WO2020087499A1 - 一种阻燃蚕丝及其制备方法和应用 - Google Patents

一种阻燃蚕丝及其制备方法和应用 Download PDF

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WO2020087499A1
WO2020087499A1 PCT/CN2018/113686 CN2018113686W WO2020087499A1 WO 2020087499 A1 WO2020087499 A1 WO 2020087499A1 CN 2018113686 W CN2018113686 W CN 2018113686W WO 2020087499 A1 WO2020087499 A1 WO 2020087499A1
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silk
flame
flame retardant
retardant
tannic acid
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French (fr)
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唐人成
杨童童
关晋平
陈国强
杨旭红
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Suzhou University
Nantong Textile and Silk Industrial Technology Research Institute
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Suzhou University
Nantong Textile and Silk Industrial Technology Research Institute
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/10—Animal fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30—Flame or heat resistance, fire retardancy properties

Definitions

  • the invention relates to the technical field of textile finishing, in particular to a method for preparing flame-retardant silk and flame-retardant silk prepared by the method.
  • Silk is one of the most common natural protein fibers. Because of its soft and natural luster, unique silk sensation, good health and comfort, it is deeply loved by consumers. Silk textiles are often used to make high-end clothing and ornaments. Silk ornaments and some daily-use garments have high requirements for flame retardancy.
  • Good flame-retardant finishing in addition to providing flame-retardant function, must also be non-toxic, less smoke, can withstand a certain degree of washing and dry cleaning, and does not hinder the original quality of silk.
  • the flame retardant finishing of silk was treated with stannic acid or boric acid-borax dipping method in the early stage. Although the flame retardant effect is good and good, it is not resistant to washing.
  • Halogen flame retardants have been used in the flame retardant finishing of silk, but were later banned due to toxicity issues.
  • Phosphorus and nitrogen flame retardants for cotton have also been used in the flame retardant finishing of silk, and can give silks better flame retardant performance and washing resistance, but its disadvantages are high processing costs, more complicated processes, and the resulting silk feel Hardening and yellowing, and the problem of free formaldehyde release.
  • the "Zirpro" process which is widely used in the flame retardant finishing of wool, also has certain applications in silk.
  • This process uses flame retardant finishing of silk with metal complexes such as titanium and zirconium to effectively improve the flame retardant performance of silk
  • metal complexes such as titanium and zirconium
  • the price is relatively expensive, and the washing resistance of the flame retardant function is also poor.
  • phosphorus will cause eutrophication in water, halogen flame retardants will release toxic gases during use, thus harming the environment and human body. Therefore, paying attention to environmental issues and developing green, friendly, economical, and easy-to-use flame retardant technologies are urgent problems in this field.
  • the technical problem to be solved by the present invention is to provide a method for preparing flame retardant silk with simple preparation method and good flame retardant effect.
  • the solution provided by the present invention is: a method for preparing flame-retardant silk, including the following steps:
  • step S2 Immerse the silk processed in step S1 in a metal salt solution of 2-6g / L, and heat up to 50-70 ° C for treatment to obtain a flame-retardant silk.
  • Tannic acid is derived from plant tissues and contains carboxyl groups, which can be adsorbed on silk under weak acid conditions and ionic bond with silk. After tannic acid is adsorbed on silk, it is then treated with metal salt, metal ion energy Complexes with tannic acid adsorbed on silk and silk fiber, which changes the thermal degradation process of silk burning and plays a flame retardant role.
  • the silk treated with tannic acid and metal salt has good flame retardancy and excellent wash resistance.
  • the heat preservation treatment time in the step S1 is 45-75min.
  • the processing time at 50-70 ° C in the step S2 is 20-40min.
  • step S1 the amount of tannic acid is 10-30% of the relative weight of silk.
  • the metal salt is one or more of ferrous sulfate, ferric sulfate, titanium sulfate or calcium sulfate.
  • the present invention further provides a flame-retardant silk prepared according to the above method.
  • the present invention further provides an application of the flame-retardant silk prepared according to the above method in textiles.
