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WO2016058110A1 - 一种多孔胶原蛋白改性的超细腈纶的制备方法 - Google Patents

一种多孔胶原蛋白改性的超细腈纶的制备方法 Download PDF

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WO2016058110A1
WO2016058110A1 PCT/CN2014/000902 CN2014000902W WO2016058110A1 WO 2016058110 A1 WO2016058110 A1 WO 2016058110A1 CN 2014000902 W CN2014000902 W CN 2014000902W WO 2016058110 A1 WO2016058110 A1 WO 2016058110A1
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solution
collagen
polymer solution
porous
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袁振其
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Taicang Su Lun Textile Chemical Fiber Co Ltd
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Taicang Su Lun Textile Chemical Fiber Co Ltd
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00—Treatment of filament-forming or like material
    • D01D1/02—Preparation of spinning solutions
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles

Definitions

  • the invention relates to a preparation method of ultrafine acrylic fiber, in particular to a preparation method of porous collagen modified ultrafine acrylic fiber.
  • acrylic fiber is a kind of synthetic fiber. Because of its soft, fluffy and warmth, it is always favored by the market. However, due to the relatively regular molecular structure of the acrylic fiber and the synthetic fiber, it is a hydrophobic fiber, lacking a hydrophilic group in the macromolecule, having a tight molecular chain structure, high crystallinity and orientation, and poor hydrophilicity. Traditional chemical modification consumes a lot of water and chemicals, which is not only complicated to operate but also pollutes the environment.
  • the electrospinning method is a device for producing polymer filaments by using electrostatic force.
  • the prepared inorganic fiber structure can be controlled by solution properties, spinning parameters and post-treatment to achieve morphology and structure, and exhibits excellent properties in the field of textile materials. characteristic. Since the molecular structure of the ultrafine acrylic fiber is relatively regular, its hydrophilicity and dyeability are poor, and the fuel easily forms dyed spots such as color flowers and stains on the dye.
  • HF Hydrofluoric acid
  • SiO 2 silica
  • SiO 2 +6HF H 2 SIF 6 +2H 2 O.
  • the SiO 2 sacrificial layer is etched by HF.
  • the acrylic fiber is expected to react differently with HF 2 to HF, the effect of pore-forming on the surface of the acrylic fiber can be achieved by means of particle doping and removal, thereby providing a comparative area of the fabric and improving the dyeability. the goal of.
  • a method for preparing porous collagen-modified ultrafine acrylic fiber comprising:
  • Acrylic fiber containing SiO 2 nanoparticles is soaked in HF solution and slowly stirred, washed and dried to obtain a porous protein collagen-modified ultrafine acrylic fabric.
  • the solvent is one of dimethylformamide or dimethylacetamide.
  • the mass fraction of collagen in the collagen solution is 3% to 7%.
  • the mass ratio of the polyphenylene nitrile to the solvent is 1:9 to 1:5, and the mass fraction of the polyvinylpyrrolidone is 10%; in the step 2), the fiber polymer solution and the collagen The mass ratio of the solution is 5:1-3:1, and the standing time is 1-2 h; in step 3), the mass fraction of the SiO 2 nanoparticles is 5-13%, and in step 4), the additional electric field The field strength is 0.2 kv/cm-2 kv/cm, the receiving screen is 10-45 cm from the spinneret, the baking temperature is 400-650 ° C, and in step 5), the mass fraction of the HF solution is 25-55%, Soak and slowly stir for 8-16h.
  • the mass ratio of the polyphenylene nitrile to the solvent is 1:7, the mass fraction of the polyvinylpyrrolidone is 10%; and in the step 2), the mass ratio of the fiber polymer solution to the collagen solution 4:1, the rest time is 1 h; in step 3), the mass fraction of SiO 2 nanoparticles is 8%, and in step 4), the additional electric field strength is 1 kv/cm, and the screen distance is required to be spun.
