CN117431680A - A kind of preparation method of light and breathable fabric - Google Patents

A kind of preparation method of light and breathable fabric Download PDF

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Publication number
CN117431680A
CN117431680A CN202311588079.XA CN202311588079A CN117431680A CN 117431680 A CN117431680 A CN 117431680A CN 202311588079 A CN202311588079 A CN 202311588079A CN 117431680 A CN117431680 A CN 117431680A
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polyester fiber
light
breathable fabric
preparing
chitosan
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陆志坚
刘煊菲
曾美莲
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Chaozhou Sophia Fashion Co ltd
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Chaozhou Sophia Fashion Co ltd
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    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20Woven 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
    • D03D15/283Woven 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
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/07Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88Monocomponent 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
    • D01F6/92Monocomponent 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 polyesters
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20Woven 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
    • D03D15/242Woven 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 inorganic, e.g. basalt
    • D03D15/275Carbon fibres
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/50Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/50Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
    • D03D15/513Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads heat-resistant or fireproof
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00Physical properties
    • D10B2401/13Physical properties anti-allergenic or anti-bacterial

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to the technical field of textiles and discloses a preparation method of a light and thin breathable fabric, which is formed by spinning polyester fibers and coffee carbon fibers through a high count yarn compact spinning process and weaving through a plain weaving process, wherein the polyester fibers are prepared from polyester fiber slices, an organosilicon antibacterial finishing agent, functional chitosan and an antioxidant through a blending-granulating-spinning process, and the effects of the organosilicon antibacterial finishing agent and the functional chitosan are utilized to endow the polyester fibers with good antibacterial effect, and meanwhile, the strength of the polyester fibers can be improved to a certain extent.

Description

一种轻薄透气面料的制备方法A kind of preparation method of light and breathable fabric

技术领域Technical field

本发明涉及纺织品技术领域,具体涉及一种轻薄透气面料的制备方法。The invention relates to the technical field of textiles, and in particular to a method for preparing light and breathable fabrics.

背景技术Background technique

涤纶又称聚酯纤维,是以聚对苯二甲酸乙二醇酯或对苯二甲酸二甲酯和乙二醇为原料,经过酯化或者酯交换和缩聚反应制得的成纤高聚物,具有良好的耐光、耐腐蚀、易快洗干和高弹性等诸多优点,深受市场以及消费者的喜爱,并在纺织品领域占据重要地位。然而,涤纶面料的缺点也较为突出,例如透气性差、抗菌性能不佳等,而服装若无法透气,会造成汗渍难以挥发,不仅会造成极大的不适感,还有可能滋生细菌,造成皮肤瘙痒等问题,这就导致涤纶面料在服装领域中受到严重限制。此外,涤纶作为合成高分子材料,极限氧指数只有20左右,本身属于易燃物,而且涤纶面料燃烧时还会发生熔融和滴落现象,容易导致火势扩大,因此具有潜在的火灾隐患。Polyester, also known as polyester fiber, is a fiber-forming polymer made from polyethylene terephthalate or dimethyl terephthalate and ethylene glycol through esterification or transesterification and polycondensation reaction. , has many advantages such as good light resistance, corrosion resistance, easy to wash and dry, and high elasticity. It is deeply loved by the market and consumers and occupies an important position in the field of textiles. However, polyester fabrics also have prominent shortcomings, such as poor air permeability and poor antibacterial performance. If the clothing is not breathable, sweat stains will be difficult to evaporate, which will not only cause great discomfort, but may also breed bacteria and cause itchy skin. and other problems, which has resulted in polyester fabrics being severely restricted in the field of clothing. In addition, as a synthetic polymer material, polyester has a limiting oxygen index of only about 20, which makes it flammable. Polyester fabrics will also melt and drip when burned, which can easily cause the fire to expand, so it is a potential fire hazard.

目前可采用物理改性和化学改性的方式解决上述技术问题,例如申请号为CN202110900542.4的发明专利,公开了一种改性涤纶纤维及其制备方法和抗菌涤棉面料,通过将纳米银粉末、载体以及聚对苯二甲酸乙二醇酯进行混合,再经造粒和纺丝工艺,制得改性涤纶纤维,利用纳米银优异的抗菌性能,赋予涤纶纤维良好的抗菌效果。因此,本发明通过制备有机硅抗菌整理剂和功能性壳聚糖为添加剂,与涤纶纤维切片混合,制备功能性涤纶纤维,以其为主要原料,可制得抗菌和耐燃性能优异的面料。At present, physical modification and chemical modification can be used to solve the above technical problems. For example, the invention patent application number CN202110900542.4 discloses a modified polyester fiber and its preparation method and antibacterial polyester fabric. By incorporating nanosilver The powder, carrier and polyethylene terephthalate are mixed, and then undergo granulation and spinning processes to produce modified polyester fiber. The excellent antibacterial properties of nanosilver are used to give the polyester fiber a good antibacterial effect. Therefore, the present invention prepares silicone antibacterial finishing agent and functional chitosan as additives, mixes them with polyester fiber slices to prepare functional polyester fiber, and uses it as the main raw material to produce fabrics with excellent antibacterial and flame-resistant properties.

