WO2021109865A1 - 一种黑色无机纤维及其等离子体制备方法 - Google Patents

一种黑色无机纤维及其等离子体制备方法 Download PDF

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WO2021109865A1
WO2021109865A1 PCT/CN2020/129207 CN2020129207W WO2021109865A1 WO 2021109865 A1 WO2021109865 A1 WO 2021109865A1 CN 2020129207 W CN2020129207 W CN 2020129207W WO 2021109865 A1 WO2021109865 A1 WO 2021109865A1
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fiber
plasma
black inorganic
sugar
carbonized
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French (fr)
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黄逸凡
高明
梅婷婷
王裕
顾晓滨
喻学锋
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中国科学院深圳先进技术研究院
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/673—Inorganic compounds
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/80—Inorganic fibres
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/20—Physical treatments affecting dyeing, e.g. ultrasonic or electric
    • D06P5/2011—Application of vibrations, pulses or waves for non-thermic purposes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/20—Physical treatments affecting dyeing, e.g. ultrasonic or electric
    • D06P5/2016—Application of electric energy

Definitions

  • the invention belongs to the field of fiber materials, and specifically relates to a black inorganic fiber and a plasma preparation method thereof.
  • fiber post-treatment dyeing is a common dyeing method.
  • plasma technology is used to treat the fiber to increase the surface roughness and chemically active groups of the fiber, so that the dye can be more easily adsorbed to the fiber surface.
  • Chinese patent documents 200810059897.X and 201811577679.5 both disclose related methods for dyeing aramid fibers using inert gas plasma, and have achieved good results.
  • inorganic fibers have a denser structure and stronger surface inertness.
  • the existing technologies often fail to achieve excellent results, and there are fewer reports on the dyeing methods of such inorganic fibers.
  • inorganic fibers represented by basalt fibers have developed rapidly. If basalt fibers of different colors can be provided, it will be of practical significance to promote their downstream applications.
  • other inorganic fibers such as ceramic fibers and sepiolite fibers face the same technical problems.
  • the disadvantage of the prior art is that plasma technology cannot be used to achieve the preparation of black inorganic fibers.
  • the purpose of the present invention is to use wet plasma for fiber pretreatment, use sugar aqueous solution as a dye source, and achieve fiber discoloration by high-temperature carbonization, thereby obtaining black inorganic fibers.
  • One aspect of the present invention provides a black inorganic fiber, comprising a fiber matrix and a carbonized sugar attached to the fiber matrix.
  • the fiber matrix is an inorganic fiber that can withstand 500°C or more, preferably selected from basalt fiber, ceramic Fiber, quartz fiber, sepiolite fiber.
  • the carbonized sugar attached to the fiber matrix is obtained by the following method:
  • Pretreatment Use wet plasma to modify the surface of the fiber matrix to obtain activated fibers, and soak the activated fibers in a sugar solution under tension;
  • step 2) Carbonized dyeing: The soaked fiber obtained in step 1) is carbonized at a high temperature to obtain a fiber matrix with carbonized sugar attached to form a dyed inorganic fiber.
  • the wet plasma is formed by high-voltage discharge using a mixed gas of water vapor and an inert gas.
  • Another aspect of the present invention provides a plasma preparation method of black inorganic fibers, including the following steps:
  • Pretreatment Use wet plasma to modify the surface of the fiber matrix to obtain activated fibers, and soak the activated fibers in a sugar solution under tension;
  • step 2) Carbonized dyeing: the soaked fiber obtained in step 1) is carbonized at high temperature to obtain black inorganic fiber;
  • the wet plasma is formed by high-voltage discharge using a mixed gas of water vapor and an inert gas.
