CN118516777A - High elastic tensile-resistant fabric and preparation method thereof - Google Patents
High elastic tensile-resistant fabric and preparation method thereof Download PDFInfo
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- CN118516777A CN118516777A CN202410613228.1A CN202410613228A CN118516777A CN 118516777 A CN118516777 A CN 118516777A CN 202410613228 A CN202410613228 A CN 202410613228A CN 118516777 A CN118516777 A CN 118516777A
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- 239000004744 fabric Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title 1
- 239000000835 fiber Substances 0.000 claims abstract description 60
- 238000009987 spinning Methods 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims description 80
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- 239000007795 chemical reaction product Substances 0.000 claims description 25
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 21
- 238000010992 reflux Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 16
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 16
- 238000001291 vacuum drying Methods 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- SKNUPXIXICTRJE-UHFFFAOYSA-N 1-butyl-4-chlorobenzene Chemical compound CCCCC1=CC=C(Cl)C=C1 SKNUPXIXICTRJE-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 8
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000005457 ice water Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 229940078552 o-xylene Drugs 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 239000011630 iodine Substances 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000012074 organic phase Substances 0.000 claims description 4
- 238000009941 weaving Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 3
- 125000003277 amino group Chemical group 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229920005575 poly(amic acid) Polymers 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 7
- 238000001914 filtration Methods 0.000 claims 5
- 230000001376 precipitating effect Effects 0.000 claims 4
- 230000001276 controlling effect Effects 0.000 claims 3
- 238000001816 cooling Methods 0.000 claims 2
- 238000002390 rotary evaporation Methods 0.000 claims 2
- 150000008065 acid anhydrides Chemical class 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 230000001546 nitrifying effect Effects 0.000 claims 1
- 230000001590 oxidative effect Effects 0.000 claims 1
- 230000000379 polymerizing effect Effects 0.000 claims 1
- 238000005086 pumping Methods 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 239000004753 textile Substances 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 238000007792 addition Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009940 knitting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- KDLHZDBZIXYQEI-VENIDDJXSA-N palladium-100 Chemical compound [100Pd] KDLHZDBZIXYQEI-VENIDDJXSA-N 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- 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
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/74—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
- C08G73/1071—Wholly aromatic polyimides containing oxygen in the form of ether bonds in the main chain
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
- D03D15/283—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明涉及纺织面料领域,具体涉及一种高弹抗拉面料及其制备方法,用于解决了现有的弹性面料的抗拉伸性能和弹性性能不佳的问题;该制备方法利用高弹抗拉纤维纺丝液制备得到高弹抗拉纤维,该高弹抗拉纤维的分子结构上含有大量的环状结构,赋予了高弹抗拉纤维良好的力学性能,使其能够受力而不会轻易破坏,高弹抗拉纤维的分子结构上还含有大量的长碳链从而赋予了其良好的柔软性,使其弹性大幅度提升,从而使得由高弹抗拉纤维制备的高弹抗拉面料具有优良的抗拉性能,具有高弹性,使其能够在拉伸后不会被轻易破坏,且使其能够快速回弹,不会变形,大幅度提升了高弹抗拉面料的适用范围。The invention relates to the field of textile fabrics, and in particular to a high-elastic tensile-resistant fabric and a preparation method thereof, which are used to solve the problem of poor tensile resistance and elasticity of existing elastic fabrics; the preparation method uses a high-elastic tensile-resistant fiber spinning solution to prepare a high-elastic tensile-resistant fiber, the molecular structure of the high-elastic tensile-resistant fiber contains a large number of ring structures, which give the high-elastic tensile-resistant fiber good mechanical properties, so that it can be subjected to force without being easily damaged, and the molecular structure of the high-elastic tensile-resistant fiber also contains a large number of long carbon chains, thereby giving it good softness and greatly improving its elasticity, so that the high-elastic tensile-resistant fabric prepared from the high-elastic tensile-resistant fiber has excellent tensile resistance and high elasticity, so that it can not be easily damaged after being stretched, and can rebound quickly without deformation, thereby greatly improving the application range of the high-elastic tensile-resistant fabric.
Description
技术领域Technical Field
本发明涉及纺织面料领域,具体涉及一种高弹抗拉面料及其制备方法。The invention relates to the field of textile fabrics, and in particular to a high-elastic tensile-resistant fabric and a preparation method thereof.
背景技术Background Art
随着社会和经济的发展,人们生活水平的提高,单一功能的纺织品已远远不能满足人们的需求,多功能整理的纺织品因其优良的性能越来越得到人们的认可和使用。现有的弹性面料大多为一面为胶片另一面为织物面料的复合面料,复合面料是通过粘合剂将胶片与织物面料粘合,由于粘合剂是水溶性的,胶与织物面料很容易分离,特别是经水洗后织物面料与胶片基本分离起不到回弹塑身作用,影响塑形效果,而且现有的弹性面料虽然具备一定的抗拉伸和抗褶皱能力,但是,在承受较大的拉伸和拉拽时,极易发生面料变形,同时弹性不佳,甚至会给面料造成较大的损害,部分撕裂就会导致面料层的破损漏洞,面料的抗拉拽能力有限,使得面料无法承受强拉拽力,降低了面料的适用范围。With the development of society and economy, and the improvement of people's living standards, textiles with single functions can no longer meet people's needs. Textiles with multifunctional finishing are increasingly recognized and used by people due to their excellent performance. Most of the existing elastic fabrics are composite fabrics with film on one side and fabric on the other side. The composite fabric is made by bonding the film and fabric with adhesive. Since the adhesive is water-soluble, the adhesive and the fabric are easily separated. Especially after washing, the fabric and the film are basically separated and cannot play a role in rebounding and shaping, which affects the shaping effect. Although the existing elastic fabrics have certain tensile and wrinkle resistance, they are very easy to deform when subjected to large stretching and pulling. At the same time, the elasticity is poor, and it may even cause great damage to the fabric. Partial tearing will cause damage and holes in the fabric layer. The fabric has limited tensile resistance, which makes the fabric unable to withstand strong pulling force, reducing the scope of application of the fabric.