发明内容Contents of the invention

本发明的目的在于提供一种轻薄透气面料的制备方法,解决了涤纶面料易燃烧、透气性差以及抗菌性能不佳的问题。The purpose of the present invention is to provide a method for preparing light and breathable fabrics, which solves the problems of polyester fabrics being easy to burn, having poor air permeability and poor antibacterial performance.

本发明的目的可以通过以下技术方案实现:The object of the present invention can be achieved through the following technical solutions:

一种轻薄透气面料的制备方法,所述轻薄透气面料由质量比为6-7:1的涤纶纤维和咖啡碳纤维组成;所述涤纶纤维包括以下重量份的原料:涤纶纤维切片80-95份、有机硅抗菌整理剂1-3份、功能性壳聚糖2-4.5份、抗氧剂0.5-1份;A method for preparing a light and breathable fabric. The light and breathable fabric is composed of polyester fiber and coffee carbon fiber with a mass ratio of 6-7:1; the polyester fiber includes the following parts by weight of raw materials: 80-95 parts of polyester fiber slices, 1-3 parts of silicone antibacterial finishing agent, 2-4.5 parts of functional chitosan, 0.5-1 part of antioxidant;

所述制备方法包括以下步骤:The preparation method includes the following steps:

第一步:采用高支纱紧密纺工艺,将涤纶纤维和咖啡碳纤维结合,制备成紧密纱线;The first step: using a high-count yarn compact spinning process to combine polyester fiber and coffee carbon fiber to prepare compact yarn;

第二步:使用平纹织造工艺,对紧密纱线进行织造,即可获得轻薄透气面料;Step 2: Use plain weaving technology to weave tight yarns to obtain light and breathable fabrics;

所述有机硅抗菌整理剂是以1,3-二(氯甲基)-1,1,3,3-四甲基二硅氧烷和双端叔胺化合物为原料制得;The silicone antibacterial finishing agent is prepared by using 1,3-bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane and a double-terminated tertiary amine compound as raw materials;

所述功能性壳聚糖是以壳聚糖和阻燃剂DDP为原料制得。The functional chitosan is prepared by using chitosan and flame retardant DDP as raw materials.

进一步优选地,所述涤纶纤维的制备方法为:Further preferably, the preparation method of the polyester fiber is:

步骤(1):将配方量的涤纶纤维切片、有机硅抗菌整理剂、功能性壳聚糖和抗氧剂置于高速混料机中搅拌混合均匀后,倒入挤出机中,控制温度为240-260℃,螺杆转速为120-150rpm,进行挤出造粒,对获得的母粒进行熔融纺丝,控制纺丝温度为280-300℃、纺丝速度为500-1000m/min,牵引倍数为2.7-3.0倍,得到初生涤纶纤维;Step (1): Place the formula amount of polyester fiber slices, silicone antibacterial finishing agent, functional chitosan and antioxidant in a high-speed mixer, stir and mix evenly, then pour into the extruder, and control the temperature to 240-260℃, screw speed is 120-150rpm, perform extrusion granulation, melt and spin the obtained masterbatch, control the spinning temperature to 280-300℃, the spinning speed to 500-1000m/min, and the pulling multiple is 2.7-3.0 times, and virgin polyester fiber is obtained;

步骤(2):对初生涤纶纤维进行牵伸纺丝,经卷绕、成型、集束牵伸和热定型工艺,即可获得涤纶纤维。Step (2): The virgin polyester fiber is drafted and spun. After winding, forming, bundled drafting and heat setting processes, the polyester fiber can be obtained.

进一步优选地,所述有机硅抗菌整理剂的制备方法为:Further preferably, the preparation method of the silicone antibacterial finishing agent is:

向反应器中加入1,3-二(氯甲基)-1,1,3,3-四甲基二硅氧烷和甲苯溶剂,开启搅拌,待形成均匀溶液后,通入氮气,除去空气,开启加热,将温度升高至60-70℃,控制加入速度,将双端叔胺化合物缓慢加入反应器中,加毕,恒温搅拌12-18h后,蒸发出溶剂,分离出产物,即可获得有机硅抗菌整理剂。Add 1,3-bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane and toluene solvent to the reactor, start stirring, and wait until a uniform solution is formed, then add nitrogen and remove the air , turn on heating, raise the temperature to 60-70°C, control the addition speed, slowly add the double-ended tertiary amine compound into the reactor, complete the addition, stir at constant temperature for 12-18 hours, evaporate the solvent, and separate the product. Get Silicone Antimicrobial Finish.

通过采用上述技术方案,1,3-二(氯甲基)-1,1,3,3-四甲基二硅氧烷的结构两端为卤素基团,可在高温条件下与双端叔胺化合物结构两端的叔胺基团发生季铵化反应,通过控制滴加速度,使产物的分子链不断延伸,形成高分子长链有机硅抗菌整理剂,该有机硅抗菌整理剂结构中含有大量季铵盐抗菌官能团和硅氧键,不仅能够表现出极强的抗菌性能,还具有优异的稳定性。By adopting the above technical solution, the structure of 1,3-bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane has halogen groups at both ends, and can be combined with the double-terminated tertiary siloxane under high temperature conditions. The tertiary amine groups at both ends of the amine compound structure undergo a quaternization reaction. By controlling the dropping speed, the molecular chain of the product is continuously extended to form a long-chain polymeric silicone antibacterial finishing agent. The structure of this organosilicon antibacterial finishing agent contains a large amount of quaternary ammonium. The ammonium salt antibacterial functional group and silicon-oxygen bond not only exhibit strong antibacterial properties, but also have excellent stability.