  • the mouth is 25 cm, the calcination temperature is 550 ° C, in step 5), the mass fraction of the HF solution is 45%, and the time of the soaking and slow stirring is 10 h.
  • porous ultrafine acrylic fiber has a diameter of 100 to 300 nm.
  • the collagen-modified ultrafine acrylic fiber is used, and since the collagen has good hygroscopicity, skin-friendly property and the like, combined with the chemical structural characteristics of the acrylic fiber, the hydrophilicity can be effectively improved, and the grooves and cracks on the surface of the fiber are filled.
  • the modified ultra-fine acrylic fiber has a soft touch and a smooth feel, and has the effect of silk-like silk.
  • the SiO2 sacrificial layer is etched by HF. Since the reaction of the ultrafine acrylic fiber and the SiO 2 to HF is different, the effect of the pores of the ultrafine acrylic fiber can be achieved by the method of particle doping and removal, mesoporous and microporous structure. Coexistence, can improve the specific surface area of the fabric, controllability of the structure, enhance the surface roughness, and achieve the hole making of the nano material, thereby improving the dyeability.
  • the polyacrylonitrile was dissolved in a solvent at a mass ratio of 1:9, 10% polyvinylpyrrolidone was added, and the fiber polymer solution was prepared by stirring uniformly; the solvent was dimethylacetamide.
  • the spinning solution was added to an electrospinning machine for electrospinning, the additional electric field strength was 0.2 kV/cm, the screen was received at a distance of 10 cm from the spinneret, and the firing temperature was 400 °C.
  • the ultrafine acrylic fiber containing SiO 2 nanoparticles was immersed in a 25% HF solution and slowly stirred for 8 hours, and washed and dried to obtain a porous collagen-modified ultrafine fiber.
  • the polyacrylonitrile was dissolved in a solvent at a mass ratio of 1:5, 10% polyvinylpyrrolidone was added, and the fiber polymer solution was prepared by stirring uniformly; the solvent was dimethylformamide.
  • SiO 2 nanoparticles were added to the protein collagen-modified fiber polymer solution, and magnetically stirred until uniform as a spin solution.
  • the spinning solution was added to an electrospinning machine to perform electrospinning with an additional electric field strength of 2 kV/cm, a screen distance of 45 cm from the spinneret, and a calcination temperature of 650 °C.
  • the acrylic fiber containing SiO 2 nanoparticles was soaked in a 55% HF solution and slowly stirred for 16 hours, and washed and dried to obtain a porous ultrafine acrylic fiber fabric to obtain a collagen-modified ultrafine fiber containing SiO 2 nanoparticles.
  • the polyacrylonitrile was dissolved in a solvent at a mass ratio of 1:6, 10% polyvinylpyrrolidone was added, and the fiber polymer solution was prepared by stirring uniformly; the solvent was dimethylformamide.
  • the spinning solution was added to an electrospinning machine to perform electrospinning, the additional electric field strength was 1 kV/cm, the screen was 25 cm from the spinneret, and the baking temperature was 550 °C.
  • the ultrafine acrylic fiber containing SiO 2 nanoparticles was immersed in a 45% HF solution and slowly stirred for 10 hours, and washed and dried to obtain a porous collagen-modified ultrafine acrylic fiber.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

一种多孔胶原蛋白改性的超细腈纶的制备方法，包括：将聚丙烯腈溶解于溶剂中，加入聚乙烯吡咯烷酮，搅拌均匀制备纤维聚合物溶液；在40℃的环境下，向纤维聚合物溶液中加入胶原蛋白溶液，磁力搅拌至均匀，静置，制成蛋白胶原改性纤维聚合物溶液；将SiO2纳米颗粒加入所述蛋白胶原改性纤维聚合物溶液中，磁力搅拌至均匀，作为喷丝溶液；将所述喷丝溶液灌入喷射器中，在附加电场的作用下喷丝，通过控制喷丝时间和移动接受屏，沉积在收集装置中，焙烧；将含SiO2纳米颗粒的腈纶纤维使用HF溶液浸泡并缓慢搅拌，清洗烘干，获得多孔蛋白胶原改性超细腈纶织物。通过本发明的制备方法，不仅可以改善织物的染色性，而且能使腈纶纤维具有手感柔软、滑糯，具有仿蚕丝的效果。

