CN111636117B - Preparation method of tough polyurethane nano composite fiber - Google Patents
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- 239000000835 fiber Substances 0.000 title claims abstract description 28
- 239000004814 polyurethane Substances 0.000 title claims abstract description 23
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 23
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000009987 spinning Methods 0.000 claims abstract description 18
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims abstract description 13
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims abstract description 13
- 239000006185 dispersion Substances 0.000 claims abstract description 8
- 239000012046 mixed solvent Substances 0.000 claims abstract description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 2
- 238000010041 electrostatic spinning Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 238000001523 electrospinning Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 239000004744 fabric Substances 0.000 abstract description 2
- 229920006306 polyurethane fiber Polymers 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
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- 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
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Abstract
本发明公开了一种强韧聚氨酯纳米复合纤维的制备方法，该制备方法是将热塑性聚氨酯溶解于体积比为1：2的四氢呋喃和N,N‑二甲基甲酰胺混合溶剂中,配制成浓度为150 mg/ml的热塑性聚氨酯溶液，然后加入浓度为15 mg/ml的改性氧化石墨烯N,N‑二甲基甲酰胺分散液，超声分散4小时，制得聚氨酯/改性氧化石墨烯纺丝液，利用静电纺丝技术将纺丝液在一定电压下纺丝，即得聚氨酯纳米复合纤维。该纤维同时具备高强度、高韧性和自修复能力。该纤维能被广泛应用于过滤材料、生物工程材料、防水透湿层压织物等领域。The invention discloses a preparation method of strong and tough polyurethane nano-composite fibers. The preparation method comprises the steps of dissolving thermoplastic polyurethane in a mixed solvent of tetrahydrofuran and N,N-dimethylformamide with a volume ratio of 1:2, and preparing a concentration of 150 mg/ml thermoplastic polyurethane solution, then adding modified graphene oxide N,N-dimethylformamide dispersion with a concentration of 15 mg/ml, and ultrasonically dispersing for 4 hours to obtain polyurethane/modified graphene oxide The spinning solution is spun under a certain voltage by using the electrospinning technology to obtain polyurethane nanocomposite fibers. The fiber has high strength, high tenacity and self-healing ability at the same time. The fiber can be widely used in filter materials, bioengineering materials, waterproof and moisture-permeable laminated fabrics and other fields.
Description
技术领域technical field
本发明涉及一种强韧聚氨酯纳米复合纤维的制备方法，属纤维生产领域。The invention relates to a preparation method of strong and tough polyurethane nano composite fiber, and belongs to the field of fiber production.
背景技术Background technique
聚氨酯纤维是指用聚氨酯为原料，经过化学方法加工而成的纤维。聚氨酯纤维共有两大品类。一类是由含有羟基的聚酯链段和芳香双异氰酸酯的镶嵌共聚物（简称聚酯型聚氨酯纤维），另一类是由含有羟基的聚醚链段和芳香双异氰酸酯的镶嵌共聚物（简称聚醚型聚氨酯纤维）。聚氨酯纤维同时具备高强度、高韧性、难燃和耐磨损等优异性能，被广泛应用于过滤材料、生物工程材料、防水透湿层压织物等领域。目前，为了进一步提升聚氨酯纤维的拉伸强度，会加入一些补强填料如石墨烯进行补强。然而，目前许多关于石墨烯补强聚氨酯的报道在提升拉伸强度的同时会牺牲材料延展性。如何同时提升并最优化纤维复合材料的强度与韧性，是材料科学界的一个重要问题。Polyurethane fiber refers to the fiber that is processed by chemical method using polyurethane as raw material. There are two types of polyurethane fibers. One is a mosaic copolymer composed of a hydroxyl-containing polyester segment and an aromatic diisocyanate (referred to as polyester polyurethane fiber), and the other is a mosaic copolymer composed of a hydroxyl-containing polyether segment and an aromatic diisocyanate (referred to as a mosaic copolymer). Polyether polyurethane fibers). Polyurethane fibers also have excellent properties such as high strength, high toughness, flame retardancy and wear resistance, and are widely used in filter materials, bioengineering materials, waterproof and moisture-permeable laminated fabrics and other fields. At present, in order to further improve the tensile strength of polyurethane fibers, some reinforcing fillers such as graphene are added for reinforcement. However, many current reports on graphene-reinforced polyurethanes increase tensile strength while sacrificing material ductility. How to simultaneously improve and optimize the strength and toughness of fiber composites is an important issue in the material science community.