  • the fiber matrix in step 1) is selected from basalt fiber, ceramic fiber, quartz fiber, sepiolite fiber.
  • the inert gas mentioned in step 1) is selected from one or a combination of argon, nitrogen, and helium.
  • the volume ratio of water vapor to inert gas in step 1) is 1:5-1:20, preferably 1:8-1:12, more preferably 1:10.
  • the plasma modification time described in step 1) is 2-10 min.
  • step 1) tension is applied to the fiber during the plasma treatment.
  • the tension is 1N or more, more preferably 1-3N.
  • a tension of 1N or more is applied to the activated fiber, preferably 3-5N.
  • the sugar water in step 1) is an aqueous solution of sugars, and the sugars are selected from monomers, dimers, oligomers, and polyhydroxy aldehydes or ketones.
  • the carbonization in step 2) is carried out under a protective atmosphere of an inert gas, and the inert gas is selected from argon or nitrogen.
  • the carbonization temperature in step 3) is 500°C or higher, preferably 500-700°C.
  • the carbonization time in step 3) is 30-300 min.
  • the concentration of the aqueous sugar solution in step 2) is more than 30%, preferably 40-60%.
  • Another aspect of the present invention provides black inorganic fibers prepared by the method of the present invention.
  • the invention discloses a black inorganic fiber and a plasma preparation method thereof.
  • the black inorganic fiber comprises a fiber matrix and a carbon film attached to the surface.
  • the specific preparation method of the present invention is: using wet plasma to activate the surface of the inorganic fiber under a certain tension, so that the surface has a large number of oxygen-containing active groups, and enhances its surface wettability and adsorption. Subsequently, under a certain tension, the fiber is soaked in the sugar solution, so that the sugar solution is immersed in the fiber gap. Finally, the high-temperature carbonization process is used to carbonize the sugar into black, thereby obtaining black inorganic fibers.
  • the method of the invention is novel and unique, simple and efficient, breaks through the limitation that the prior art cannot prepare black inorganic fibers, and the prepared black inorganic fibers have excellent performance, good color fastness, and excellent practical application prospects.
  • the purpose of the present invention is to propose a method for preparing black inorganic fibers by using plasma technology and the obtained fibers, which have the advantages of simplicity, high efficiency and the like.
  • the present invention can realize the dyeing of inorganic fibers without changing the fiber composition and fiber-forming process.
  • sugar water is used as the dye source, combined with the carbonization process, the use of chemical dyes can be avoided, and the dyeing wastewater is not generated.
  • Figure 1 is a photo of a fabric woven from basalt fibers. The picture shows that the basalt fibers are yellow-brown.
  • Figure 2 is a photograph of a black basalt fiber product dyed by the method of the present invention. The picture shows that the dyed product is black.
  • the fabric woven from basalt fibers (as shown in Figure 1, the yellow-brown fabric) is placed in a plasma atmosphere, and the volume ratio of water vapor and argon are mixed to discharge the basalt fiber under a tension of 2N.
  • the fiber undergoes surface activation for 5 minutes.
  • the activated fabric was immersed in a 50% sugar aqueous solution for 10 minutes at a bath ratio of 1:30.
  • the fabric was taken out, it was placed in a tube furnace under a nitrogen atmosphere at a temperature of 500 degrees to protect and carbonize for 60 minutes, and then rinsed with clean water at room temperature to obtain a black basalt fiber product (as shown in Figure 2, the black fabric).
  • the color fastness to washing and the color fastness to rubbing of the black basalt fiber are all above level 3, which has a good dyeing effect.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Coloring (AREA)