进一步优选地,所述1,3-二(氯甲基)-1,1,3,3-四甲基二硅氧烷和双端叔胺化合物的摩尔比为1:1。Further preferably, the molar ratio of the 1,3-bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane and the double-ended tertiary amine compound is 1:1.

进一步优选地,所述加入速度为1-2mL/min。Further preferably, the addition speed is 1-2 mL/min.

进一步优选地,所述双端叔胺化合物为N,N,N',N'-四甲基-1,3-丙二胺或者N,N,N',N'-四甲基-1,6-己二胺中的任一种。Further preferably, the double-ended tertiary amine compound is N,N,N',N'-tetramethyl-1,3-propanediamine or N,N,N',N'-tetramethyl-1, Any of 6-hexanediamine.

进一步优选地,所述功能性壳聚糖的制备方法为:Further preferably, the preparation method of the functional chitosan is:

步骤A:将阻燃剂DDP和活化剂搅拌混合,加入至二甲基亚砜中,避光搅拌1-3h,获得活性反应液;Step A: Stir and mix the flame retardant DDP and the activator, add it to dimethyl sulfoxide, and stir in the dark for 1-3 hours to obtain an active reaction solution;

步骤B:将壳聚糖与体积分数为1%的醋酸水溶液搅拌混合,搅拌至形成均匀溶液,向溶液中滴加活性反应液,滴加结束后,室温条件下避光搅拌8-12h后,移入透析袋中,在蒸馏水中透析2-3天,每隔4-6h进行换水,之后经冷冻凝固和冷冻干燥处理,即可获得功能性壳聚糖。Step B: Stir chitosan and an acetic acid aqueous solution with a volume fraction of 1% until a uniform solution is formed. Add the active reaction solution dropwise to the solution. After the dropwise addition, stir for 8-12 hours at room temperature in the dark. Move it into a dialysis bag, dialyze in distilled water for 2-3 days, change the water every 4-6 hours, and then undergo freeze-coagulation and freeze-drying to obtain functional chitosan.

通过采用上述技术方案,阻燃剂DDP结构中的羧基经活化剂活化后,可以与壳聚糖结构中的氨基发生缩合反应,并逐渐交联,形成具有交联结构的功能性壳聚糖,交联结构的壳聚糖作为碳源具有更高的成炭度,以其为碳源和气源,以阻燃剂DDP为酸源,可形成膨胀阻燃体系,达到较少的添加量即刻起到良好的阻燃改性效果。By adopting the above technical solution, the carboxyl group in the DDP structure of the flame retardant, after being activated by the activator, can undergo a condensation reaction with the amino group in the chitosan structure and gradually cross-link to form functional chitosan with a cross-linked structure. The cross-linked structure of chitosan has a higher carbonization degree as a carbon source. Using it as a carbon source and a gas source, and using the flame retardant DDP as an acid source, an intumescent flame retardant system can be formed to achieve instant results with a small amount of addition. It has a good flame retardant modification effect.

进一步优选地,步骤A中,所述活化剂为N,N-二环己基碳二亚胺或者1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐中的任一种。Further preferably, in step A, the activator is N,N-dicyclohexylcarbodiimide or 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride. Any kind.

进一步优选地,步骤B中,所述壳聚糖的重均分子量为20-30KDa,脱乙酰度为90%。Further preferably, in step B, the weight average molecular weight of the chitosan is 20-30KDa, and the deacetylation degree is 90%.

进一步优选地,所述抗氧剂为抗氧剂1010、抗氧剂168或者抗氧剂1076中的任一种或两种以上任意比例的混合物。Further preferably, the antioxidant is any one of antioxidant 1010, antioxidant 168 or antioxidant 1076 or a mixture of two or more in any proportion.

本发明的有益效果:Beneficial effects of the present invention:

1)本发明通过使用高分子型有机硅抗菌整理剂与涤纶纤维切片进行混合,利用有机硅抗菌整理剂结构中大量的季铵盐官能团,赋予涤纶纤维良好的抗菌性能,而且由于有机硅抗菌整理剂的稳定性较佳,因此能够长期保持良好的抗菌活性,而且高分子型有机硅抗菌整理剂能够避免小分子抗菌剂易迁移的问题,保持涤纶纤维的长期抗菌效果,使制备的面料具有长效抗菌性能。1) The present invention uses a polymeric silicone antibacterial finishing agent and mixes it with polyester fiber slices, and utilizes a large number of quaternary ammonium salt functional groups in the structure of the silicone antibacterial finishing agent to give the polyester fiber good antibacterial properties. Moreover, due to the silicone antibacterial finishing The agent has good stability, so it can maintain good antibacterial activity for a long time, and the polymeric silicone antibacterial finishing agent can avoid the problem of easy migration of small molecule antibacterial agents, maintain the long-term antibacterial effect of polyester fibers, and make the prepared fabrics have long-term Effective antibacterial properties.