发明内容SUMMARY OF THE INVENTION
本发明针对现有技术的不足，提供一种具备高强度、高韧性和自修复能力的强韧聚氨酯纳米复合纤维的制备方法。Aiming at the deficiencies of the prior art, the invention provides a preparation method of strong and tough polyurethane nanocomposite fibers with high strength, high toughness and self-repairing ability.
本发明提供的一种强韧聚氨酯纳米复合纤维的制备方法，该制备方法是将热塑性聚氨酯溶解于体积比为1：2的四氢呋喃和N,N-二甲基甲酰胺混合溶剂中,配制成浓度为150mg/ml的热塑性聚氨酯溶液，然后加入浓度为15 mg/ml的改性氧化石墨烯N, N-二甲基甲酰胺分散液，超声分散4小时，制得聚氨酯/改性氧化石墨烯纺丝液，利用静电纺丝技术将纺丝液在一定电压下纺丝，即得聚氨酯纳米复合纤维。The invention provides a preparation method of strong and tough polyurethane nanocomposite fibers. The preparation method comprises dissolving thermoplastic polyurethane in a mixed solvent of tetrahydrofuran and N,N-dimethylformamide with a volume ratio of 1:2 to prepare a concentration of 150 mg/ml thermoplastic polyurethane solution, then adding 15 mg/ml modified graphene oxide N, N-dimethylformamide dispersion, ultrasonically dispersing for 4 hours to prepare polyurethane/modified graphene oxide spinning The spinning solution is spun under a certain voltage by using the electrospinning technology to obtain the polyurethane nanocomposite fiber.
所述热塑性聚氨酯为聚酯型或聚醚型聚氨酯。The thermoplastic polyurethane is polyester or polyether polyurethane.
所述改性氧化石墨烯为氧化石墨烯表面用聚乙烯醇接枝改性而成，且聚乙烯醇在氧化石墨烯表面的接枝率为20～25%。The modified graphene oxide is obtained by grafting and modifying the surface of graphene oxide with polyvinyl alcohol, and the graft ratio of polyvinyl alcohol on the surface of graphene oxide is 20-25%.
所述接枝改性用聚乙烯醇的分子量为200～1000。The molecular weight of the polyvinyl alcohol for graft modification is 200-1000.
所述改性氧化石墨烯N, N-二甲基甲酰胺分散液的浓度为15 mg/ml。The concentration of the modified graphene oxide N, N-dimethylformamide dispersion liquid is 15 mg/ml.
聚氨酯与改性氧化石墨烯固含量重量比为100：1。The solid content weight ratio of polyurethane and modified graphene oxide is 100:1.
所述纺丝电压为19～22 kV。The spinning voltage is 19-22 kV.
本发明与现有技术相比，具有下述优点和有益效果：Compared with the prior art, the present invention has the following advantages and beneficial effects:
本发明中改性氧化石墨烯表面接枝的聚乙烯醇可与聚氨酯基体生成分子间氢键。氢键的解离能小于碳-碳共价键的解离能。在纤维拉伸过程中，这些氢键会首先发生逐步解离，从而消耗大量应变能，实现纤维强度与韧性的同时提升。在纤维停放或热处理过程中，氢键可重新生成从而实现纤维性能自修复。In the present invention, the polyvinyl alcohol grafted on the surface of the modified graphene oxide can form intermolecular hydrogen bonds with the polyurethane matrix. The dissociation energy of hydrogen bonds is less than that of carbon-carbon covalent bonds. In the process of fiber stretching, these hydrogen bonds will firstly dissociate gradually, which consumes a lot of strain energy and achieves the simultaneous improvement of fiber strength and toughness. During fiber parking or heat treatment, hydrogen bonds can be regenerated to achieve self-healing fiber properties.
