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CN117344396A - Preparation method of high-performance flame-retardant artificial viscose fiber - Google Patents

Preparation method of high-performance flame-retardant artificial viscose fiber Download PDF

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Publication number
CN117344396A
CN117344396A CN202311297487.XA CN202311297487A CN117344396A CN 117344396 A CN117344396 A CN 117344396A CN 202311297487 A CN202311297487 A CN 202311297487A CN 117344396 A CN117344396 A CN 117344396A
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viscose fiber
retardant
flame
steps
preparing
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夏铁
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Wuxi Shilead Bleaching And Dyeing Co ltd
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Wuxi Shilead Bleaching And Dyeing Co ltd
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    • 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

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  • Artificial Filaments (AREA)

Abstract

本发明属于粘胶纤维技术领域,公开了高性能阻燃人造粘胶纤维的制备方法,包括下述步骤,S1.选用天然纤维为制造粘胶纤维的原材料;S2.天然纤维浸渍并形成浆粥;S3.制备碱纤维素,降低聚合度;S4.碱纤维素进行黄化反应;S5.溶解;S6.过滤;S7.熟成;S8.加入抗菌剂,所述抗菌剂包括芦荟大黄苷、聚氧化乙烯三甲基氯化铵、醋酸、过硫酸钾、硫酸铜、碳酸氢钠、甲基壬基酮;S9.加入阻燃剂,所述阻燃剂为无卤阻燃剂;S10.脱泡;S11.纺丝。

The invention belongs to the technical field of viscose fiber. It discloses a preparation method of high-performance flame-retardant artificial viscose fiber, which includes the following steps: S1. Select natural fiber as the raw material for manufacturing viscose fiber; S2. Impregnate the natural fiber and form a slurry. ; S3. Prepare alkali cellulose and reduce the degree of polymerization; S4. Carry out yellowing reaction of alkali cellulose; S5. Dissolve; S6. Filter; S7. Mature; S8. Add antibacterial agents, the antibacterial agents include aloe-emodin, poly Ethylene trimethyl ammonium chloride, acetic acid, potassium persulfate, copper sulfate, sodium bicarbonate, methyl nonyl ketone; S9. Add flame retardant, the flame retardant is a halogen-free flame retardant; S10. Remove Bubble; S11. Spinning.

Description

高性能阻燃人造粘胶纤维的制备方法Preparation method of high-performance flame-retardant artificial viscose fiber

技术领域Technical field

本发明属于粘胶纤维技术领域,具体涉及高性能阻燃人造粘胶纤维的制备方法。The invention belongs to the technical field of viscose fibers, and specifically relates to a preparation method of high-performance flame-retardant artificial viscose fibers.

背景技术Background technique

粘胶纤维(Viscose fibre),简称粘纤,又名黏胶丝,人造纤维的一种。粘胶纤维是人造纤维的主要品种,是中国产量第二大的化纤品种,其主要原料是化学浆粕,包括棉浆粕和木浆粕两种,通过化学反应将天然纤维素分离出来再生而成,国内所用原料主要是棉浆粕。粘胶纤维吸湿性好,易于染色,不易起静电,有较好的可纺性能,被广泛应用于各类纺织、服装等领域。如绝大多数纺织纤维一样,粘胶纤维属于易燃物质,LOI值只有18%左右,极易发生火灾,而且,粘胶纤维的抗菌性较差,不能妨碍细菌生长繁殖及其活性。当今,人们的生活质量已经得到空前提高,人们对于干净卫生的追求有较大的需求,另外,人们对于生活及作业安全尤其是对火灾的预防的重视程度也达到了新的高度。Viscose fiber, referred to as viscose fiber, also known as viscose silk, is a type of man-made fiber. Viscose fiber is the main type of man-made fiber and the second largest chemical fiber type in China. Its main raw material is chemical pulp, including cotton pulp and wood pulp. Natural cellulose is separated and regenerated through chemical reactions. The raw materials used domestically are mainly cotton pulp. Viscose fiber has good hygroscopicity, is easy to dye, is not prone to static electricity, and has good spinnability. It is widely used in various textiles, clothing and other fields. Like most textile fibers, viscose fiber is a flammable substance with an LOI value of only about 18%, making it extremely prone to fire. Moreover, viscose fiber has poor antibacterial properties and cannot hinder the growth, reproduction and activity of bacteria. Today, people's quality of life has been unprecedentedly improved, and people have a greater demand for cleanliness and hygiene. In addition, people's emphasis on life and work safety, especially fire prevention, has also reached a new height.