2)本发明通过使用功能性壳聚糖为膨胀阻燃剂,对涤纶纤维进行阻燃改性,在面料发生燃烧时,迅速形成膨胀碳层,同时配合有机硅抗菌整理剂中的硅元素,形成硅沉积的膨胀碳层,该膨胀碳层具有良好的阻热隔氧作用和较高的强度,能够阻止燃烧,而且壳聚糖具有一定的增塑作用,可提高涤纶纤维的强度。2) The present invention uses functional chitosan as an intumescent flame retardant to perform flame retardant modification on the polyester fiber. When the fabric burns, an expanded carbon layer is quickly formed. At the same time, it is combined with the silicon element in the silicone antibacterial finishing agent. A silicon-deposited expanded carbon layer is formed. The expanded carbon layer has good heat and oxygen insulation and high strength, and can prevent burning. Moreover, chitosan has a certain plasticizing effect and can improve the strength of the polyester fiber.

3)本发明将涤纶纤维和咖啡碳纤维组合,制作成紧密纱线,再将其纺织成面料,利用咖啡碳纤维的质轻和具有多孔结构的优点,提高面料的透气率,使制得的面料轻薄透气,舒适感墙。3) The present invention combines polyester fiber and coffee carbon fiber to make a compact yarn, and then weaves it into fabric. It takes advantage of the light weight and porous structure of coffee carbon fiber to improve the air permeability of the fabric and make the fabric light and thin. Breathable, comfortable wall.

当然,实施本发明的任一产品并不一定需要同时达到以上所述的所有优点。Of course, any product implementing the present invention does not necessarily need to achieve all the above-mentioned advantages at the same time.

附图说明Description of the drawings

为了更清楚地说明本发明实施例的技术方案,下面将对实施例描述所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to explain the technical solutions of the embodiments of the present invention more clearly, the drawings needed to describe the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without exerting creative efforts.

图1为本发明实施例和对比例中使用的有机硅抗菌整理剂的红外表征图。Figure 1 is an infrared characterization diagram of the silicone antibacterial finishing agent used in the examples and comparative examples of the present invention.

具体实施方式Detailed ways

下面将结合本发明实施例中的附图,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 technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.

实施例1Example 1

一、有机硅抗菌整理剂的制备1. Preparation of silicone antibacterial finishing agent

向反应器中加入1mol的1,3-二(氯甲基)-1,1,3,3-四甲基二硅氧烷和甲苯溶剂,开启搅拌,待形成均匀溶液后,通入氮气,除去空气,开启加热,将温度升高至70℃,控制加入速度为1mL/min,将1mol的N,N,N',N'-四甲基-1,6-己二胺缓慢加入反应器中,加毕,恒温搅拌16h后,蒸发出溶剂,分离出产物,即可获得有机硅抗菌整理剂。Add 1 mol of 1,3-bis(chloromethyl)-1,1,3,3-tetramethyldisiloxane and toluene solvent into the reactor, start stirring, and wait until a uniform solution is formed, then add nitrogen. Remove the air, turn on heating, raise the temperature to 70°C, control the addition speed to 1mL/min, and slowly add 1 mol of N,N,N',N'-tetramethyl-1,6-hexanediamine to the reactor After the addition is completed, stir at constant temperature for 16 hours, evaporate the solvent, and separate the product to obtain the silicone antibacterial finishing agent.

取适量有机硅抗菌整理剂,与溴化钾混匀压片,进行红外吸收光谱测试,波数范围为4000-500cm-1,测试结果如图1所示,其中2880~2945cm-1处为-CH3/-CH2-伸缩特征吸收峰,1398~1485cm-1处为季铵盐官能团中C-N特征吸收峰;1046cm-1处为Si-O-Si特征吸收峰。Take an appropriate amount of silicone antibacterial finishing agent, mix it with potassium bromide, and press into tablets. Conduct an infrared absorption spectrum test. The wave number range is 4000-500cm -1 . The test results are shown in Figure 1, where 2880-2945cm -1 is -CH. 3 /-CH 2 -Stretching characteristic absorption peak, 1398~1485cm -1 is the CN characteristic absorption peak in the quaternary ammonium salt functional group; 1046cm -1 is the Si-O-Si characteristic absorption peak.

二、功能性壳聚糖的制备2. Preparation of functional chitosan

步骤A:将1.2g阻燃剂DDP和0.5g的1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐搅拌混合,加入至20mL二甲基亚砜中,避光搅拌2h,获得活性反应液;Step A: Stir and mix 1.2g of flame retardant DDP and 0.5g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, and add it to 20mL of dimethyl sulfoxide. Stir in the dark for 2 hours to obtain active reaction solution;

步骤B:将2g重均分子量为20KDa,脱乙酰度为90%的壳聚糖与240mL体积分数为1%的醋酸水溶液搅拌混合,搅拌至形成均匀溶液,向溶液中滴加活性反应液,滴加结束后,室温条件下避光搅拌9h后,移入透析袋中,在蒸馏水中透析3天,每隔6h进行换水,之后经冷冻凝固和冷冻干燥处理,即可获得功能性壳聚糖。Step B: Stir and mix 2g of chitosan with a weight average molecular weight of 20KDa and a deacetylation degree of 90% with 240mL of acetic acid aqueous solution with a volume fraction of 1% until a uniform solution is formed. Add the active reaction solution dropwise to the solution. After the addition is completed, stir for 9 hours at room temperature in the dark, then move to a dialysis bag and dialyze in distilled water for 3 days. Change the water every 6 hours. Afterwards, the functional chitosan can be obtained by freeze-solidification and freeze-drying.