  • the tannic acid used in the present invention is derived from plant tissues and is an environmentally friendly natural compound.
  • the flame-retardant finishing method used in the present invention is a brand-new flame-retardant method and technology.
  • the flame-retardant finishing process is simple to operate and has obvious effects, and the metal ions used are easily available and inexpensive.
  • the flame retardant performance of silk fabrics is in accordance with GB / T 5454-1997 "Textile Combustion Performance Test Oxygen Index Method” and GB / T 5455-2014 "Textile Combustion Performance Vertical Damage Length Smoldering and Afterburning Time “Measurement” to determine.
  • the washing method of the flame-retardant silk fabric is carried out according to the standard of GB / T 3921-2008 "Textile color fastness test soap color fastness", using a special detergent for silk fabric 2g / L, bath ratio 1:50, at 40 °C Wash once every 30 minutes. Repeat washing to the required number of times.
  • the silk treated with tannic acid and ferrous sulfate has a limiting oxygen index of 27.5%, and the damaged length is only 11.0cm; the silk treated with tannic acid and ferric sulfate has a limiting oxygen index of 27.6%, and the damaged length is only 11.1cm.
  • the silk treated with tannic acid and ferrous sulfate or ferric sulfate meets the B1 flame retardant performance requirements of China's GB / T 17591-2006 "Flame Retardant Fabric" (the damage length is less than 15cm).
  • the silk treated with tannic acid and calcium sulfate has a limiting oxygen index of 27.5% and the damaged length is only 12.3cm; the silk treated with tannic acid and titanium sulfate has a limiting oxygen index of 28.5% and the damaged length is only 10.0 cm.
  • the silk treated with tannic acid and calcium sulfate or titanium sulfate meets the B1 flame retardant performance requirements in China's GB / T 17591-2006 "Flame Retardant Fabric".
  • Table 1 shows that: the silk treated with ferrous sulfate alone has a limiting oxygen index of 25.1%, completely burned during the vertical combustion test, and the damaged length is 30.0 cm; the silk treated with tannic acid alone has a limiting oxygen index of 26.1%.
  • the length of the damage during vertical burning is 19.5cm; silk treated with ferrous sulfate or tannic acid alone cannot meet the B1 flame retardant performance requirements in China's GB / T 17591-2006 "Flame Retardant Fabric".
  • the limit oxygen index of silk treated with 10%, 20% and 30% tannic acid solution and 2g / L ferrous sulfate is 26.9% to 27.9%, and the length of damage during vertical burning is about 11cm, which meets China ’s GB / L T17591-2006 "flame retardant fabric" B1 level flame retardant performance requirements.
  • Example 2 According to the method described in Example 1, the silk fabric is subjected to flame retardant treatment, and the obtained flame retardant silk is subjected to a wash resistance test. The results are shown in Table 2.
  • Table 2 shows that after repeated washing for many times, the limit oxygen index of the flame-retardant silk changes very little, and the damage length during vertical burning is still less than 15cm, indicating that the flame-retardant effect of the silk prepared by the method of the present invention has excellent wash resistance Sex or washing durability.
  • the above examples show that the method for preparing flame-retardant silk in the present invention can provide silk with good flame-retardant performance, and the flame-retardant function has excellent washing durability.
  • This method has the advantages of environmental protection, high efficiency, and simplicity.
  • the method of the present invention imparts good flame retardant performance to silk without adding flame retardants containing traditional nitrogen, phosphorus and halogen elements, and can avoid the production and use of flame retardant silk due to the use of traditional flame retardants Environmental pollution problems caused by nitrogen, phosphorus and halogen elements in the process and after the flame-retardant silk is discarded. This method has the advantages of environmental protection, high efficiency, and simplicity.
  • Tannic acid is derived from plant tissues and contains carboxyl groups, which can be adsorbed on silk under weak acid conditions and ionic bond with silk. After tannic acid is adsorbed on silk, it is then treated with metal salt, metal ion energy Complexes with tannic acid adsorbed on silk and silk fiber, which changes the thermal degradation process of silk burning and plays a flame retardant role.
  • the silk treated with tannic acid and metal salt has good flame retardancy and excellent wash resistance.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