发明内容Contents of the invention

针对上述背景技术所提出的问题,本发明的目的是:旨在提供高性能阻燃人造粘胶纤维的制备方法。In view of the problems raised by the above background technology, the purpose of the present invention is to provide a method for preparing high-performance flame-retardant artificial viscose fibers.

为实现上述技术目的,本发明采用的技术方案如下:In order to achieve the above technical objectives, the technical solutions adopted by the present invention are as follows:

高性能阻燃人造粘胶纤维的制备方法,包括下述步骤,The preparation method of high-performance flame-retardant artificial viscose fiber includes the following steps:

S1.选用天然纤维为制造粘胶纤维的原材料;S1. Use natural fibers as raw materials for making viscose fibers;

S2.天然纤维浸渍并形成浆粥;S2. Natural fibers are impregnated and formed into pulp;

S3.制备碱纤维素,降低聚合度;S3. Prepare alkali cellulose and reduce the degree of polymerization;

S4.碱纤维素进行黄化反应;S4. Alkaline cellulose undergoes yellowing reaction;

S5.溶解;S5. Dissolve;

S6.过滤;S6. Filter;

S7.熟成;S7. Mature;

S8.加入抗菌剂,所述抗菌剂包括芦荟大黄苷、聚氧化乙烯三甲基氯化铵、醋酸、过硫酸钾、硫酸铜、碳酸氢钠、甲基壬基酮;S8. Add antibacterial agents, which include aloe-emodin, polyoxyethylene trimethylammonium chloride, acetic acid, potassium persulfate, copper sulfate, sodium bicarbonate, and methyl nonyl ketone;

S9.加入阻燃剂,所述阻燃剂为无卤阻燃剂;S9. Add a flame retardant, which is a halogen-free flame retardant;

S10.脱泡;S10.Degassing;

S11.纺丝。S11. Spinning.

进一步限定,所述天然纤维为木纤维,这样的设计,因为相较于棉纤维素,木纤维的溶解性好。It is further limited that the natural fiber is wood fiber. This design is because wood fiber has better solubility than cotton cellulose.

进一步限定,所述木纤维为山毛榉纤维,这样的设计,山毛榉的硫酸盐浆粕在老化过程中的讲解速度更快,有利于提高生产速度和质量。It is further limited that the wood fiber is beech fiber. With this design, the beech sulfate pulp decomposes faster during the aging process, which is beneficial to improving the production speed and quality.

进一步限定,所述木纤维通过亚硫酸盐法蒸煮溶解成浆粥,这样的设计,蒸煮过程中,木质素和半纤维素会溶出,而采用亚硫酸盐法蒸煮时,产生的硫酸盐浆粕更少,硫酸盐浆粕的结晶度更低,并且黄化时,不容残渣更少。It is further limited that the wood fiber is dissolved into pulp and porridge through sulfite cooking. With such a design, lignin and hemicellulose will be dissolved during the cooking process, and when sulfite cooking is used, the sulfate pulp produced Less, sulfate pulp is less crystalline and leaves less residue when yellowed.

进一步限定,制备碱纤维素时,浆粥中加入16%~20%氢氧化钠溶剂,这样的设计,采用16%~20%的氢氧化钠溶剂进行碱化作用的效果最好,老化速度最快,有利于提高黄化时二硫化碳的利用率,总的来说溶解性能和黄化性能好。It is further limited that when preparing alkali cellulose, 16% to 20% sodium hydroxide solvent is added to the pulp porridge. In this design, using 16% to 20% sodium hydroxide solvent for alkalization has the best effect and the fastest aging speed. It is fast and helps to improve the utilization rate of carbon disulfide during yellowing. Generally speaking, it has good solubility and yellowing properties.

进一步限定,所述氢氧化钠溶剂为18%,这样的设计,提供最优的氢氧化钠溶剂含量。It is further limited that the sodium hydroxide solvent is 18%. This design provides the optimal sodium hydroxide solvent content.

进一步限定,黄化反应时,所述碱纤维素与二硫化碳进行,这样的设计,通过二硫化碳完成碱纤维素的黄化,改变碱纤维素的结构。It is further limited that during the yellowing reaction, the alkali cellulose is carried out with carbon disulfide. Such a design completes the yellowing of the alkali cellulose through carbon disulfide and changes the structure of the alkali cellulose.