将10mL的浓硝酸和0.5mL浓盐酸溶液混合,形成混合溶液,向混合溶液中加入0.5g功能性壳聚糖样品,加热至80℃,搅拌2h,停止加热,待其自然冷却,倒入容量瓶中定容,移取30mL定溶液,与去离子水混合,煮沸,参考参考国标GB/T 10512-2008,配置喹钼柠酮溶液,将100mL喹钼柠酮溶液倒入冷却后的沸液中,再次加热至微沸后,停止加热,待其自然冷却,过滤分离出固体,干燥至恒重,称重,记为M1(g),同时做空白对照试验,记录干燥后的滤饼重量,记为M2(g),利用公式{[(M1-M2)×0.0145×5]/m}×100%计算磷含量,其中m为样品质量,g;测试得出样品中磷含量为12.31%。Mix 10 mL of concentrated nitric acid and 0.5 mL of concentrated hydrochloric acid solution to form a mixed solution. Add 0.5 g of functional chitosan sample to the mixed solution, heat to 80°C, stir for 2 hours, stop heating, wait for it to cool naturally, and pour into the volume. Set the volume in the bottle, transfer 30 mL of the constant solution, mix with deionized water, and boil. Refer to the national standard GB/T 10512-2008 to prepare the quinolinone solution. Pour 100 mL of the quinolinone solution into the cooled boiling liquid. in, heat it again to a slight boil, stop heating, wait for it to cool naturally, filter to separate the solid, dry to constant weight, weigh, record as M 1 (g), and do a blank control test at the same time, record the filter cake after drying Weight, recorded as M 2 (g), use the formula {[(M 1 -M 2 )×0.0145×5]/m}×100% to calculate the phosphorus content, where m is the sample mass, g; the test results show that the phosphorus in the sample The content is 12.31%.

三、涤纶纤维的制备3. Preparation of polyester fiber

步骤(1):将80份涤纶纤维切片、1份有机硅抗菌整理剂、2份功能性壳聚糖和0.5份抗氧剂1010置于高速混料机中搅拌混合均匀后,倒入挤出机中,控制温度为240℃,螺杆转速为120rpm,进行挤出造粒,对获得的母粒进行熔融纺丝,控制纺丝温度为280℃、纺丝速度为500m/min,牵引倍数为3.0倍,得到初生涤纶纤维;Step (1): Place 80 parts of polyester fiber slices, 1 part of silicone antibacterial finishing agent, 2 parts of functional chitosan and 0.5 part of antioxidant 1010 in a high-speed mixer, stir and mix evenly, then pour and extrusion In the machine, the temperature is controlled to 240°C, the screw speed is 120rpm, extrusion granulation is performed, and the obtained masterbatch is melt-spun. The spinning temperature is controlled to 280°C, the spinning speed is 500m/min, and the pulling multiple is 3.0 times to obtain virgin polyester fiber;

步骤(2):对初生涤纶纤维进行牵伸纺丝,经卷绕、成型、集束牵伸和热定型工艺,即可获得涤纶纤维。Step (2): The virgin polyester fiber is drafted and spun. After winding, forming, bundled drafting and heat setting processes, the polyester fiber can be obtained.

实施例2Example 2

涤纶纤维的制备Preparation of polyester fiber

步骤(1):将90份涤纶纤维切片、2.5份有机硅抗菌整理剂、4份功能性壳聚糖和0.6份抗氧剂1010置于高速混料机中搅拌混合均匀后,倒入挤出机中,控制温度为250℃,螺杆转速为150rpm,进行挤出造粒,对获得的母粒进行熔融纺丝,控制纺丝温度为300℃、纺丝速度为800m/min,牵引倍数为3.0倍,得到初生涤纶纤维;Step (1): Place 90 parts of polyester fiber slices, 2.5 parts of silicone antibacterial finishing agent, 4 parts of functional chitosan and 0.6 parts of antioxidant 1010 in a high-speed mixer, stir and mix evenly, then pour into the extruder In the machine, the temperature is controlled to 250°C, the screw speed is 150rpm, extrusion granulation is performed, and the obtained masterbatch is melt-spun. The spinning temperature is controlled to 300°C, the spinning speed is 800m/min, and the pulling factor is 3.0 times to obtain virgin polyester fiber;

步骤(2):对初生涤纶纤维进行牵伸纺丝,经卷绕、成型、集束牵伸和热定型工艺,即可获得涤纶纤维。Step (2): The virgin polyester fiber is drafted and spun. After winding, forming, bundled drafting and heat setting processes, the polyester fiber can be obtained.

所述有机硅抗菌整理剂和功能性壳聚糖的制备方法见实施例1。The preparation method of the silicone antibacterial finishing agent and functional chitosan is shown in Example 1.