本发明公开了一种制备阻燃蚕丝的方法，包括以下步骤：将蚕丝浸入pH值为3-4的单宁酸溶液中，升温至80-90℃进行保温处理；将经过处理后的蚕丝浸入至2-6g/L的金属盐溶液中，并升温至50-70℃进行处理，得到阻燃蚕丝。。本发明的方法在不添加含有传统氮、磷、卤族元素阻燃剂的情况下赋予蚕丝良好的阻燃性能，并且能够避免因使用传统阻燃剂而带来的在阻燃蚕丝生产和使用过程中以及及阻燃蚕丝被废弃后氮、磷、卤族元素带来的环境污染问题。该方法具有环保、高效、简单易行的优点。

Description

一种阻燃蚕丝及其制备方法和应用 技术领域
本发明涉及纺织品整理技术领域，具体涉及一种制备阻燃蚕丝的方法以及使用该方法制备的阻燃蚕丝。
背景技术
蚕丝是最常见的天然蛋白质纤维之一，因其柔和自然的光泽、独有的丝鸣感、良好的保健性及舒适性而深受消费者喜爱。蚕丝纺织品常用于制作高档的服装及装饰物，蚕丝装饰物和部分日用服装对阻燃性能有着较高的要求。蚕丝作为天然蛋白质纤维，不能通过与阻燃剂共混纺丝的方法对其进行阻燃改性，只能通过印染的后整理加工来达到阻燃的目的。良好的阻燃整理，除了能提供阻燃功能外，还必须无毒性、发烟少、可耐一定程度的水洗和干洗，且不妨碍蚕丝原有的优良品质。
蚕丝的阻燃整理，早期采用的是锡酸或者硼酸-硼砂浸渍法处理，虽然阻燃效果好较好，但不耐水洗。卤素阻燃剂曾被应用于蚕丝的阻燃整理，但后因毒性问题而被禁用。棉用磷氮类阻燃剂也曾被应用于蚕丝的阻燃整理，并能赋予蚕丝较好的阻燃性能和耐水洗性能，然而其缺点是加工费用高，工艺比较复杂，而且所得蚕丝手感发硬和泛黄，并存在游离甲醛释放问题。目前，广泛应用于羊毛阻燃整理的“Zirpro”工艺，在蚕丝上也有一定的应用，该工艺通过钛、锆等金属络合物对蚕丝进行阻燃整理，能有效地提升蚕丝的阻燃性能，但所适用的金属离子种类较少，且价格相对昂贵，阻燃功能的耐洗性也欠佳。由于磷元素在水体中会引起富营养化，卤族元素阻燃剂在使用过程中会释放有毒气体从而危害环境和人体。因此，重视环境问题，开发绿色友好、经济适用、应用 工艺简单的阻燃技术是本领域亟需解决的问题。
发明内容
本发明要解决的技术问题是提供一种制备方法简单，阻燃效果好的一种制备阻燃蚕丝的方法。
为了解决上述技术问题，本发明提供的方案是：一种制备阻燃蚕丝的方法，包括以下步骤：
S1、将蚕丝浸入pH值为3-4的单宁酸溶液中，升温至80-90℃进行保温处理；
S2、将经过步骤S1处理后的蚕丝浸入至2-6g/L的金属盐溶液中，并升温至50-70℃进行处理，得到阻燃蚕丝。
单宁酸来源于植物组织，含有羧基，能在弱酸性条件下在蚕丝上发生吸附，并与蚕丝发生离子键结合；单宁酸在蚕丝上发生吸附后，再经金属盐处理，金属离子能与蚕丝上吸附的单宁酸以及蚕丝纤维发生络合作用，进而改变了蚕丝燃烧时的热降解进程而起到阻燃作用。单宁酸和金属盐联合处理的蚕丝具有良好的阻燃性能以及极佳的耐洗性。
进一步的是：所述步骤S1中保温处理的时间为45-75min。
进一步的是：所述步骤S2中在50-70℃下的处理时间为20-40min。
进一步的是：所述步骤S1中，单宁酸的用量为对蚕丝的相对重量的10-30％。
进一步的是：所述的金属盐为硫酸亚铁、硫酸铁、硫酸钛或硫酸钙中的一种或多种。
本发明进一步的提供一种根据上述方法制备得到的阻燃蚕丝。
本发明进一步的提供一种根据上述方法制备得到的阻燃蚕丝在纺织方面的应用。
本发明的有益效果：