Abstract

本发明涉及一种黑色无机纤维及其等离子体制备方法，具体公开了一种黑色无机纤维，包括纤维基体及附在纤维基体上的碳化糖组成，所述的纤维基体为耐受500℃以上的无机纤维，例如玄武岩纤维、陶瓷纤维、石英纤维、海泡石纤维。所述附在纤维基体上的碳化糖通过以下方法获得：1）预处理：利用湿润等离子体对纤维基体进行表面改性获得活化后的纤维，在张力作用下将活化后的纤维在糖水溶液中浸泡；2）碳化染色：将步骤1）所得经浸泡的纤维通过高温碳化，得到纤维基体上附有碳化糖，即形成染色后的无机纤维。本发明新颖独特，制备方法简单，环保无污染。

Description

一种黑色无机纤维及其等离子体制备方法 技术领域
本发明属于纤维材料领域，具体涉及一种黑色无机纤维及其等离子体制备方法。
 背景技术
众所周知，纤维后处理染色是一种常见的染色方法。特别是利用等离子体技术对纤维进行处理，以增加纤维表面粗糙度和化学活性基团，从而使染料更容易吸附到纤维表面。中国专利文献200810059897.X和 201811577679.5都公开了利用惰性气体等离子体来进行芳纶纤维染色的相关方法，并取得良好效果。
但是，不同于芳纶等有机纤维，无机纤维其结构更为致密且表面惰性更强，采用现有技术往往无法达到优异的效果，且对这类无机纤维染色方法的报道较少。近年来，以玄武岩纤维为代表的无机纤维发展迅速，若能提供不同颜色的玄武岩纤维，则对推广其下游应用具有实际意义。同样的，作为其他无机纤维如陶瓷纤维、海泡石纤维等面临相同的技术问题。
 技术问题
现有技术的缺点在于无法利用等离子体技术来实现黑色无机纤维的制备。针对这些缺点，本发明的目的在于利用湿润等离子体进行纤维前处理，以糖水溶液作为染料源，通过高温碳化的方式来实现纤维变色，从而得到黑色无机纤维。
 技术解决方案
本发明一个方面提供了一种黑色无机纤维，包括纤维基体及附在纤维基体上的碳化糖组成，所述的纤维基体为耐受500℃以上的无机纤维，优选地，选自玄武岩纤维、陶瓷纤维、石英纤维、海泡石纤维。
在本发明的技术方案中，所述附在纤维基体上的碳化糖通过以下方法获得：
1）预处理：利用湿润等离子体对纤维基体进行表面改性获得活化后的纤维，在张力作用下将活化后的纤维在糖水溶液中浸泡；
2）碳化染色：将步骤1）所得经浸泡的纤维通过高温碳化，得到纤维基体上附有碳化糖，即形成染色后的无机纤维。
所述步骤1）中湿润等离子体是利用水蒸气与惰性气体的混合气体进行高压放电而形成的。
本发明另一个方面提供了一种黑色无机纤维的等离子体制备方法，包括以下步骤：
1）预处理：利用湿润等离子体对纤维基体进行表面改性获得活化后的纤维，在张力作用下将活化后的纤维在糖水溶液中浸泡；
2）碳化染色：将步骤1）所得经浸泡的纤维通过高温碳化，即得到黑色无机纤维；
所述步骤1）中湿润等离子体是利用水蒸气与惰性气体的混合气体进行高压放电而形成的。
在本发明的技术方案中，步骤1）中纤维基体选自玄武岩纤维、陶瓷纤维、石英纤维、海泡石纤维。
在本发明的技术方案中，步骤1）中所述的惰性气体选自氩气、氮气、氦气中的一种或多种的组合。
在本发明的技术方案中，步骤1）中所述的水蒸气与惰性气体的体积比为1:5-1:20，优选为1:8-1:12，更优选为1:10。
在本发明的技术方案中，步骤1）中所述的等离子体改性时间为2-10min。
在本发明的技术方案中，步骤1）中等离子体处理时对纤维施加张力，优选地所述的张力为1N以上，更优选为1-3N。
在本发明的技术方案中，步骤1）中浸泡糖水时，对活化后的纤维施加1N以上张力，优选为3-5N。
在本发明的技术方案中，步骤1）中所述糖水为糖的水溶液，所述的糖选自单体、二聚、寡聚体以及多聚的多羟基醛或酮。
在本发明的技术方案中，步骤2）中所述的碳化是在惰性气体的保护氛围下进行的，所述的惰性气体选自氩气或氮气。
在本发明的技术方案中，步骤3）中碳化的温度为500℃以上，优选为500-700℃。
在本发明的技术方案中，步骤3）中碳化时间为30～300min。
在本发明的技术方案中，步骤2）中糖水溶液的浓度为30%以上，优选为40-60%。
本发明再一个方面提供了本发明所述的方法制备获得的黑色无机纤维。
 有益效果
本发明公开了一种黑色无机纤维及其等离子体制备方法，所述的黑色无机纤维包括纤维基体及附在表面的碳膜组成。本发明的具体制备方法是：利用湿润等离子体，在一定张力下对无机纤维进行表面活化，使其表面具有大量的含氧活性基团，并增强其表面浸润性和吸附性。随后，在一定张力下，纤维浸泡在糖水溶液中，使含糖溶液浸入到纤维缝隙中。最后，利用高温碳化工艺，将糖碳化成黑色，从而得到黑色无机纤维。本发明方法新颖独特，简单高效，突破现有技术无法制备黑色无机纤维的限制，制得的黑色无机纤维性能优异、色牢度好，具有极好的实际应用前景。
本发明的目的在于提出一种利用等离子体技术来制备黑色无机纤维的方法及所得到的纤维，具有简单、高效等优点。
与现有技术相比，本发明可以实现无机纤维的染色，无需改变纤维的组成和成纤工艺，同时利用糖水作为染料来源，结合碳化工艺，可以避免化学染料的使用，也不产生染色废水。
 附图说明
图1为玄武岩纤维织造成的织物的照片，图片显示玄武岩纤维呈黄棕色。
图2为通过本发明方法染色处理后的黑色玄武岩纤维制品照片，图片显示染色后的产品呈黑色。
 本发明的实施方式
为了使本发明的上述目的、特征和优点能够更加明显易懂，下面结合附图对本发明的具体实施方式做详细的说明，但不能理解为对本发明的可实施范围的限定。
实施例1
将玄武岩纤维织造而成的织物（如图1所示，为黄棕色织物）置于等离子体氛围下，利用体积比为1：10的水蒸气和氩气混合放电，在2N的张力下对玄武岩纤维进行表面活化5min。随后在3N张力下，将活化后的织物按照浴比1：30浸入浓度为50%的糖水溶液中10min。取出织物后放置于管式炉中在500度的温度下氮气氛围保护碳化60min，随后在室温下用清水冲洗后，即得到黑色玄武岩纤维制品（如图2所示，为黑色织物）。经测试，黑色玄武岩纤维的耐水洗色牢度、耐摩擦色牢度均在3级以上，具有较好的染色效果。