实施例3Example 3

涤纶纤维的制备Preparation of polyester fiber

步骤(1):将95份涤纶纤维切片、3份有机硅抗菌整理剂、4.5份功能性壳聚糖和1份抗氧剂1010置于高速混料机中搅拌混合均匀后,倒入挤出机中,控制温度为260℃,螺杆转速为150rpm,进行挤出造粒,对获得的母粒进行熔融纺丝,控制纺丝温度为300℃、纺丝速度为1000m/min,牵引倍数为3.0倍,得到初生涤纶纤维;Step (1): Place 95 parts of polyester fiber slices, 3 parts of silicone antibacterial finishing agent, 4.5 parts of functional chitosan and 1 part of antioxidant 1010 in a high-speed mixer, stir and mix evenly, then pour into the extruder In the machine, the temperature is controlled to 260°C, the screw speed is 150rpm, extrusion granulation is performed, and the obtained masterbatch is melt-spun. The spinning temperature is controlled to 300°C, the spinning speed is 1000m/min, and the pulling factor is 3.0 times to obtain virgin polyester fiber;

步骤(2):对初生涤纶纤维进行牵伸纺丝,经卷绕、成型、集束牵伸和热定型工艺,即可获得涤纶纤维。Step (2): The virgin polyester fiber is drafted and spun. After winding, forming, bundled drafting and heat setting processes, the polyester fiber can be obtained.

所述有机硅抗菌整理剂和功能性壳聚糖的制备方法见实施例1。The preparation method of the silicone antibacterial finishing agent and functional chitosan is shown in Example 1.

对比例1Comparative example 1

涤纶纤维的制备Preparation of polyester fiber

步骤(1):将90份涤纶纤维切片、4份功能性壳聚糖和0.6份抗氧剂1010置于高速混料机中搅拌混合均匀后,倒入挤出机中,控制温度为250℃,螺杆转速为150rpm,进行挤出造粒,对获得的母粒进行熔融纺丝,控制纺丝温度为300℃、纺丝速度为800m/min,牵引倍数为3.0倍,得到初生涤纶纤维;Step (1): Place 90 parts of polyester fiber slices, 4 parts of functional chitosan and 0.6 parts of antioxidant 1010 in a high-speed mixer, stir and mix evenly, then pour into the extruder, and control the temperature to 250°C , the screw speed is 150rpm, extrusion granulation is performed, and the obtained masterbatch is melt-spun. Control the spinning temperature to 300°C, the spinning speed to 800m/min, and the pulling multiple to 3.0 times to obtain virgin polyester fiber;

步骤(2):对初生涤纶纤维进行牵伸纺丝,经卷绕、成型、集束牵伸和热定型工艺,即可获得涤纶纤维。Step (2): The virgin polyester fiber is drafted and spun. After winding, forming, bundled drafting and heat setting processes, the polyester fiber can be obtained.

所述功能性壳聚糖的制备方法见实施例1。The preparation method of the functional chitosan is shown in Example 1.

对比例2Comparative example 2

涤纶纤维的制备Preparation of polyester fiber

步骤(1):将90份涤纶纤维切片、2.5份有机硅抗菌整理剂、4份壳聚糖和0.6份抗氧剂1010置于高速混料机中搅拌混合均匀后,倒入挤出机中,控制温度为250℃,螺杆转速为150rpm,进行挤出造粒,对获得的母粒进行熔融纺丝,控制纺丝温度为300℃、纺丝速度为800m/min,牵引倍数为3.0倍,得到初生涤纶纤维;Step (1): Place 90 parts of polyester fiber slices, 2.5 parts of silicone antibacterial finishing agent, 4 parts of chitosan and 0.6 parts of antioxidant 1010 in a high-speed mixer, mix evenly, and then pour into the extruder. , control the temperature to 250°C, the screw speed to 150rpm, perform extrusion granulation, and perform melt spinning on the obtained masterbatch. Control the spinning temperature to 300°C, the spinning speed to 800m/min, and the traction multiple to 3.0 times. Obtain virgin polyester fiber;

步骤(2):对初生涤纶纤维进行牵伸纺丝,经卷绕、成型、集束牵伸和热定型工艺,即可获得涤纶纤维。Step (2): The virgin polyester fiber is drafted and spun. After winding, forming, bundled drafting and heat setting processes, the polyester fiber can be obtained.

所述有机硅抗菌整理剂的制备方法见实施例1。The preparation method of the silicone antibacterial finishing agent is shown in Example 1.

对比例3Comparative example 3

涤纶纤维的制备Preparation of polyester fiber

步骤(1):将90份涤纶纤维切片、2.5份有机硅抗菌整理剂和0.6份抗氧剂1010置于高速混料机中搅拌混合均匀后,倒入挤出机中,控制温度为250℃,螺杆转速为150rpm,进行挤出造粒,对获得的母粒进行熔融纺丝,控制纺丝温度为300℃、纺丝速度为800m/min,牵引倍数为3.0倍,得到初生涤纶纤维;Step (1): Place 90 parts of polyester fiber slices, 2.5 parts of silicone antibacterial finishing agent and 0.6 parts of antioxidant 1010 in a high-speed mixer, stir and mix evenly, then pour into the extruder, and control the temperature to 250°C , the screw speed is 150rpm, extrusion granulation is performed, and the obtained masterbatch is melt-spun. Control the spinning temperature to 300°C, the spinning speed to 800m/min, and the pulling multiple to 3.0 times to obtain virgin polyester fiber;

步骤(2):对初生涤纶纤维进行牵伸纺丝,经卷绕、成型、集束牵伸和热定型工艺,即可获得涤纶纤维。Step (2): The virgin polyester fiber is drafted and spun. After winding, forming, bundled drafting and heat setting processes, the polyester fiber can be obtained.