进一步限定,所述阻燃剂包括三氯氧磷、苯酚和双酚A,这样的设计,不包含卤系成分,可以避免卤系阻燃剂受热时分解出HX,HX是一种高腐蚀性和毒性的气体,它的存在给火灾中的被困人群带来了极大的二次伤害。Further qualification, the flame retardant includes phosphorus oxychloride, phenol and bisphenol A. Such a design does not contain halogen components, which can avoid the decomposition of HX when the halogen flame retardant is heated. HX is a highly corrosive and toxic gases, whose presence has brought great secondary harm to the people trapped in the fire.

进一步限定,纺丝时,纤维素在纺丝液中的含量为5%~11%,这样的设计,提高纺丝的质量。It is further limited that during spinning, the content of cellulose in the spinning liquid is 5% to 11%. This design improves the quality of spinning.

进一步限定,纺丝时,抗菌剂与纺丝液的重量比为3~5:100,阻燃剂与纺丝液的重量比为3~10:100,这样的设计,保证抗菌剂、阻燃剂的合适比例,起到良好的抗菌以及阻燃的效果,同时避免影响纺丝后的粘胶纤维的物理性能。Further limit, during spinning, the weight ratio of antibacterial agent to spinning solution is 3 to 5:100, and the weight ratio of flame retardant to spinning solution is 3 to 10:100. This design ensures that the antibacterial agent and flame retardant The appropriate proportion of the agent can achieve good antibacterial and flame retardant effects while avoiding affecting the physical properties of the spun viscose fiber.

本发明的有益效果:抗菌剂能够抑制菌群的生长,妨碍细菌生长繁殖并压制活性,满足用户对于干净卫生的需求,而阻燃剂可以提高粘胶纤维的阻燃性能,提高使用安全性,进一步的,阻燃剂为无卤阻燃剂,不包含卤系成分,可以避免卤系阻燃剂受热时分解出HX,HX是一种高腐蚀性和毒性的气体,防止HX的存在给火灾中的被困人群带来二次伤害。The beneficial effects of the present invention: antibacterial agents can inhibit the growth of bacterial flora, hinder bacterial growth and reproduction and suppress activity, meeting users' needs for cleanliness and hygiene, while flame retardants can improve the flame retardant performance of viscose fibers and improve the safety of use. Furthermore, the flame retardant is a halogen-free flame retardant and does not contain halogen components, which can prevent the halogen flame retardant from decomposing HX when heated. HX is a highly corrosive and toxic gas, preventing the presence of HX from causing fire hazards. causing secondary harm to the trapped people.

附图说明Description of drawings

本发明可以通过附图给出的非限定性实施例进一步说明;The invention can be further illustrated by the non-limiting examples given in the accompanying drawings;

图1为本发明高性能阻燃人造粘胶纤维的制备方法实施例的流程图;Figure 1 is a flow chart of an embodiment of the preparation method of high-performance flame-retardant artificial viscose fiber of the present invention;

具体实施方式Detailed ways

为了使本领域的技术人员可以更好地理解本发明,下面结合附图和实施例对本发明技术方案进一步说明。In order to enable those skilled in the art to better understand the present invention, the technical solution of the present invention is further described below in conjunction with the accompanying drawings and examples.

如图1所示,本发明的高性能阻燃人造粘胶纤维的制备方法,包括下述步骤,As shown in Figure 1, the preparation method of the high-performance flame-retardant artificial viscose fiber of the present invention includes the following steps:

S1.选用天然纤维为制造粘胶纤维的原材料;S1. Use natural fibers as raw materials for making viscose fibers;

S2.天然纤维浸渍并形成浆粥;S2. Natural fibers are impregnated and formed into pulp;

S3.制备碱纤维素,降低聚合度;S3. Prepare alkali cellulose and reduce the degree of polymerization;

S4.碱纤维素进行黄化反应;S4. Alkaline cellulose undergoes yellowing reaction;

S5.溶解;S5. Dissolve;

S6.过滤;S6. Filter;

S7.熟成;S7. Mature;

S8.加入抗菌剂,抗菌剂包括芦荟大黄苷、聚氧化乙烯三甲基氯化铵、醋酸、过硫酸钾、硫酸铜、碳酸氢钠、甲基壬基酮;S8. Add antibacterial agents, which include aloe-emodin, polyoxyethylene trimethylammonium chloride, acetic acid, potassium persulfate, copper sulfate, sodium bicarbonate, and methyl nonyl ketone;

S9.加入阻燃剂,阻燃剂为无卤阻燃剂;S9. Add flame retardant, which is halogen-free flame retardant;

S10.脱泡;S10.Degassing;

S11.纺丝。S11. Spinning.