Claims (10)

  1. 一种黑色无机纤维，包括纤维基体及附在纤维基体上的碳化糖组成，所述的纤维基体为耐受500℃以上的无机纤维，优选地，选自玄武岩纤维、陶瓷纤维、石英纤维、海泡石纤维。
  2. 根据权利要求1所述的黑色无机纤维，所述附在纤维基体上的碳化糖通过以下方法获得：
    1）预处理：利用湿润等离子体对纤维基体进行表面改性获得活化后的纤维，在张力作用下将活化后的纤维在糖水溶液中浸泡；
    2）碳化染色：将步骤1）所得经浸泡的纤维通过高温碳化，得到纤维基体上附有碳化糖，即形成染色后的无机纤维；
    所述步骤1）中湿润等离子体是利用水蒸气与惰性气体的混合气体进行高压放电而形成的。
  3. 一种黑色无机纤维的等离子体制备方法，包括以下步骤：
    1）预处理：利用湿润等离子体对纤维基体进行表面改性获得活化后的纤维，在张力作用下将活化后的纤维在糖水溶液中浸泡；
    2）碳化染色：将步骤1）所得经浸泡的纤维通过高温碳化，即得到黑色无机纤维；
    所述步骤1）中湿润等离子体是利用水蒸气与惰性气体的混合气体进行高压放电而形成的。
  4. 根据权利要求2所述的黑色无机纤维或权利要求3所述的等离子体制备方法，步骤1）中纤维基体选自玄武岩纤维、陶瓷纤维、石英纤维、海泡石纤维。
  5. 根据权利要求2所述的黑色无机纤维或权利要求3所述的等离子体制备方法，步骤1）中所述的惰性气体选自氩气、氮气、氦气中的一种或多种的组合；
    优选地，步骤1）中所述的水蒸气与惰性气体的体积比为1:5-1:20，更优选为1:8-1:12。
  6. 根据权利要求2所述的黑色无机纤维或权利要求3所述的等离子体制备方法，步骤1）中浸泡糖水时，对活化后的纤维施加1N以上张力，优选为3-5N。
  7. 根据权利要求2所述的黑色无机纤维或权利要求3所述的等离子体制备方法，步骤1）中等离子体处理时对纤维施加张力，优选地，所述的张力为1N以上，更优选为1-3N。
  8. 根据权利要求2所述的黑色无机纤维或权利要求3所述的等离子体制备方法，步骤1）中所述的糖水溶液为糖的水溶液，所述的糖选自单体、二聚、寡聚体以及多聚的多羟基醛或酮；
    优选地，步骤1）中糖水溶液的浓度为30%以上，优选为40%-60%。
  9. 根据权利要求2所述的黑色无机纤维或权利要求3所述的等离子体制备方法，步骤2）中碳化的温度为500℃以上，优选为500℃-700℃。
  10. 根据权利要求3-9任一项所述的等离子体制备方法制备获得的黑色无机纤维。
PCT/CN2020/129207 2019-12-02 2020-11-17 一种黑色无机纤维及其等离子体制备方法 WO2021109865A1 (zh)

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