所述有机硅抗菌整理剂的制备方法见实施例1。The preparation method of the silicone antibacterial finishing agent is shown in Example 1.

对比例4Comparative example 4

涤纶纤维的制备Preparation of polyester fiber

步骤(1):将90份涤纶纤维切片和0.6份抗氧剂1010置于高速混料机中搅拌混合均匀后,倒入挤出机中,控制温度为250℃,螺杆转速为150rpm,进行挤出造粒,对获得的母粒进行熔融纺丝,控制纺丝温度为300℃、纺丝速度为800m/min,牵引倍数为3.0倍,得到初生涤纶纤维;Step (1): Place 90 parts of polyester fiber slices and 0.6 parts of antioxidant 1010 in a high-speed mixer, stir and mix evenly, then pour into the extruder, control the temperature to 250°C, and the screw speed to 150rpm, and perform extrusion. After granulation, the obtained masterbatch is melt-spun, and the spinning temperature is controlled to 300°C, the spinning speed is 800m/min, and the pulling multiple is 3.0 times to obtain virgin polyester fiber;

步骤(2):对初生涤纶纤维进行牵伸纺丝,经卷绕、成型、集束牵伸和热定型工艺,即可获得涤纶纤维。Step (2): The virgin polyester fiber is drafted and spun. After winding, forming, bundled drafting and heat setting processes, the polyester fiber can be obtained.

性能检测Performance testing

参考国标GB/T 3923.1-2003,对本发明实施例1-实施例3以及对比例1-对比例4制备的涤纶纤维进行断裂强度测试,测试结果如下表所示:With reference to the national standard GB/T 3923.1-2003, the polyester fibers prepared in Examples 1 to 3 and Comparative Examples 1 to 4 of the present invention were tested for breaking strength. The test results are as shown in the following table:

分析测试结果可知,组分中添加了壳聚糖制备的涤纶纤维断裂强力明显较高。Analyzing the test results shows that the breaking strength of polyester fibers prepared by adding chitosan to the components is significantly higher.

采用本发明实施例1-实施例3和对比例1-对比例4制备的涤纶纤维制备面料,具体方法如下所示:The polyester fibers prepared in Examples 1 to 3 and Comparative Examples 1 to 4 of the present invention are used to prepare fabrics. The specific method is as follows:

第一步:采用高支纱紧密纺工艺,将60g涤纶纤维和10g咖啡碳纤维结合,制备成紧密纱线;The first step: using a high-count yarn compact spinning process, combine 60g polyester fiber and 10g coffee carbon fiber to prepare compact yarn;

第二步:使用平纹织造工艺,对紧密纱线进行织造,即可形成面料;Step 2: Use plain weaving technology to weave tight yarns to form fabric;

对面料进行进行以下性能测试:Conduct the following performance tests on fabrics:

参考国标GB/T 20944.2-2007,将面料剪裁成10cm×10cm的样布,测试面料的抗菌性能,测试菌种选择大肠杆菌;Referring to the national standard GB/T 20944.2-2007, cut the fabric into 10cm×10cm sample cloth, test the antibacterial performance of the fabric, and select E. coli as the test strain;

参考国标GB/T 5453-1997,将面料剪裁成面积为20cm2的试样,测试透气性能;Referring to the national standard GB/T 5453-1997, cut the fabric into a sample with an area of 20cm2 to test the breathability;

参考国标GB/T 5454-1997,测试面料的极限氧指数;Refer to the national standard GB/T 5454-1997 to test the limiting oxygen index of fabrics;

测试结果如下表所示:The test results are shown in the table below:

分析上表的测试结果可知,以本发明实施例1-实施例3制备的涤纶面料与咖啡碳纤维结合制作的面料抗菌、阻燃效果好,透气性佳,而采用对比例1制备的涤纶纤维为主要原料制作的面料抗菌性能和阻燃性能均发生不同程度的下降,推测是由于未添加有机硅抗菌整理剂,涤纶纤维不含季铵盐抗菌官能团和硅元素导致的。对比例2制备的涤纶纤维中添加常规壳聚糖,因此不含有机磷阻燃剂,导致面料的阻燃性能下降明显。对比例3制备的涤纶纤维中未添加壳聚糖,因此面料的阻燃性能进一步下降。对比例4制备的涤纶纤维未添加有机硅抗菌整理剂和有机磷阻燃剂,因此阻燃和抗菌性能表现为最差。Analysis of the test results in the above table shows that the fabric made by combining the polyester fabrics prepared in Examples 1 to 3 of the present invention and coffee carbon fiber has good antibacterial and flame retardant effects and good air permeability, while the polyester fiber prepared in Comparative Example 1 is The antibacterial and flame retardant properties of fabrics made from the main raw materials have declined to varying degrees. It is speculated that this is due to the fact that no silicone antibacterial finishing agent is added and the polyester fiber does not contain quaternary ammonium salt antibacterial functional groups and silicon elements. Conventional chitosan was added to the polyester fiber prepared in Comparative Example 2, so it did not contain organophosphorus flame retardant, resulting in a significant decrease in the flame retardant performance of the fabric. Chitosan was not added to the polyester fiber prepared in Comparative Example 3, so the flame retardant properties of the fabric were further reduced. The polyester fiber prepared in Comparative Example 4 did not add silicone antibacterial finishing agent and organophosphorus flame retardant, so the flame retardant and antibacterial properties were the worst.