本实施例中:In this example:

选用天然纤维为制造粘胶纤维的原材料,具体可以选用木纤维,相较于棉纤维素,木纤维的溶解性好,选用山毛榉纤维更加,山毛榉的硫酸盐浆粕在老化过程中的讲解速度更快,有利于提高生产速度和质量,随后,天然纤维浸渍通过亚硫酸盐法蒸煮溶解成浆粥;制备碱纤维素,降低聚合度,制备时,浆粥中加入16%~20%氢氧化钠溶剂,碱纤维素随后添加二硫化碳进行黄化反应,黄化反应之后,依次进行溶解、过滤、熟成并添加抗菌剂和阻燃剂,抗菌剂能够抑制菌群的生长,妨碍细菌生长繁殖并压制活性,满足用户对于干净卫生的需求,而阻燃剂可以提高粘胶纤维的阻燃性能,提高使用安全性,进一步的,阻燃剂为无卤阻燃剂,不包含卤系成分,可以避免卤系阻燃剂受热时分解出HX,HX是一种高腐蚀性和毒性的气体,防止HX的存在给火灾中的被困人群带来二次伤害。Natural fiber is selected as the raw material for making viscose fiber. Specifically, wood fiber can be used. Compared with cotton cellulose, wood fiber has better solubility. It is more convenient to use beech fiber. The beech sulfate pulp decomposes faster during the aging process. Fast, which is beneficial to improving production speed and quality. Subsequently, the natural fiber is impregnated and dissolved into pulp porridge through sulfite method; alkali cellulose is prepared to reduce the degree of polymerization. During preparation, 16% to 20% sodium hydroxide is added to the pulp porridge. Solvent, alkali cellulose and then add carbon disulfide for yellowing reaction. After the yellowing reaction, it is dissolved, filtered, matured, and antibacterial agents and flame retardants are added. Antibacterial agents can inhibit the growth of bacterial flora, hinder bacterial growth and reproduction, and suppress activity. , to meet users’ needs for cleanliness and hygiene, and flame retardants can improve the flame retardant properties of viscose fibers and improve the safety of use. Furthermore, the flame retardants are halogen-free flame retardants, which do not contain halogen components and can avoid halogen When the flame retardant is heated, it decomposes into HX, which is a highly corrosive and toxic gas. This prevents the presence of HX from causing secondary harm to the people trapped in the fire.

优选,天然纤维为木纤维,这样的设计,因为相较于棉纤维素,木纤维的溶解性好。实际上,也可以根据具体情况具体考虑其它的天然纤维。Preferably, the natural fiber is wood fiber. This design is because wood fiber has better solubility than cotton cellulose. In fact, other natural fibers may also be considered on a case-by-case basis.

优选,木纤维为山毛榉纤维,这样的设计,山毛榉的硫酸盐浆粕在老化过程中的讲解速度更快,有利于提高生产速度和质量。实际上,也可以根据具体情况具体考虑其它的木纤维种类。Preferably, the wood fiber is beech fiber. With this design, the beech sulfate pulp decomposes faster during the aging process, which is beneficial to improving production speed and quality. In fact, other wood fiber types can also be considered on a case-by-case basis.

优选,木纤维通过亚硫酸盐法蒸煮溶解成浆粥,这样的设计,蒸煮过程中,木质素和半纤维素会溶出,而采用亚硫酸盐法蒸煮时,产生的硫酸盐浆粕更少,硫酸盐浆粕的结晶度更低,并且黄化时,不容残渣更少。实际上,也可以根据具体情况具体考虑用于溶出木质素和半纤维素的其它的方式。Preferably, wood fiber is dissolved into pulp and porridge through sulfite cooking. With this design, lignin and hemicellulose will be dissolved during the cooking process, and when sulfite cooking is used, less sulfate pulp is produced. Kraft pulp is less crystalline and leaves less residue when yellowed. In fact, other methods for dissolving lignin and hemicellulose may also be considered based on specific circumstances.

优选,制备碱纤维素时,浆粥中加入16%~20%氢氧化钠溶剂,这样的设计,采用16%~20%的氢氧化钠溶剂进行碱化作用的效果最好,老化速度最快,有利于提高黄化时二硫化碳的利用率,总的来说溶解性能和黄化性能好。实际上,也可以根据具体情况具体考虑氢氧化钠溶剂其它的含量。Preferably, when preparing alkali cellulose, 16% to 20% sodium hydroxide solvent is added to the pulp porridge. In this design, using 16% to 20% sodium hydroxide solvent for alkalization has the best effect and the fastest aging speed. , it is helpful to improve the utilization rate of carbon disulfide during yellowing, and generally has good solubility and yellowing properties. In fact, other contents of the sodium hydroxide solvent can also be considered based on specific circumstances.