具体实施方式Detailed ways
为了更好理解本发明，下面结合实施例对本发明作进一步地详细说明，但是本发明要求保护的范围并不局限于实施例表示的范围。In order to better understand the present invention, the present invention will be further described in detail below with reference to the embodiments, but the scope of protection claimed in the present invention is not limited to the scope represented by the embodiments.
实施例1Example 1
称取15 g热塑性聚氨酯溶解于100 ml体积比为1：2的四氢呋喃和N,N-二甲基甲酰胺混合溶剂中，然后加入 10 ml浓度为15 mg/ml的聚乙烯醇-200接枝改性氧化石墨烯N,N-二甲基甲酰胺分散液。超声分散4小时，制得聚氨酯/改性氧化石墨烯纺丝液。利用静电纺丝技术将纺丝液在21 kV电压下纺丝，即得聚氨酯纳米复合纤维。Weigh 15 g of thermoplastic polyurethane and dissolve it in 100 ml of a mixed solvent of tetrahydrofuran and N,N-dimethylformamide with a volume ratio of 1:2, and then add 10 ml of polyvinyl alcohol-200 with a concentration of 15 mg/ml to graft. Modified graphene oxide N,N-dimethylformamide dispersion. Ultrasonic dispersion was carried out for 4 hours to obtain a polyurethane/modified graphene oxide spinning solution. The spinning solution was spun at 21 kV using electrospinning technology to obtain polyurethane nanocomposite fibers.
实施例2Example 2
称取15 g热塑性聚氨酯溶解于100 ml体积比为1：2的四氢呋喃和N,N-二甲基甲酰胺混合溶剂中，然后加入 10 ml浓度为15 mg/ml的聚乙烯醇-600接枝改性氧化石墨烯N,N-二甲基甲酰胺分散液。超声分散4小时，制得聚氨酯/改性氧化石墨烯纺丝液。利用静电纺丝技术将纺丝液在21 kV电压下纺丝，即得聚氨酯纳米复合纤维。Weigh 15 g of thermoplastic polyurethane and dissolve it in 100 ml of a mixed solvent of tetrahydrofuran and N,N-dimethylformamide with a volume ratio of 1:2, and then add 10 ml of polyvinyl alcohol-600 with a concentration of 15 mg/ml to graft. Modified graphene oxide N,N-dimethylformamide dispersion. Ultrasonic dispersion was carried out for 4 hours to obtain a polyurethane/modified graphene oxide spinning solution. The spinning solution was spun at 21 kV using electrospinning technology to obtain polyurethane nanocomposite fibers.
实施例3Example 3
称取15 g热塑性聚氨酯溶解于100 ml体积比为1：2的四氢呋喃和N,N-二甲基甲酰胺混合溶剂中，然后加入 10 ml浓度为15 mg/ml的聚乙烯醇-1000接枝改性氧化石墨烯N,N-二甲基甲酰胺分散液。超声分散4小时，制得聚氨酯/改性氧化石墨烯纺丝液。利用静电纺丝技术将纺丝液在21 kV电压下纺丝，即得聚氨酯纳米复合纤维。Weigh 15 g of thermoplastic polyurethane and dissolve it in 100 ml of a mixed solvent of tetrahydrofuran and N,N-dimethylformamide with a volume ratio of 1:2, and then add 10 ml of polyvinyl alcohol-1000 with a concentration of 15 mg/ml to graft. Modified graphene oxide N,N-dimethylformamide dispersion. Ultrasonic dispersion was carried out for 4 hours to obtain a polyurethane/modified graphene oxide spinning solution. The spinning solution was spun at 21 kV using electrospinning technology to obtain polyurethane nanocomposite fibers.