如何改善现有的弹性面料的抗拉伸性能和弹性性能不佳是本发明的关键,因此,亟需一种高弹抗拉面料及其制备方法来解决以上问题。How to improve the poor tensile strength and elasticity of existing elastic fabrics is the key to the present invention. Therefore, a high-elastic tensile-resistant fabric and a preparation method thereof are urgently needed to solve the above problems.
发明内容Summary of the invention
为了克服上述的技术问题,本发明的目的在于提供一种高弹抗拉面料及其制备方法:通过将高弹抗拉纤维纺丝液由喷丝板喷入乙醇溶液中,得到预成型纤维,将预成型纤维用蒸馏水洗涤,之后放置于真空干燥箱中干燥,之后放置于管式炉中干燥,得到高弹抗拉纤维,将高弹抗拉纤维进行编制成型,得到该高弹抗拉面料,解决了现有的弹性面料的抗拉伸性能和弹性性能不佳的问题。In order to overcome the above-mentioned technical problems, the purpose of the present invention is to provide a high-elastic tensile-resistant fabric and a preparation method thereof: by spraying a high-elastic tensile-resistant fiber spinning solution into an ethanol solution from a spinneret to obtain a preformed fiber, washing the preformed fiber with distilled water, and then placing it in a vacuum drying oven for drying, and then placing it in a tubular furnace for drying to obtain a high-elastic tensile-resistant fiber, and the high-elastic tensile-resistant fiber is knitted and formed to obtain the high-elastic tensile-resistant fabric, thereby solving the problem of poor tensile resistance and elasticity of existing elastic fabrics.
本发明的目的可以通过以下技术方案实现:The purpose of the present invention can be achieved through the following technical solutions:
一种高弹抗拉面料的制备方法,包括以下步骤:A method for preparing a high-elastic tensile-resistant fabric comprises the following steps:
步骤一:将高弹抗拉纤维纺丝液在压力为0.3-0.4MPa的条件下,由喷丝板喷入体积分数为40-50%的乙醇溶液中,得到预成型纤维;Step 1: Spraying the high-elastic tensile fiber spinning solution into an ethanol solution with a volume fraction of 40-50% from a spinneret under a pressure of 0.3-0.4 MPa to obtain a preformed fiber;
步骤二:将预成型纤维用蒸馏水洗涤3-5次,之后放置于真空干燥箱中,在温度为60-70℃的条件下干燥3-5h,之后放置于管式炉中,之后在温度为200℃的条件下干燥2-2.5h,之后升温至280℃的条件下干燥1.5-2h,之后升温至310℃的条件下干燥1-1.5h,得到高弹抗拉纤维;Step 2: Wash the preformed fiber with distilled water for 3-5 times, then place it in a vacuum drying oven, dry it at a temperature of 60-70°C for 3-5h, then place it in a tube furnace, then dry it at a temperature of 200°C for 2-2.5h, then heat it to 280°C for 1.5-2h, then heat it to 310°C for 1-1.5h, to obtain a high elastic tensile fiber;
步骤三:将高弹抗拉纤维进行编制成型,得到该高弹抗拉面料。Step 3: Weaving the high-elastic tensile-resistant fibers into a shape to obtain the high-elastic tensile-resistant fabric.
反应原理如下:The reaction principle is as follows:
作为本发明进一步的方案:所述高弹抗拉纤维纺丝液由以下步骤制备得到:As a further solution of the present invention: the high elastic tensile fiber spinning solution is prepared by the following steps:
步骤A1:将4-正丁基氯苯加入至安装有搅拌器、温度计、恒压滴液漏斗以及回流冷凝管的四口烧瓶中,在温度为-5-0℃,搅拌速率为400-500r/min的条件下边搅拌边逐滴加入混合酸,控制滴加速率为1-2滴/s,滴加完毕后升温至70-75℃的条件下继续搅拌反应5-6h,反应结束后将反应产物加入至冰水中,之后用无水乙醚萃取2-3次,将有机相用饱和碳酸钠溶液洗涤2-3次,之后用无水硫酸钠干燥,之后真空抽滤,将滤液旋转蒸发去除溶剂,得到中间体1;Step A1: 4-n-butylchlorobenzene is added to a four-necked flask equipped with a stirrer, a thermometer, a constant pressure dropping funnel and a reflux condenser, and a mixed acid is added dropwise while stirring at a temperature of -5-0°C and a stirring rate of 400-500r/min, and the dropping rate is controlled to be 1-2 drops/s. After the dropwise addition is completed, the temperature is raised to 70-75°C and the stirring reaction is continued for 5-6h. After the reaction is completed, the reaction product is added to ice water, and then extracted with anhydrous ether for 2-3 times. The organic phase is washed with a saturated sodium carbonate solution for 2-3 times, and then dried with anhydrous sodium sulfate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain intermediate 1;
反应原理如下:The reaction principle is as follows:
步骤A2:将中间体1、对苯二酚、碳酸钾以及N,N-二甲基甲酰胺加入至安装有搅拌器、温度计以及导气管的三口烧瓶中,通入氮气保护,在温度为150-155℃,搅拌速率为400-500r/min的条件下搅拌反应6-8h,反应结束后将反应产物冷却至室温,之后加入至冰水中,析出沉淀,之后真空抽滤,将滤饼放置于真空干燥箱中,在温度为60-70℃的条件下干燥3-5h,得到中间体2;Step A2: Add intermediate 1, hydroquinone, potassium carbonate and N,N-dimethylformamide to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, introduce nitrogen protection, stir and react for 6-8 hours at a temperature of 150-155° C. and a stirring rate of 400-500 r/min. After the reaction is completed, the reaction product is cooled to room temperature, then added to ice water to precipitate, and then vacuum filtered. The filter cake is placed in a vacuum drying oven and dried at a temperature of 60-70° C. for 3-5 hours to obtain intermediate 2;