Description

一种多孔胶原蛋白改性的超细腈纶的制备方法 技术领域
本发明涉及一种超细腈纶的制备方法，特别是涉及一种多孔胶原蛋白改性的超细腈纶的制备方法。
背景技术
目前，随着人们生活水平的日益提高，消费观念的不断更新，消费者对腈纶纺织品，对其质量、品种、颜色等的要求越来越高。普遍使用的腈纶是一种合成纤维，因其手感柔软、蓬松、保暖性好，可替代羊毛的特点始终受到市场的青睐。但由于腈纶的分子结构比较规整，而且是合成纤维，属于疏水性纤维，大分子中缺乏亲水性基团，分子链结构紧密，结晶度和取向度均较高，其亲水性较差，传统的化学改性要消耗大量的水和化学药品，不仅操作复杂，而且污染环境。
静电纺丝方法是一种利用静电力生产聚合物细丝的装置，制备的无机纤维结构可通过溶液性质、纺丝参数以及后处理实现形态、结构的可控，在纺织材料领域展现出优异的特性。由于超细腈纶的分子结构比较规整，其亲水性和染色性较差，燃料容易在染物上形成色花、色斑等染疵。
综上所述，目前迫切需要一种胶原蛋白改性的超细腈纶的制备方法，能够改善提高织物的结构可控性，提高其染色性和固色性，使改性的腈纶纤维具有手感柔软、滑糯，具有仿蚕丝的效果。
发明内容
胶原蛋白是哺乳动物体中含量最丰富的蛋白质，具有良好的吸湿性、亲肤性等性能，结合腈纶的化学结构特点，能够有效改善亲水性差，填充 纤维表面的沟槽和裂缝，使改性的超细腈纶具有手感柔软、滑糯，具有仿蚕丝的效果。氢氟酸(HF)是一种弱酸，可以专一地与二氧化硅(SiO2)反应，其化学反应方程式为：SiO2+6HF＝H2SIF6+2H2O。使用HF腐蚀SiO2牺牲层，由于腈纶希望和SiO2对HF的反应不同，采用颗粒掺杂再去除的方式，可以达到对腈纶纤维表面制孔的效果，从而使用提供织物比较面积，提高染色性的目的。
为实现上述发明目的，本发明所提供的技术方案是：
一种多孔胶原蛋白改性的超细腈纶的制备方法，包括：
1)将聚丙烯腈溶解于溶剂中，加入聚乙烯吡咯烷酮，搅拌均匀制备纤维聚合物溶液；
2)在40℃的环境下，向纤维聚合物溶液中加入胶原蛋白溶液，磁力搅拌至均匀，静置，制成蛋白胶原改性纤维聚合物溶液；
3)将SiO2纳米颗粒加入所述蛋白胶原改性纤维聚合物溶液中，磁力搅拌至均匀，作为喷丝溶液；
4)将所述喷丝溶液灌入喷射器中，在附加电场的作用下喷丝，通过控制喷丝时间和移动接受屏，沉积在收集装置中，焙烧；
5)将含SiO2纳米颗粒的腈纶纤维使用HF溶液浸泡并缓慢搅拌，清洗烘干，获得多孔蛋白胶原改性超细腈纶织物。
进一步地，所述溶剂为二甲基甲酰胺或二甲基乙酰胺中的一种。
进一步地，所述胶原蛋白溶液中胶原蛋白的质量分数为3％-7％。
进一步地，在步骤1)中，聚苯烯腈与溶剂的质量比为1:9-1:5，聚乙烯吡咯烷酮的质量分数为10％；在步骤2)中，纤维聚合物溶液和胶原蛋白溶液的质量比为5:1-3:1，静置时间为1-2h；在步骤3)中，SiO2纳米颗粒的质量分数为5-13％，在步骤4)中，所述附加电场场强为0.2kv/cm-2kv/cm，接受屏距离喷丝口10-45cm，焙烧温度为400-650℃，在步骤5)中，所述HF溶液质量分数为25-55％，所述浸泡并缓慢搅拌的时间为8-16h。