在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”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必须针对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一个或多个实施例或示例中以合适的方式结合。此外,在不相互矛盾的情况下,本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。In the description of this specification, reference to the terms "one embodiment," "some embodiments," "an example," "specific examples," or "some examples" or the like means that specific features are described in connection with the embodiment or example. , structures, materials or features are included in at least one embodiment or example of the invention. In this specification, the schematic expressions of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the specific features, structures, materials or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, those skilled in the art may combine and combine different embodiments or examples and features of different embodiments or examples described in this specification unless they are inconsistent with each other.

以上内容仅仅是对本发明的构思所作的举例和说明,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,只要不偏离发明的构思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 only examples and explanations of the concept of the invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or substitute them in similar ways, as long as they do not deviate from the concept of the invention. or beyond the scope defined by the claims, shall belong to the protection scope of the present invention.

Claims (10)

1. The preparation method of the light and thin breathable fabric is characterized in that the light and thin breathable fabric consists of polyester fibers and coffee carbon fibers in a mass ratio of 6-7:1; the polyester fiber comprises the following raw materials in parts by weight: 80-95 parts of polyester fiber slice, 1-3 parts of organic silicon antibacterial finishing agent, 2-4.5 parts of functional chitosan and 0.5-1 part of antioxidant;
the preparation method comprises the following steps:
the first step: adopting a high count yarn compact spinning process to combine polyester fiber and coffee carbon fiber to prepare compact yarn;
and a second step of: weaving the compact yarns by using a plain weaving process to obtain a light and thin breathable fabric;
the organosilicon antibacterial finishing agent is prepared from 1, 3-bis (chloromethyl) -1, 3-tetramethyl disiloxane and double-end tertiary amine compounds serving as raw materials;
the functional chitosan is prepared from chitosan and a flame retardant DDP.
2. The method for preparing the light and thin breathable fabric according to claim 1, wherein the method for preparing the polyester fiber is as follows:
step (1): placing polyester fiber slices, an organosilicon antibacterial finishing agent, functional chitosan and an antioxidant in a formula amount into a high-speed mixer, uniformly stirring and mixing, pouring into an extruder, controlling the temperature to be 240-260 ℃, extruding and granulating at the screw speed of 120-150rpm, performing melt spinning on the obtained master batch, controlling the spinning temperature to be 280-300 ℃, and the spinning speed to be 500-1000m/min, wherein the traction multiple is 2.7-3.0 times, thus obtaining the nascent polyester fiber;
step (2): drawing and spinning the nascent polyester fiber, and obtaining the polyester fiber through winding, forming, bundling and drawing and heat setting processes.
3. The method for preparing the light and thin breathable fabric according to claim 1, wherein the method for preparing the organosilicon antibacterial finishing agent is as follows:
adding 1, 3-bis (chloromethyl) -1, 3-tetramethyl disiloxane and toluene solvent into a reactor, starting stirring, introducing nitrogen after forming a uniform solution, removing air, starting heating, raising the temperature to 60-70 ℃, controlling the adding speed, slowly adding a double-end tertiary amine compound into the reactor, stirring at constant temperature for 12-18h after adding, evaporating the solvent, and separating out a product to obtain the organosilicon antibacterial finishing agent.
4. The method for preparing a light and thin breathable fabric according to claim 3, wherein the molar ratio of the 1, 3-bis (chloromethyl) -1, 3-tetramethyldisiloxane to the double-ended tertiary amine compound is 1:1.
5. The method for preparing the light and thin breathable fabric according to claim 3, wherein the adding speed is 1-2mL/min.
6. The method for producing a light and thin breathable fabric according to claim 3, wherein the double-ended tertiary amine compound is any one of N, N '-tetramethyl-1, 3-propanediamine or N, N' -tetramethyl-1, 6-hexanediamine.
7. The method for preparing the light and thin breathable fabric according to claim 1, wherein the method for preparing the functional chitosan is as follows:
step A: stirring and mixing a flame retardant DDP and an activator, adding the mixture into dimethyl sulfoxide, and stirring the mixture for 1 to 3 hours in a dark place to obtain an active reaction solution;
and (B) step (B): stirring chitosan and acetic acid aqueous solution with volume fraction of 1% to form uniform solution, dropwise adding active reaction solution into the solution, stirring at room temperature for 8-12h under dark condition, transferring into dialysis bag, dialyzing in distilled water for 2-3 days, changing water every 4-6h, and freeze-solidifying and freeze-drying to obtain functional chitosan.
8. The method for preparing a light and thin breathable fabric according to claim 7, wherein in the step a, the activator is any one of N, N-dicyclohexylcarbodiimide or 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride.
9. The method for preparing a light and thin breathable fabric according to claim 7, wherein in the step B, the weight average molecular weight of the chitosan is 20-30KDa, and the deacetylation degree is 90%.
10. The method for preparing the light and thin breathable fabric according to claim 1, wherein the antioxidant is any one or a mixture of more than two of antioxidant 1010, antioxidant 168 and antioxidant 1076 in any proportion.
CN202311588079.XA 2023-11-27 2023-11-27 A kind of preparation method of light and breathable fabric Pending CN117431680A (en)

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