反应原理如下:The reaction principle is as follows:
步骤A3:将中间体2、5%钯碳以及无水乙醇加入至安装有搅拌器、温度计以及恒压滴液漏斗的三口烧瓶中,在温度为25-30℃,搅拌速率为400-500r/min的条件下边搅拌边逐滴加入水合肼溶液,控制滴加速率为1-2滴/s,滴加完毕后升温至70-75℃的条件下继续搅拌反应5-6h,反应结束后将反应产物加入至蒸馏水中,析出沉淀,之后真空抽滤,将滤饼放置于真空干燥箱中,在温度为60-70℃的条件下干燥3-5h,得到中间体3;Step A3: Add intermediate 2, 5% palladium carbon and anhydrous ethanol to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, add hydrazine hydrate solution dropwise while stirring at a temperature of 25-30°C and a stirring rate of 400-500r/min, and control the dropping rate to 1-2 drops/s. After the dropwise addition is completed, the temperature is raised to 70-75°C and the stirring reaction is continued for 5-6h. After the reaction is completed, the reaction product is added to distilled water to precipitate, and then vacuum filtered. The filter cake is placed in a vacuum drying oven and dried at a temperature of 60-70°C for 3-5h to obtain intermediate 3;
反应原理如下:The reaction principle is as follows:
步骤A4:将邻二甲苯、碘以及铁粉加入至安装有搅拌器、温度计以及恒压滴液漏斗的三口烧瓶中,在温度为0-5℃,搅拌速率为400-500r/min的条件下边搅拌边逐滴加入液溴,控制滴加速率为1-2滴/s,滴加完毕后升温至25-30℃的条件下继续搅拌反应8-10h,反应结束后向反应产物中滴加氢氧化钠溶液直至红色褪去,之后真空抽滤,将滤液常压蒸馏,收集温度为214-215℃的馏分,得到中间体4;Step A4: o-xylene, iodine and iron powder are added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and liquid bromine is added dropwise while stirring at a temperature of 0-5°C and a stirring rate of 400-500r/min, and the dropping rate is controlled to be 1-2 drops/s. After the addition is completed, the temperature is raised to 25-30°C and the stirring reaction is continued for 8-10 hours. After the reaction is completed, sodium hydroxide solution is added dropwise to the reaction product until the red color fades, and then vacuum filtration is performed, and the filtrate is distilled at atmospheric pressure, and the fraction with a temperature of 214-215°C is collected to obtain intermediate 4;
反应原理如下:The reaction principle is as follows:
步骤A5:将中间体4、二氯二甲基硅烷、钠以及甲苯加入至安装有搅拌器、温度计以及回流冷凝管的三口烧瓶中,在温度为25-30℃,搅拌速率为400-500r/min的条件下搅拌反应20-25min,之后升温至回流的条件下继续搅拌反应1-2h,反应结束后将反应产物旋转蒸发去除甲苯,之后减压蒸馏,收集压力为0.002MPa,温度为226-229℃的馏分,得到中间体5;Step A5: Add intermediate 4, dichlorodimethylsilane, sodium and toluene into a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, stir and react for 20-25 minutes at a temperature of 25-30° C. and a stirring rate of 400-500 r/min, then heat to reflux and continue stirring and reacting for 1-2 hours. After the reaction is completed, the reaction product is rotary evaporated to remove toluene, and then distilled under reduced pressure to collect a fraction with a pressure of 0.002 MPa and a temperature of 226-229° C. to obtain intermediate 5;
反应原理如下:The reaction principle is as follows:
步骤A6:将中间体5、吡啶、高锰酸钾以及去离子水加入至安装有搅拌器、温度计以及回流冷凝管的三口烧瓶中,在温度为25-30℃,搅拌速率为400-500r/min的条件下搅拌反应20-25min,之后升温至回流的条件下继续搅拌反应1-2h,之后加入无水甲醇继续搅拌反应1-2h,反应结束后将反应产物冷却至室温,之后真空抽滤,将滤液用盐酸溶液调节pH为1-2,析出沉淀,之后真空抽滤,将滤饼加入至乙酸酐中,之后在温度70-80℃,搅拌速率为400-500r/min的条件下搅拌反应2-3h,之后旋转蒸发去除溶解,之后用正己烷重结晶,得到中间体6;Step A6: Add intermediate 5, pyridine, potassium permanganate and deionized water to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, stir and react for 20-25 minutes at a temperature of 25-30°C and a stirring rate of 400-500r/min, then heat to reflux and continue stirring and reacting for 1-2 hours, then add anhydrous methanol and continue stirring and reacting for 1-2 hours, after the reaction is completed, cool the reaction product to room temperature, then vacuum filter, adjust the pH of the filtrate to 1-2 with hydrochloric acid solution, precipitate, then vacuum filter, add the filter cake to acetic anhydride, then stir and react for 2-3 hours at a temperature of 70-80°C and a stirring rate of 400-500r/min, then rotary evaporate to remove the solvent, and then recrystallize with n-hexane to obtain intermediate 6;
反应原理如下:The reaction principle is as follows:
步骤A7:将中间体3、中间体6以及N,N-二甲基乙酰胺加入至安装有搅拌器、温度计的三口烧瓶中,在温度为35-40℃,搅拌速率为400-500r/min的条件下搅拌反应10-15h,得到高弹抗拉纤维纺丝液。Step A7: Add intermediate 3, intermediate 6 and N,N-dimethylacetamide to a three-necked flask equipped with a stirrer and a thermometer, and stir the reaction for 10-15 hours at a temperature of 35-40°C and a stirring rate of 400-500 r/min to obtain a high-elastic tensile fiber spinning solution.