1、本发明使用的单宁酸来源于植物组织，是一种环境友好的天然化合物。
2、本发明使用的阻燃整理方法是一种全新的阻燃方法和技术，阻燃整理过程操作简单、效果明显，且所用金属离子易得、价格低廉。
3、在不添加传统氮、磷、卤族元素阻燃剂的情况下，能赋予蚕丝良好的阻燃性能，且阻燃功能的耐久性极佳，并且能够避免因使用传统阻燃剂而带来的在阻燃蚕丝生产和使用过程中以及及阻燃蚕丝被废弃后氮、磷、卤族元素带来的环境污染问题。该方法具有环保、高效、简单易行的优点。
具体实施方式
下面结合具体实施例对本发明作进一步说明，以使本领域的技术人员可以更好地理解本发明并能予以实施，但所举实施例不作为对本发明的限定。
本发明以下实施例中，蚕丝织物的阻燃性能按照GB/T 5454-1997《纺织品燃烧性能实验氧指数法》和GB/T 5455-2014《纺织品燃烧性能垂直方向损毁长度阴燃和续燃时间的测定》进行测定。阻燃蚕丝织物的水洗方法参照GB/T 3921-2008《纺织品色牢度试验耐皂洗色牢度》标准进行，使用丝毛织物专用洗涤剂2g/L，浴比1:50，40℃下洗涤30min为一次。重复水洗至所需水洗次数。
实施例1
S1、将20％(对蚕丝的相对重量)的单宁酸溶于水中，常温下搅拌10min，使用柠檬酸/磷酸氢二钠缓冲溶液将pH值调节至4；将蚕丝浸入上述单宁酸溶液中，升温至90℃，保温处理45min，取出蚕丝，洗净、烘干。
S2、将上述单宁酸处理后的蚕丝浸入2g/L的硫酸亚铁或硫酸铁溶液中，于70℃处理20min，洗净、烘干，得到耐久性的阻燃功能的蚕丝。
经单宁酸和硫酸亚铁联合处理的蚕丝的极限氧指数为27.5％，损毁长度仅为11.0cm；经单宁酸和硫酸铁联合处理的蚕丝的极限氧指数为27.6％，损毁长 度仅为11.1cm。经单宁酸和硫酸亚铁或硫酸铁联合处理的蚕丝均满足我国GB/T 17591-2006《阻燃织物》中B1级阻燃性能要求(损毁长度小于15cm)。
实施例2
S1、将20％(对蚕丝的相对重量)的单宁酸溶于水中，常温下搅拌10min，使用柠檬酸/磷酸氢二钠缓冲溶液将上述溶液的pH值调节至3；将蚕丝浸入上述单宁酸溶液中，升温至80℃，保温处理75min，取出蚕丝，洗净、烘干。
S2、将上述单宁酸处理后的蚕丝浸入6g/L的硫酸钙或硫酸钛溶液中，于50℃处理40min，洗净、烘干，得到耐久性的阻燃功能的蚕丝。
经单宁酸和硫酸钙联合处理的蚕丝的极限氧指数为27.5％，损毁长度仅为12.3cm；经单宁酸和硫酸钛联合处理的蚕丝的极限氧指数为28.5％，损毁长度仅为10.0cm。经单宁酸和硫酸钙或硫酸钛联合处理的蚕丝均满足我国GB/T 17591-2006《阻燃织物》中B1级阻燃性能要求。
实施例3
S1、分别将10％、20％和30％(对蚕丝的相对重量)单宁酸溶于水中，常温下搅拌10min，使用柠檬酸/磷酸氢二钠缓冲溶液将上述溶液的pH值调节至3；将蚕丝分别浸入上述单宁酸溶液中，升温至90℃，保温处理60min，取出蚕丝，洗净、烘干。
S2、将上述单宁酸处理后的蚕丝浸入2g/L的硫酸亚铁溶液中，于60℃处理30min，洗净、烘干，得到耐久性的阻燃功能的蚕丝。
作为比较例，单独使用硫酸亚铁处理蚕丝：将蚕丝织物浸于2g/L的硫酸亚铁溶液中于70℃处理30min；单独使用单宁酸处理蚕丝：将蚕丝织物浸于20％(对蚕丝的相对重量)单宁酸溶液中于90℃处理60min。
对未处理和处理的蚕丝织物进行阻燃性能测试，结果见表1。
表1 蚕丝织物的阻燃性能