进一步地，在步骤1)中，聚苯烯腈与溶剂的质量比为1:7，聚乙烯吡 咯烷酮的质量分数为10％；在步骤2)中，纤维聚合物溶液和胶原蛋白溶液的质量比为4:1，静置时间为1h；在步骤3)中，SiO2纳米颗粒的质量分数为8％，在步骤4)中，所述附加电场场强为1kv/cm，接受屏距离喷丝口25cm，焙烧温度为550℃，在步骤5)中，所述HF溶液质量分数为45％，所述浸泡并缓慢搅拌的时间为10h。
进一步地，所述多孔超细腈纶纤维的直径为100-300nm。
采用上述技术方案，本发明的有益效果有：
在本发明中使用胶原蛋白改性超细腈纶，由于胶原蛋白具有良好的吸湿性、亲肤性等性能，结合腈纶的化学结构特点，能够有效改善亲水性差，填充纤维表面的沟槽和裂缝，使改性的超细腈纶具有手感柔软、滑糯，具有仿蚕丝的效果。
在本发明中使用HF腐蚀SiO2牺牲层，由于超细腈纶和SiO2对HF的反应不同，采用颗粒掺杂再去除的方式，可以达到对超细腈纶制孔的效果，介孔和微孔结构共存其中，能够改善提高织物的比表面积、结构可控性，增强表面粗糙程度，实现对对纳米材料制孔，从而提高其染色性。
具体实施方式
实施例1
将聚丙烯腈溶解于溶剂中，质量比为1:9，加入10％的聚乙烯吡咯烷酮，搅拌均匀后制备纤维聚合物溶液；溶剂为二甲基乙酰胺。
在40℃的环境下，向纤维聚合物溶液中加入3％的胶原蛋白溶液，纤维聚合物溶液和胶原蛋白溶液质量比的5:1，磁力搅拌至均匀，静置1h后作为制成蛋白胶原改性纤维聚合物溶液。
将5％的SiO2纳米颗粒加入所述蛋白胶原改性纤维聚合物溶液中，磁力搅拌至均匀，作为喷丝溶液。
将喷丝溶液加入至静电纺丝机中，进行静电纺丝，附加电场场强为0.2kv/cm，接受屏距离喷丝口10cm，焙烧温度为400℃。
将含SiO2纳米颗粒的超细腈纶纤维使用25％的HF溶液浸泡并缓慢搅拌8h，清洗烘干，制得多孔的胶原蛋白改性超细纤维。
实施例2
将聚丙烯腈溶解于溶剂中，质量比为1:5，加入10％的聚乙烯吡咯烷酮，搅拌均匀后制备纤维聚合物溶液；溶剂为二甲基甲酰胺。
在40℃的环境下，向纤维聚合物溶液中加入7％的胶原蛋白溶液，纤维聚合物溶液和胶原蛋白溶液质量比的3:1，磁力搅拌至均匀，静置2h。
将13％的SiO2纳米颗粒加入所述蛋白胶原改性纤维聚合物溶液中，磁力搅拌至均匀，作为喷丝溶液。
将喷丝溶液加入至静电纺丝机中，进行静电纺丝，附加电场场强为2kv/cm，接受屏距离喷丝口45cm，焙烧温度为650℃。
将含SiO2纳米颗粒的腈纶纤维使用55％的HF溶液浸泡并缓慢搅拌16h，清洗烘干，获得多孔超细腈纶纤维织物，制得含SiO2纳米颗粒的胶原蛋白改性超细纤维。
实施例3
将聚丙烯腈溶解于溶剂中，质量比为1:6，加入10％的聚乙烯吡咯烷酮，搅拌均匀后制备纤维聚合物溶液；溶剂为二甲基甲酰胺。
在40℃的环境下，向纤维聚合物溶液中加入5％的胶原蛋白溶液，纤维聚合物溶液和胶原蛋白溶液质量比的4:1，磁力搅拌至均匀，静置1h。
将8％的SiO2纳米颗粒加入腈纶纤维聚合物溶液中，磁力搅拌至均匀，作为喷丝溶液。
将喷丝溶液加入至静电纺丝机中，进行静电纺丝，附加电场场强为1kv/cm，接受屏距离喷丝口25cm，焙烧温度为550℃。
将含SiO2纳米颗粒的超细腈纶纤维使用45％的HF溶液浸泡并缓慢搅拌10h，清洗烘干，制得多孔的胶原蛋白改性超细腈纶纤维。
以上所述实施例仅表达了本发明的实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对 于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。

