碎并过筛;准确称量粉碎处理过的栀子果,按照料液比1:12g/mL加入体积分数为90%乙醇溶液浸提后,浓缩至近无醇,加水溶解后用等体积正丁醇萃取2次,浓缩回收正丁醇至干。含有栀子苷的组分浓缩后再用体积比为1:4的石油醚与乙酸乙酯混合溶剂重结晶,得到白色晶体栀子苷;
栀子苷与水按质量比1:15混合溶解后,按照米曲霉发酵液与栀子苷的质量比为1:1.8的量加入米曲霉发酵液,温度为70℃,搅拌速率为220r/min反应13h后,在溶液中添加3%的谷氨酸钠反应60h,85℃保温4h,得栀子蓝粗品。
采用70%的乙醇浸泡溶胀的AB-8大孔树脂,蒸馏水洗至无醇味,采用静态吸附,流速控制100滴/min,收集洗脱液,旋蒸干燥,干燥温度为60℃,得色素成品。
对莫代尔40S单面布进行前处理,加入浓度为4g/L的茶皂素分散液,温度升至90℃,保温60min,然后进行冷水洗,热水醋酸酸洗,至布面的pH为8。
对前处理好的面料进行改性处理,加入浓度为0.8g/L氧化镨分散液,控制布料与氧化镨分散液的重量比即浴比1:15,常温升温,升温速率为5℃/min,升至95℃,保温60min,降温至60℃,开始水洗,先用冷水洗一道,再热水洗一道,最后再用冷水洗至布面干净为止,降至室温,待染色。
进行染色,将提取的色素粉末制备得到浓度为5g/L的染液,之后加醋酸将染料的pH调至8,室温条件下依次加入染料助剂,控制布料和染液的重量比即浴比为1:15,常温升温,升温速度为5℃/min,升温至70℃,保温60min,降温至50℃,降温速率为3℃/min,开始水洗,先冷水洗,接着用弱酸性皂洗剂(BM-2)水洗,冷水洗一道,加固色剂(CF-3),最后水洗。
在130℃条件下烘干,定型、打包。
产品检测:
对实施例1、2和3得到的样品分别进行检测,检测的结果取平均值,结果如下所示,通过以下的结果说明,本发明生产出的产品符合预期标准。
1、耐洗色牢度
2、耐汗渍色牢度
3、耐摩擦色牢度
4、pH值
5、甲醛含量
6、偶氮染料
7、纺织品抗菌性能的评价
最后应说明的是:显然,上述实施例仅仅是为清楚地说明本发明所作的举例,而并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明的保护范围之中。
Claims (10)
1.一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,所述的方法包括以下步骤:
1)栀子果中蓝色色素的提取:栀子苷的提取、栀子苷转化为栀子蓝粗品、栀子蓝粗品浓缩纯化,最后得到蓝色色素成品;
2)纺织品前处理:使用天然可降解非离子表面活性剂茶皂素分散液对纺织品进行去杂、脱浆处理,之后进行蒸煮,结束后水洗,再用醋酸洗;
3)改性纺织品:将步骤2)前处理后的纺织品采用稀土化合物进行改性处理;
4)染色:将步骤1)中提取的蓝色色素成品溶解于水中,对步骤3)中改性后的纺织品进行染色;
5)烘干定型:将步骤4)染色后得到纺织品进行烘干定型。
2.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤1)中,所述的栀子苷的提取过程中,首先将鲜栀子果在45-60℃烘干至恒重,粉碎并过筛得到栀子果粉末;在栀子果粉末中加入体积分数为50-95%的乙醇溶液进行浸提,栀子果粉末与乙醇溶液的料液比为(1:6)-(1:12)g/mL;浸提后浓缩至近无醇;加水溶解后用等体积正丁醇萃取2次,浓缩回收正丁醇至干;含有栀子苷的组分浓缩后再用体积比为(1:2)-(1:4)的石油醚与乙酸乙酯混合溶剂重结晶,即可得到白色栀子苷晶体。
3.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤1)中,所述的栀子苷转化为栀子蓝粗品过程中,将栀子苷溶解于水中,栀子苷与水的质量比为(1:10)-(1:15),再添加米曲霉发酵液,米曲霉发酵液与栀子苷的质量比为(1:1)-(1:1.8),在温度为45-85℃下搅拌8-16h,搅拌速率为140-220r/min;搅拌结束后再在溶液中添加谷氨酸钠反应36-48h,谷氨酸钠的添加量为溶液质量的2-6%;搅拌结束后,在40-60℃保温1-4h,得栀子蓝粗品。
4.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤1)中,所述的浓缩纯化过程中,采用70%的乙醇浸泡溶胀的大孔树脂,蒸馏水洗至无醇味,采用静态吸附,流速为60-100滴/min,收集洗脱液,旋蒸干燥,干燥温度为40-60℃,得到蓝色色素成品。
5.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤2)中,所述的纺织品包括羊毛、丝绸、棉麻制品、竹炭或莫代尔中的一种。
6.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤2)中,所述的天然可降解非离子表面活性剂茶皂素分散液的浓度为0.1-0.3g/L;蒸煮时间为30-60min,蒸煮的温度为70-98℃;采用醋酸洗后直至纺织品表面的pH为6-8。
7.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤3)中,所述的稀土化合物包括氧化镧、氧化铈或氧化镨中的一种,稀土化合物分散液的浓度为0.1-2g/L,浴比为(1:6)-(1:30)。
8.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤3)中,改性起始温度为常温,之后开始升温,升温速度为1-5℃/min,升温至70-95℃,保温20-60min,降温至50-60℃,开始水洗,先用冷水洗一道,再热水洗一道,最后再用冷水洗至布面干净为止,降至室温,待染色。
9.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤4)中,将步骤1)得到的色素成品溶解于水中得到浓度为0.1-10g/L的染料,之后加醋酸将染料的pH调至6-8,室温条件下依次加入染料助剂,开始对纺织品进行染色,浴比为(1:6)-(1:30),然后开始升温,升温速率1-5℃/min,温度升至70-95℃,保温30-60min,开始降温至60-70℃,降温速率为1-3℃/min,开始水洗,先冷水洗一次,再用90℃热水和皂洗剂进行皂洗10-30min,采用浓度为1-2g/L的皂洗剂,洗至干净,整个染色流程结束。
10.如权利要求1所述的一种栀子果中蓝色色素的提取及其对纺织品染色的方法,其特征在于,步骤5)中,烘干的温度为110-150℃。
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