Figure PCTCN2018113686-appb-000001
Figure PCTCN2018113686-appb-000002
表1表明：单独用硫酸亚铁处理的蚕丝的极限氧指数为25.1％，在垂直燃烧测试时完全燃烧，损毁长度为30.0cm；单独用单宁酸处理的蚕丝的极限氧指数为26.1％，在垂直燃烧时损毁长度为19.5cm；单独用硫酸亚铁或单宁酸处理的蚕丝均不能满足我国GB/T 17591-2006《阻燃织物》中B1级阻燃性能要求。经10％、20％和30％单宁酸溶液和2g/L硫酸亚铁联合处理的蚕丝的极限氧指数在26.9％至27.9％，在垂直燃烧时损毁长度在11cm左右，均满足我国GB/T 17591-2006《阻燃织物》中B1级阻燃性能要求。
实施例4
按照实施例1所述方法对蚕丝织物进行阻燃处理，对所得阻燃功能的蚕丝进行耐洗性试验，结果见表2。
表2 蚕丝织物阻燃性能的耐洗性
Figure PCTCN2018113686-appb-000003
表2表明，经多次重复洗涤后，阻燃蚕丝的极限氧指数变化极小，在垂直燃烧时损毁长度仍然小于15cm，说明用本发明方法制备的蚕丝的阻燃效果具 有极佳的耐洗性或水洗耐久性。
以上实施例说明，采用本发明中制备阻燃蚕丝的方法，能赋予蚕丝良好的阻燃性能，而且阻燃功能的水洗耐久性极佳。该方法具有环保、高效、简单易行的优点。
本发明的方法在不添加含有传统氮、磷、卤族元素阻燃剂的情况下赋予蚕丝良好的阻燃性能，并且能够避免因使用传统阻燃剂而带来的在阻燃蚕丝生产和使用过程中以及及阻燃蚕丝被废弃后氮、磷、卤族元素带来的环境污染问题。该方法具有环保、高效、简单易行的优点。
单宁酸来源于植物组织，含有羧基，能在弱酸性条件下在蚕丝上发生吸附，并与蚕丝发生离子键结合；单宁酸在蚕丝上发生吸附后，再经金属盐处理，金属离子能与蚕丝上吸附的单宁酸以及蚕丝纤维发生络合作用，进而改变了蚕丝燃烧时的热降解进程而起到阻燃作用。单宁酸和金属盐联合处理的蚕丝具有良好的阻燃性能以及极佳的耐洗性。
以上所述实施例仅是为充分说明本发明而所举的较佳的实施例，本发明的保护范围不限于此。本技术领域的技术人员在本发明基础上所作的等同替代或变换，均在本发明的保护范围之内。本发明的保护范围以权利要求书为准。

Claims (7)

  1. 一种制备阻燃蚕丝的方法，其特征在于，包括以下步骤：
    S1、将蚕丝浸入pH值为3-4的单宁酸溶液中，升温至80-90℃进行保温处理；
    S2、将经过步骤S1处理后的蚕丝浸入至2-6g/L的金属盐溶液中，并升温至50-70℃进行处理，得到阻燃蚕丝。
  2. 如权利要求1所述的制备阻燃蚕丝的方法，其特征在于，所述步骤S1中保温处理的时间为45-75min。
  3. 如权利要求1所述的制备阻燃蚕丝的方法，其特征在于，所述步骤S2中在50-70℃下的处理时间为20-40min。
  4. 如权利要求1所述的制备阻燃蚕丝的方法，其特征在于，所述步骤S1中，单宁酸的用量为对蚕丝的相对重量的10-30％。
  5. 如权利要求1所述的制备阻燃蚕丝的方法，其特征在于，所述的金属盐为硫酸亚铁、硫酸铁、硫酸钛或硫酸钙中的一种或多种。
  6. 一种根据权利要求1至5中任一方法制备得到的阻燃蚕丝。
  7. 一种根据权利要求1至5中任一方法制备得到的阻燃蚕丝在纺织中的应用。
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