反应原理如下:The reaction principle is as follows:
作为本发明进一步的方案:步骤A1中的所述4-正丁基氯苯、混合酸的用量比为1g:5-10mL,所述混合酸为浓硫酸、浓硝酸以及去离子水按照25-30g:65-70g:3-6g混合而成的混合物,所述浓硫酸的质量分数为95-98%,所述浓硝酸的质量分数为66-67%。As a further scheme of the present invention: the dosage ratio of the 4-n-butylchlorobenzene and the mixed acid in step A1 is 1g:5-10mL, the mixed acid is a mixture of concentrated sulfuric acid, concentrated nitric acid and deionized water according to 25-30g:65-70g:3-6g, the mass fraction of the concentrated sulfuric acid is 95-98%, and the mass fraction of the concentrated nitric acid is 66-67%.
作为本发明进一步的方案:步骤A2中的所述中间体1、对苯二酚、碳酸钾以及N,N-二甲基甲酰胺的用量比为0.2-0.22mo l:0.1mo l:0.2-0.22mo l:100-120mL。As a further scheme of the present invention: the usage ratio of the intermediate 1, hydroquinone, potassium carbonate and N,N-dimethylformamide in step A2 is 0.2-0.22 mol: 0.1 mol: 0.2-0.22 mol: 100-120 mL.
作为本发明进一步的方案:步骤A3中的所述中间体2、5%钯碳、无水乙醇以及水合肼溶液的用量比为10mmo l:0.25-0.35g:80-100mL:12-15mL,所述水合肼溶液的质量分数为64-65%。As a further scheme of the present invention: the usage ratio of the intermediate 2, 5% palladium carbon, anhydrous ethanol and hydrazine hydrate solution in step A3 is 10 mmol: 0.25-0.35 g: 80-100 mL: 12-15 mL, and the mass fraction of the hydrazine hydrate solution is 64-65%.
作为本发明进一步的方案:步骤A4中的所述邻二甲苯、碘、铁粉以及液溴的用量比为0.1mo l:0.1-0.15g:0.2-0.25g:0.11-0.13mo l,所述氢氧化钠溶液的质量分数为5-10%。As a further solution of the present invention: the dosage ratio of the o-xylene, iodine, iron powder and liquid bromine in step A4 is 0.1 mol: 0.1-0.15 g: 0.2-0.25 g: 0.11-0.13 mol, and the mass fraction of the sodium hydroxide solution is 5-10%.
作为本发明进一步的方案:步骤A5中的所述中间体4、二氯二甲基硅烷、钠以及甲苯的用量比为0.2mo l:0.1mo l:0.1mo l:120-150mL。As a further solution of the present invention: the usage ratio of the intermediate 4, dichlorodimethylsilane, sodium and toluene in step A5 is 0.2 mol: 0.1 mol: 0.1 mol: 120-150 mL.
作为本发明进一步的方案:步骤A6中的所述中间体5、吡啶、高锰酸钾、去离子水、无水甲醇以及乙酸酐的用量比为10mmo l:70-80mL:25-30g:20-30mL:3-5mL:25-30mL,所述盐酸溶液的质量分数为20-25%。As a further scheme of the present invention: the usage ratio of the intermediate 5, pyridine, potassium permanganate, deionized water, anhydrous methanol and acetic anhydride in step A6 is 10 mmol: 70-80 mL: 25-30 g: 20-30 mL: 3-5 mL: 25-30 mL, and the mass fraction of the hydrochloric acid solution is 20-25%.
作为本发明进一步的方案:步骤A7中的所述中间体3、中间体6以及N,N-二甲基乙酰胺的用量比5mmo l:5mmo l:300-350g。As a further solution of the present invention: the usage ratio of the intermediate 3, intermediate 6 and N,N-dimethylacetamide in step A7 is 5 mmol:5 mmol:300-350 g.
作为本发明进一步的方案:一种高弹抗拉面料,所述高弹抗拉面料根据所述的高弹抗拉面料的制备方法制备得到。As a further solution of the present invention: a high-elastic tensile-resistant fabric, the high-elastic tensile-resistant fabric is prepared according to the preparation method of the high-elastic tensile-resistant fabric.
本发明的有益效果:Beneficial effects of the present invention:
本发明的一种高弹抗拉面料及其制备方法,通过将高弹抗拉纤维纺丝液由喷丝板喷入乙醇溶液中,得到预成型纤维,将预成型纤维用蒸馏水洗涤,之后放置于真空干燥箱中干燥,之后放置于管式炉中干燥,得到高弹抗拉纤维,将高弹抗拉纤维进行编制成型,得到该高弹抗拉面料;该制备方法利用高弹抗拉纤维纺丝液制备得到高弹抗拉纤维,由高弹抗拉纤维制备的高弹抗拉面料具有优良的抗拉性能,具有高弹性,使其能够在拉伸后不会被轻易破坏,且使其能够快速回弹,不会变形,大幅度提升了高弹抗拉面料的适用范围;The invention discloses a high-elastic tensile-resistant fabric and a preparation method thereof. The method comprises the following steps: spraying a high-elastic tensile-resistant fiber spinning solution into an ethanol solution from a spinneret to obtain a preformed fiber, washing the preformed fiber with distilled water, and then placing the preformed fiber in a vacuum drying oven for drying, and then placing the preformed fiber in a tubular furnace for drying to obtain a high-elastic tensile-resistant fiber, and knitting the high-elastic tensile-resistant fiber to obtain the high-elastic tensile-resistant fabric. The preparation method uses the high-elastic tensile-resistant fiber spinning solution to prepare the high-elastic tensile-resistant fiber. The high-elastic tensile-resistant fabric prepared from the high-elastic tensile-resistant fiber has excellent tensile resistance and high elasticity, so that the fiber will not be easily damaged after being stretched, and can rebound quickly without deformation, thereby greatly improving the application range of the high-elastic tensile-resistant fabric.