Claims (6)

  1. 一种多孔胶原蛋白改性的超细腈纶的制备方法，其特征在于，包括：
    1)将聚丙烯腈溶解于溶剂中，加入聚乙烯吡咯烷酮，搅拌均匀制备纤维聚合物溶液；
    2)在40℃的环境下，向纤维聚合物溶液中加入胶原蛋白溶液，磁力搅拌至均匀，静置，制成蛋白胶原改性纤维聚合物溶液；
    3)将SiO2纳米颗粒加入所述蛋白胶原改性纤维聚合物溶液中，磁力搅拌至均匀，作为喷丝溶液；
    4)将所述喷丝溶液灌入喷射器中，在附加电场的作用下喷丝，通过控制喷丝时间和移动接受屏，沉积在收集装置中，焙烧；
    5)将含SiO2纳米颗粒的腈纶纤维使用HF溶液浸泡并缓慢搅拌，清洗烘干，获得多孔蛋白胶原改性超细腈纶织物。
  2. 根据权利要求1所述的多孔胶原蛋白改性的超细腈纶的制备方法，其特征在于，所述溶剂为二甲基甲酰胺或二甲基乙酰胺中的一种。
  3. 根据权利要求1所述的多孔胶原蛋白改性的超细腈纶的制备方法，其特征在于，所述胶原蛋白溶液中胶原蛋白的质量分数为3％-7％。
  4. 根据权利要求1所述的多孔胶原蛋白改性的超细腈纶的制备方法，其特征在于，在步骤1)中，聚苯烯腈与溶剂的质量比为1:9-1:5，聚乙烯吡咯烷酮的质量分数为10％；在步骤2)中，纤维聚合物溶液和胶原蛋白溶液的质量比为5:1-3:1，静置时间为1-2h；在步骤3)中，SiO2纳米颗粒的质量分数为5-13％，在步骤4)中，所述附加电场场强为0.2kv/cm-2kv/cm，接受屏距离喷丝口10-45cm，焙烧温度为400-650℃，在步骤5)中，所述HF溶液质量分数为25-55％，所述浸泡并缓慢搅拌的时间为8-16h。
  5. 根据权利要求4所述的多孔胶原蛋白改性的超细腈纶的制备方法，其特征在于，在步骤1)中，聚苯烯腈与溶剂的质量比为1:7，聚乙烯吡咯烷酮的质量分数为10％；在步骤2)中，纤维聚合物溶液和胶原蛋白溶液 的质量比为4:1，静置时间为1h；在步骤3)中，SiO2纳米颗粒的质量分数为8％，在步骤4)中，所述附加电场场强为1kv/cm，接受屏距离喷丝口25cm，焙烧温度为550℃，在步骤5)中，所述HF溶液质量分数为45％，所述浸泡并缓慢搅拌的时间为10h。
  6. 根据权利要求1-5任一项所述的多孔胶原蛋白改性的超细腈纶的制备方法，其特征在于，所述多孔超细腈纶纤维的直径为100-300nm。
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