对比例1Comparative Example 1
称取15 g热塑性聚氨酯溶解于100 ml体积比为1：2的四氢呋喃和N,N-二甲基甲酰胺混合溶剂中，超声分散4小时，制得聚氨酯/改性氧化石墨烯纺丝液。利用静电纺丝技术将纺丝液在21 kV电压下纺丝，即得聚氨酯纳米复合纤维。15 g of thermoplastic polyurethane was weighed and dissolved in 100 ml of a mixed solvent of tetrahydrofuran and N,N-dimethylformamide with a volume ratio of 1:2, and ultrasonically dispersed for 4 hours to obtain a polyurethane/modified graphene oxide spinning solution. The spinning solution was spun at 21 kV using electrospinning technology to obtain polyurethane nanocomposite fibers.
对比例2Comparative Example 2
称取15 g热塑性聚氨酯溶解于100 ml体积比为1：2的四氢呋喃和N,N-二甲基甲酰胺混合溶剂中，然后加入 10 ml浓度为15 mg/ml的氧化石墨烯N, N-二甲基甲酰胺分散液。超声分散4小时，制得聚氨酯/改性氧化石墨烯纺丝液。利用静电纺丝技术将纺丝液在21 kV电压下纺丝，即得聚氨酯纳米复合纤维。Weigh 15 g of thermoplastic polyurethane and dissolve it in 100 ml of a mixed solvent of tetrahydrofuran and N,N-dimethylformamide with a volume ratio of 1:2, and then add 10 ml of graphene oxide N,N- Dimethylformamide dispersion. Ultrasonic dispersion was carried out for 4 hours to obtain a polyurethane/modified graphene oxide spinning solution. The spinning solution was spun at 21 kV using electrospinning technology to obtain polyurethane nanocomposite fibers.
按照实施例1～3和对比例1～2制备的样品主要物理机械性能如表1。从表1可见，纯聚氨酯纤维(对比例1)的拉伸强度、断裂伸长率和断裂能分别为5.2 MPa、420%和0.87*103 J/m2。聚氨酯/氧化石墨烯纳米复合纤维的拉伸强度上升到11.4 MPa，但断裂伸长率却下降到350%。这表明添加未改性的氧化石墨烯在提升纤维强度的同时，会使纤维的断裂伸长率下降。而添加聚乙烯醇接枝改性氧化石墨烯的纤维，拉伸强度、断裂伸长率和断裂能同时得到提升。The main physical and mechanical properties of the samples prepared according to Examples 1-3 and Comparative Examples 1-2 are shown in Table 1. It can be seen from Table 1 that the tensile strength, elongation at break and breaking energy of pure polyurethane fiber (Comparative Example 1) are 5.2 MPa, 420% and 0.87*10 3 J/m 2 , respectively. The tensile strength of the polyurethane/graphene oxide nanocomposite fiber increased to 11.4 MPa, but the elongation at break decreased to 350%. This shows that the addition of unmodified graphene oxide can increase the fiber strength while reducing the elongation at break of the fiber. The addition of polyvinyl alcohol graft modified graphene oxide fibers, the tensile strength, elongation at break and breaking energy are simultaneously improved.
表1 样品主要物理机械性能表Table 1 The main physical and mechanical properties of the samples
以上所述是本发明的优选实施方式而已，当然不能以此来限定本发明之权利范围，应当指出，对于本技术领域的普通技术人员来说，对本发明的技术方案进行修改或者等同替换，都不脱离本发明技术方案的保护范围。The above are only the preferred embodiments of the present invention, of course, the scope of the rights of the present invention cannot be limited by this. Without departing from the protection scope of the technical solution of the present invention.
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| "Electrospinning thermoplastic polyurethane/graphene oxide scaffolds for small diameter vascular graft applications"，Xin Jing等，Materials Science and Engineering C，第40-50页;Xin Jing等;《Materials Science and Engineering C》;20141218;第40-50页 * |
| HPNGO/TPU复合纳米纤维的制备及其结构与性能研究;单体坤等;《合成纤维工业》;20190415(第02期);第45-48页 * |
| 静电纺丝热塑性聚氨酯纳米纤维的制备;张丽等;《聚氨酯工业》;20130628(第03期);第29-31页 * |
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