在制备高弹抗拉面料的过程中首先制备了一种高弹抗拉纤维纺丝液,首先利用混合酸将4-正丁基氯苯进行硝化,引入硝基,得到中间体1,之后中间体1与对苯二酚发生反应,得到中间体2,之后利用水合肼将中间体2上的硝基还原成氨基,得到中间体3,利用液溴将邻二甲苯进行溴化,引入溴原子,得到中间体4,之后中间体4与二氯二甲基硅烷反应生成中间体5,之后中间体5上的甲基在高锰酸钾的氧化下形成羧基,之后在乙酸酐中形成酸酐,得到中间体6,之后中间体3与中间体6聚合反应形成聚酰胺酸,得到高弹抗拉纤维纺丝液;该高弹抗拉纤维纺丝液纺丝成型后在高温下脱水缩合进行定型,得到高弹抗拉纤维,该高弹抗拉纤维的分子结构上含有大量的环状结构,赋予了高弹抗拉纤维良好的力学性能,使其能够受力而不会轻易破坏,高弹抗拉纤维的分子结构上还含有大量的长碳链从而赋予了其良好的柔软性,使其弹性大幅度提升,从而使得制备得到的面料具有高弹抗拉性能。In the process of preparing high-elastic tensile-resistant fabrics, a high-elastic tensile-resistant fiber spinning solution is first prepared. First, 4-n-butylchlorobenzene is nitrated by a mixed acid to introduce a nitro group to obtain an intermediate 1. Then, the intermediate 1 reacts with hydroquinone to obtain an intermediate 2. Then, the nitro group on the intermediate 2 is reduced to an amino group by hydrazine hydrate to obtain an intermediate 3. Then, o-xylene is brominated by liquid bromine to introduce a bromine atom to obtain an intermediate 4. Then, the intermediate 4 reacts with dichlorodimethylsilane to generate an intermediate 5. Then, the methyl group on the intermediate 5 is oxidized by potassium permanganate to form a carboxyl group, and then an acid is formed in acetic anhydride. anhydride to obtain intermediate 6, then intermediate 3 and intermediate 6 are polymerized to form polyamic acid to obtain a high-elastic tensile-resistant fiber spinning solution; after the high-elastic tensile-resistant fiber spinning solution is spun into shape, it is dehydrated and condensed at high temperature to be shaped to obtain a high-elastic tensile-resistant fiber. The molecular structure of the high-elastic tensile-resistant fiber contains a large number of ring structures, which give the high-elastic tensile-resistant fiber good mechanical properties, so that it can be stressed without being easily damaged. The molecular structure of the high-elastic tensile-resistant fiber also contains a large number of long carbon chains, which give it good softness and greatly improve its elasticity, so that the prepared fabric has high elastic tensile properties.
具体实施方式DETAILED DESCRIPTION
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
实施例1:Embodiment 1:
本实施例为一种高弹抗拉纤维纺丝液的制备方法,包括以下步骤:This embodiment is a method for preparing a high-elastic tensile-resistant fiber spinning solution, comprising the following steps:
步骤A1:将1g4-正丁基氯苯加入至安装有搅拌器、温度计、恒压滴液漏斗以及回流冷凝管的四口烧瓶中,在温度为-5℃,搅拌速率为400r/min的条件下边搅拌边逐滴加入5mL质量分数为95%的浓硫酸、质量分数为66%的浓硝酸以及去离子水按照25g:65g:3g混合而成的混合酸,控制滴加速率为1滴/s,滴加完毕后升温至70℃的条件下继续搅拌反应5h,反应结束后将反应产物加入至冰水中,之后用无水乙醚萃取2次,将有机相用饱和碳酸钠溶液洗涤2次,之后用无水硫酸钠干燥,之后真空抽滤,将滤液旋转蒸发去除溶剂,得到中间体1;Step A1: Add 1 g of 4-n-butylchlorobenzene to a four-necked flask equipped with a stirrer, a thermometer, a constant pressure dropping funnel and a reflux condenser, and add dropwise 5 mL of a mixed acid prepared by mixing 95% concentrated sulfuric acid, 66% concentrated nitric acid and deionized water in a ratio of 25 g: 65 g: 3 g at a temperature of -5°C and a stirring rate of 400 r/min, with stirring, and the dropping rate is controlled to be 1 drop/s. After the dropwise addition is completed, the temperature is raised to 70°C and the stirring reaction is continued for 5 hours. After the reaction is completed, the reaction product is added to ice water, and then extracted twice with anhydrous ether. The organic phase is washed twice with a saturated sodium carbonate solution, and then dried with anhydrous sodium sulfate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain intermediate 1;
步骤A2:将0.2mo l中间体1、0.1mo l对苯二酚、0.2mo l碳酸钾以及100mLN,N-二甲基甲酰胺加入至安装有搅拌器、温度计以及导气管的三口烧瓶中,通入氮气保护,在温度为150℃,搅拌速率为400r/min的条件下搅拌反应6h,反应结束后将反应产物冷却至室温,之后加入至冰水中,析出沉淀,之后真空抽滤,将滤饼放置于真空干燥箱中,在温度为60℃的条件下干燥3h,得到中间体2;Step A2: 0.2 mol of intermediate 1, 0.1 mol of hydroquinone, 0.2 mol of potassium carbonate and 100 mL of N,N-dimethylformamide were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The reaction was stirred at a temperature of 150° C. and a stirring rate of 400 r/min for 6 hours. After the reaction was completed, the reaction product was cooled to room temperature, then added to ice water to precipitate, and then vacuum filtered. The filter cake was placed in a vacuum drying oven and dried at a temperature of 60° C. for 3 hours to obtain intermediate 2;
步骤A3:将10mmo l中间体2、0.25g5%钯碳以及80mL无水乙醇加入至安装有搅拌器、温度计以及恒压滴液漏斗的三口烧瓶中,在温度为25℃,搅拌速率为400r/min的条件下边搅拌边逐滴加入12mL质量分数为64%的水合肼溶液,控制滴加速率为1滴/s,滴加完毕后升温至70℃的条件下继续搅拌反应5h,反应结束后将反应产物加入至蒸馏水中,析出沉淀,之后真空抽滤,将滤饼放置于真空干燥箱中,在温度为60℃的条件下干燥3h,得到中间体3;Step A3: 10 mmol of intermediate 2, 0.25 g of 5% palladium carbon and 80 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and 12 mL of a 64% hydrazine hydrate solution was added dropwise while stirring at a temperature of 25 ° C and a stirring rate of 400 r/min. The dropping rate was controlled to be 1 drop/s. After the addition was completed, the temperature was raised to 70 ° C and the stirring reaction was continued for 5 hours. After the reaction was completed, the reaction product was added to distilled water to precipitate, and then vacuum filtered. The filter cake was placed in a vacuum drying oven and dried at a temperature of 60 ° C for 3 hours to obtain intermediate 3;
步骤A4:将0.1mo l邻二甲苯、0.1g碘以及0.2g铁粉加入至安装有搅拌器、温度计以及恒压滴液漏斗的三口烧瓶中,在温度为0℃,搅拌速率为400r/min的条件下边搅拌边逐滴加入0.11mo l液溴,控制滴加速率为1滴/s,滴加完毕后升温至25℃的条件下继续搅拌反应8h,反应结束后向反应产物中滴加质量分数为5%的氢氧化钠溶液直至红色褪去,之后真空抽滤,将滤液常压蒸馏,收集温度为214℃的馏分,得到中间体4;Step A4: 0.1 mol o-xylene, 0.1 g iodine and 0.2 g iron powder were added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and 0.11 mol liquid bromine was added dropwise while stirring at a temperature of 0°C and a stirring rate of 400 r/min. The dropping rate was controlled to be 1 drop/s. After the addition was completed, the temperature was raised to 25°C and the stirring reaction was continued for 8 hours. After the reaction was completed, a 5% sodium hydroxide solution was added dropwise to the reaction product until the red color faded, and then vacuum filtered, the filtrate was distilled at atmospheric pressure, and the fraction at a temperature of 214°C was collected to obtain intermediate 4;
步骤A5:将0.2mo l中间体4、0.1mo l二氯二甲基硅烷、0.1mo l钠以及120mL甲苯加入至安装有搅拌器、温度计以及回流冷凝管的三口烧瓶中,在温度为25℃,搅拌速率为400r/min的条件下搅拌反应20min,之后升温至回流的条件下继续搅拌反应1h,反应结束后将反应产物旋转蒸发去除甲苯,之后减压蒸馏,收集压力为0.002MPa,温度为226℃的馏分,得到中间体5;Step A5: 0.2 mol of intermediate 4, 0.1 mol of dichlorodimethylsilane, 0.1 mol of sodium and 120 mL of toluene were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 25° C. and a stirring rate of 400 r/min for 20 min, then the temperature was raised to reflux and the stirring reaction was continued for 1 h. After the reaction was completed, the reaction product was rotary evaporated to remove toluene, and then vacuum distilled to collect the fraction with a pressure of 0.002 MPa and a temperature of 226° C. to obtain intermediate 5;
步骤A6:将10mmo l中间体5、70mL吡啶、25g高锰酸钾以及20mL去离子水加入至安装有搅拌器、温度计以及回流冷凝管的三口烧瓶中,在温度为25℃,搅拌速率为400r/min的条件下搅拌反应20min,之后升温至回流的条件下继续搅拌反应1h,之后加入3mL无水甲醇继续搅拌反应1h,反应结束后将反应产物冷却至室温,之后真空抽滤,将滤液用质量分数为20%的盐酸溶液调节pH为1,析出沉淀,之后真空抽滤,将滤饼加入至25mL乙酸酐中,之后在温度70℃,搅拌速率为400r/min的条件下搅拌反应2h,之后旋转蒸发去除溶解,之后用正己烷重结晶,得到中间体6;Step A6: 10 mmol of intermediate 5, 70 mL of pyridine, 25 g of potassium permanganate and 20 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 25°C and a stirring rate of 400 r/min for 20 min, then heated to reflux and continued to stir for reaction for 1 h, then added 3 mL of anhydrous methanol and continued to stir for reaction for 1 h, after the reaction, the reaction product was cooled to room temperature, then vacuum filtered, the filtrate was adjusted to pH 1 with a 20% hydrochloric acid solution by mass fraction, a precipitate was precipitated, then vacuum filtered, the filter cake was added to 25 mL of acetic anhydride, then stirred for reaction at a temperature of 70°C and a stirring rate of 400 r/min for 2 h, then rotary evaporated to remove the solvent, and then recrystallized with n-hexane to obtain intermediate 6;
步骤A7:将5mmo l中间体3、5mmo l中间体6以及300gN,N-二甲基乙酰胺加入至安装有搅拌器、温度计的三口烧瓶中,在温度为35℃,搅拌速率为400r/min的条件下搅拌反应10h,得到高弹抗拉纤维纺丝液。Step A7: Add 5 mmol of intermediate 3, 5 mmol of intermediate 6 and 300 g of N,N-dimethylacetamide into a three-necked flask equipped with a stirrer and a thermometer, and stir the reaction for 10 hours at a temperature of 35°C and a stirring rate of 400 r/min to obtain a high-elastic tensile fiber spinning solution.
实施例2:Embodiment 2:
本实施例为一种高弹抗拉纤维纺丝液的制备方法,包括以下步骤:This embodiment is a method for preparing a high-elastic tensile-resistant fiber spinning solution, comprising the following steps:
步骤A1:将1g4-正丁基氯苯加入至安装有搅拌器、温度计、恒压滴液漏斗以及回流冷凝管的四口烧瓶中,在温度为0℃,搅拌速率为500r/min的条件下边搅拌边逐滴加入10mL质量分数为98%的浓硫酸、质量分数为67%的浓硝酸以及去离子水按照30g:70g:6g混合而成的混合酸,控制滴加速率为2滴/s,滴加完毕后升温至75℃的条件下继续搅拌反应6h,反应结束后将反应产物加入至冰水中,之后用无水乙醚萃取3次,将有机相用饱和碳酸钠溶液洗涤3次,之后用无水硫酸钠干燥,之后真空抽滤,将滤液旋转蒸发去除溶剂,得到中间体1;Step A1: Add 1 g of 4-n-butylchlorobenzene to a four-necked flask equipped with a stirrer, a thermometer, a constant pressure dropping funnel and a reflux condenser, and add dropwise 10 mL of a mixed acid prepared by mixing 98% concentrated sulfuric acid, 67% concentrated nitric acid and deionized water in a ratio of 30 g: 70 g: 6 g at a temperature of 0° C. and a stirring rate of 500 r/min, with stirring, and the dropping rate is controlled to be 2 drops/s. After the dropwise addition is completed, the temperature is raised to 75° C. and the stirring reaction is continued for 6 hours. After the reaction is completed, the reaction product is added to ice water, and then extracted with anhydrous ether for 3 times. The organic phase is washed with a saturated sodium carbonate solution for 3 times, and then dried with anhydrous sodium sulfate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain intermediate 1;
步骤A2:将0.22mo l中间体1、0.1mo l对苯二酚、0.22mo l碳酸钾以及120mLN,N-二甲基甲酰胺加入至安装有搅拌器、温度计以及导气管的三口烧瓶中,通入氮气保护,在温度为155℃,搅拌速率为500r/min的条件下搅拌反应8h,反应结束后将反应产物冷却至室温,之后加入至冰水中,析出沉淀,之后真空抽滤,将滤饼放置于真空干燥箱中,在温度为70℃的条件下干燥5h,得到中间体2;Step A2: 0.22 mol of intermediate 1, 0.1 mol of hydroquinone, 0.22 mol of potassium carbonate and 120 mL of N,N-dimethylformamide were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The reaction was stirred at a temperature of 155° C. and a stirring rate of 500 r/min for 8 hours. After the reaction was completed, the reaction product was cooled to room temperature, then added to ice water to precipitate, and then vacuum filtered. The filter cake was placed in a vacuum drying oven and dried at a temperature of 70° C. for 5 hours to obtain intermediate 2;
步骤A3:将10mmo l中间体2、0.35g5%钯碳以及100mL无水乙醇加入至安装有搅拌器、温度计以及恒压滴液漏斗的三口烧瓶中,在温度为30℃,搅拌速率为500r/min的条件下边搅拌边逐滴加入15mL质量分数为65%的水合肼溶液,控制滴加速率为2滴/s,滴加完毕后升温至75℃的条件下继续搅拌反应6h,反应结束后将反应产物加入至蒸馏水中,析出沉淀,之后真空抽滤,将滤饼放置于真空干燥箱中,在温度为70℃的条件下干燥5h,得到中间体3;Step A3: 10 mmol of intermediate 2, 0.35 g of 5% palladium carbon and 100 mL of anhydrous ethanol were added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and 15 mL of a 65% hydrazine hydrate solution was added dropwise while stirring at a temperature of 30 ° C and a stirring rate of 500 r/min. The dropping rate was controlled to be 2 drops/s. After the dropwise addition was completed, the temperature was raised to 75 ° C and the stirring reaction was continued for 6 hours. After the reaction was completed, the reaction product was added to distilled water to precipitate, and then vacuum filtered. The filter cake was placed in a vacuum drying oven and dried at a temperature of 70 ° C for 5 hours to obtain intermediate 3;
步骤A4:将0.1mo l邻二甲苯、0.15g碘以及0.25g铁粉加入至安装有搅拌器、温度计以及恒压滴液漏斗的三口烧瓶中,在温度为0-5℃,搅拌速率为500r/min的条件下边搅拌边逐滴加入0.13mo l质量分数为10%的液溴,控制滴加速率为2滴/s,滴加完毕后升温至30℃的条件下继续搅拌反应10h,反应结束后向反应产物中滴加氢氧化钠溶液直至红色褪去,之后真空抽滤,将滤液常压蒸馏,收集温度为215℃的馏分,得到中间体4;Step A4: 0.1 mol o-xylene, 0.15 g iodine and 0.25 g iron powder were added to a three-necked flask equipped with a stirrer, a thermometer and a constant pressure dropping funnel, and 0.13 mol of 10% liquid bromine was added dropwise while stirring at a temperature of 0-5°C and a stirring rate of 500 r/min. The dropping rate was controlled to be 2 drops/s. After the addition was completed, the temperature was raised to 30°C and the stirring reaction was continued for 10 hours. After the reaction was completed, sodium hydroxide solution was added dropwise to the reaction product until the red color faded, and then vacuum filtered, the filtrate was distilled at atmospheric pressure, and the fraction at a temperature of 215°C was collected to obtain intermediate 4;
步骤A5:将0.2mo l中间体4、0.1mo l二氯二甲基硅烷、0.1mo l钠以及150mL甲苯加入至安装有搅拌器、温度计以及回流冷凝管的三口烧瓶中,在温度为30℃,搅拌速率为500r/min的条件下搅拌反应25min,之后升温至回流的条件下继续搅拌反应2h,反应结束后将反应产物旋转蒸发去除甲苯,之后减压蒸馏,收集压力为0.002MPa,温度为229℃的馏分,得到中间体5;Step A5: 0.2 mol of intermediate 4, 0.1 mol of dichlorodimethylsilane, 0.1 mol of sodium and 150 mL of toluene were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 30°C and a stirring rate of 500 r/min for 25 min, then the temperature was raised to reflux and the stirring reaction was continued for 2 h. After the reaction was completed, the reaction product was rotary evaporated to remove toluene, and then vacuum distilled to collect the fraction with a pressure of 0.002 MPa and a temperature of 229°C to obtain intermediate 5;
步骤A6:将10mmo l中间体5、80mL吡啶、30g高锰酸钾以及30mL去离子水加入至安装有搅拌器、温度计以及回流冷凝管的三口烧瓶中,在温度为30℃,搅拌速率为500r/min的条件下搅拌反应25min,之后升温至回流的条件下继续搅拌反应2h,之后加入5mL无水甲醇继续搅拌反应2h,反应结束后将反应产物冷却至室温,之后真空抽滤,将滤液用质量分数为25%的盐酸溶液调节pH为2,析出沉淀,之后真空抽滤,将滤饼加入至30mL乙酸酐中,之后在温度80℃,搅拌速率为500r/min的条件下搅拌反应3h,之后旋转蒸发去除溶解,之后用正己烷重结晶,得到中间体6;Step A6: 10 mmol of intermediate 5, 80 mL of pyridine, 30 g of potassium permanganate and 30 mL of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 30°C and a stirring rate of 500 r/min for 25 min, then heated to reflux and continued to stir for reaction for 2 h, then added 5 mL of anhydrous methanol and continued to stir for reaction for 2 h, and after the reaction, the reaction product was cooled to room temperature, and then vacuum filtered, the filtrate was adjusted to pH 2 with a 25% hydrochloric acid solution, a precipitate was precipitated, and then vacuum filtered, the filter cake was added to 30 mL of acetic anhydride, and then stirred for reaction at a temperature of 80°C and a stirring rate of 500 r/min for 3 h, then rotary evaporated to remove the solvent, and then recrystallized with n-hexane to obtain intermediate 6;
步骤A7:将5mmo l中间体3、5mmo l中间体6以及350gN,N-二甲基乙酰胺加入至安装有搅拌器、温度计的三口烧瓶中,在温度为40℃,搅拌速率为500r/min的条件下搅拌反应15h,得到高弹抗拉纤维纺丝液。Step A7: Add 5 mmol of intermediate 3, 5 mmol of intermediate 6 and 350 g of N,N-dimethylacetamide into a three-necked flask equipped with a stirrer and a thermometer, and stir the reaction for 15 hours at a temperature of 40°C and a stirring rate of 500 r/min to obtain a high-elastic tensile fiber spinning solution.
实施例3:Embodiment 3:
本实施例为一种高弹抗拉面料的制备方法,包括以下步骤:This embodiment is a method for preparing a high-elastic tensile-resistant fabric, comprising the following steps:
步骤一:按照实施例1的方法制备高弹抗拉纤维纺丝液,备用;Step 1: prepare a high-elastic tensile fiber spinning solution according to the method of Example 1 and set aside;
步骤二:将高弹抗拉纤维纺丝液在压力为0.3MPa的条件下,由喷丝板喷入体积分数为40%的乙醇溶液中,得到预成型纤维;Step 2: Spraying the high-elastic tensile fiber spinning solution into a 40% by volume ethanol solution from a spinneret under a pressure of 0.3 MPa to obtain a preformed fiber;
步骤三:将预成型纤维用蒸馏水洗涤3次,之后放置于真空干燥箱中,在温度为60℃的条件下干燥3h,之后放置于管式炉中,之后在温度为200℃的条件下干燥2h,之后升温至280℃的条件下干燥1.5h,之后升温至310℃的条件下干燥1h,得到高弹抗拉纤维;Step 3: The preformed fiber is washed with distilled water for 3 times, then placed in a vacuum drying oven, dried at 60°C for 3 hours, then placed in a tubular furnace, then dried at 200°C for 2 hours, then heated to 280°C for 1.5 hours, then heated to 310°C for 1 hour, to obtain a high elastic tensile fiber;
步骤四:将高弹抗拉纤维进行编制成型,得到该高弹抗拉面料。Step 4: Weaving the high-elastic tensile-resistant fibers into shape to obtain the high-elastic tensile-resistant fabric.
实施例4:Embodiment 4:
本实施例为一种高弹抗拉面料的制备方法,包括以下步骤:This embodiment is a method for preparing a high-elastic tensile-resistant fabric, comprising the following steps:
步骤一:按照实施例2的方法制备高弹抗拉纤维纺丝液,备用;Step 1: prepare a high-elastic tensile fiber spinning solution according to the method of Example 2 and set aside;
步骤二:将高弹抗拉纤维纺丝液在压力为0.4MPa的条件下,由喷丝板喷入体积分数为50%的乙醇溶液中,得到预成型纤维;Step 2: Spraying the high-elastic tensile fiber spinning solution into a 50% by volume ethanol solution from a spinneret under a pressure of 0.4 MPa to obtain a preformed fiber;
步骤三:将预成型纤维用蒸馏水洗涤5次,之后放置于真空干燥箱中,在温度为70℃的条件下干燥5h,之后放置于管式炉中,之后在温度为200℃的条件下干燥2.5h,之后升温至280℃的条件下干燥2h,之后升温至310℃的条件下干燥1.5h,得到高弹抗拉纤维;Step 3: The preformed fiber was washed with distilled water for 5 times, then placed in a vacuum drying oven, dried at 70°C for 5 hours, then placed in a tubular furnace, then dried at 200°C for 2.5 hours, then heated to 280°C for 2 hours, then heated to 310°C for 1.5 hours, to obtain a high elastic tensile fiber;
步骤四:将高弹抗拉纤维进行编制成型,得到该高弹抗拉面料。Step 4: Weaving the high-elastic tensile-resistant fibers into shape to obtain the high-elastic tensile-resistant fabric.
对比例1:Comparative Example 1:
对比例1为申请号为202010752143.3中实施例9的方法制备的弹性面料。Comparative Example 1 is an elastic fabric prepared by the method of Example 9 in Application No. 202010752143.3.
将实施例3-4以及对比例1的高弹抗拉面料的性能进行检测,检测结果如下表所示:The performance of the high elastic tensile fabrics of Examples 3-4 and Comparative Example 1 was tested, and the test results are shown in the following table:
参阅上表数据,根据实施例3-4以及对比例1进行比较,可以得知本发明中的弹性面料不仅拉伸强度高,而且扯断伸长率高,且较对比例1中的弹性面料的性能更佳,表明本发明的弹性面料抗拉性能优良,且具备高弹性。在本说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。Referring to the data in the above table, according to the comparison between Examples 3-4 and Comparative Example 1, it can be known that the elastic fabric of the present invention not only has high tensile strength, but also has high elongation at break, and has better performance than the elastic fabric in Comparative Example 1, indicating that the elastic fabric of the present invention has excellent tensile properties and high elasticity. In the description of this specification, the description of reference terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.
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