优选,氢氧化钠溶剂为18%,这样的设计,提供最优的氢氧化钠溶剂含量。实际上,也可以根据具体情况具体考虑其它的氢氧化钠溶剂其它的含量。Preferably, the sodium hydroxide solvent is 18%. This design provides the optimal sodium hydroxide solvent content. In fact, other contents of other sodium hydroxide solvents can also be considered based on specific circumstances.

优选,黄化反应时,碱纤维素与二硫化碳进行,这样的设计,通过二硫化碳完成碱纤维素的黄化,改变碱纤维素的结构。实际上,也可以根据具体情况具体考虑改变碱纤维素结构的其它的方法。Preferably, during the yellowing reaction, alkali cellulose reacts with carbon disulfide. In this design, carbon disulfide completes the yellowing of alkali cellulose and changes the structure of alkali cellulose. In fact, other methods of changing the structure of alkali cellulose can also be considered based on specific circumstances.

优选,阻燃剂包括三氯氧磷、苯酚和双酚A,这样的设计,不包含卤系成分,可以避免卤系阻燃剂受热时分解出HX,HX是一种高腐蚀性和毒性的气体,它的存在给火灾中的被困人群带来了极大的二次伤害。实际上,也可以根据具体情况具体考虑阻燃剂其它的组份。Preferably, the flame retardant includes phosphorus oxychloride, phenol and bisphenol A. This design does not contain halogen components, which can prevent the halogen flame retardant from decomposing HX when heated. HX is a highly corrosive and toxic substance. Gas, its existence brings great secondary harm to the people trapped in the fire. In fact, other components of the flame retardant can also be considered based on specific circumstances.

优选,纺丝时,纤维素在纺丝液中的含量为5%~11%,这样的设计,提高纺丝的质量。实际上,也可以根据具体情况具体考虑纤维素其它的比例。Preferably, during spinning, the content of cellulose in the spinning liquid is 5% to 11%. This design improves the quality of spinning. In fact, other proportions of cellulose can also be considered based on specific circumstances.

优选,纺丝时,抗菌剂与纺丝液的重量比为3~5:100,阻燃剂与纺丝液的重量比为3~10:100,这样的设计,保证抗菌剂、阻燃剂的合适比例,起到良好的抗菌以及阻燃的效果,同时避免影响纺丝后的粘胶纤维的物理性能。实际上,也可以根据具体情况具体考虑抗菌剂、阻燃剂其它的比例。Preferably, during spinning, the weight ratio of antibacterial agent to spinning solution is 3 to 5:100, and the weight ratio of flame retardant to spinning solution is 3 to 10:100. This design ensures that the antibacterial agent and flame retardant The appropriate proportion can achieve good antibacterial and flame retardant effects while avoiding affecting the physical properties of the spun viscose fiber. In fact, other proportions of antibacterial agents and flame retardants can also be considered based on specific circumstances.

上述实施例仅示例性说明本发明的原理及其功效,而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下,对上述实施例进行修饰或改变。因此,凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变,仍应由本发明的权利要求所涵盖。The above embodiments only illustrate the principles and effects of the present invention, but are not intended to limit the present invention. Anyone familiar with this technology can modify or change the above embodiments without departing from the spirit and scope of the invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the technical field without departing from the spirit and technical ideas disclosed in the present invention shall still be covered by the claims of the present invention.

Claims (10)

1. The preparation method of the high-performance flame-retardant artificial viscose fiber is characterized by comprising the following steps of: comprising the steps of,
s1, selecting natural fibers as raw materials for manufacturing viscose fibers;
s2, soaking natural fibers and forming pulp porridge;
s3, preparing alkali cellulose, and reducing the polymerization degree;
s4, performing a yellowing reaction on the alkali cellulose;
s5, dissolving;
s6, filtering;
s7, ripening;
s8, adding an antibacterial agent, wherein the antibacterial agent comprises aloeresin, polyoxyethylene trimethyl ammonium chloride, acetic acid, potassium persulfate, copper sulfate, sodium bicarbonate and methyl nonylketone;
s9, adding a flame retardant, wherein the flame retardant is a halogen-free flame retardant;
s10, defoaming;
s11, spinning.
2. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 1, wherein the method comprises the following steps: the natural fibers are wood fibers.
3. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 2, wherein the method comprises the following steps: the wood fibers are beech fibers.
4. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 3, wherein the method comprises the following steps: the wood fiber is steamed and dissolved into pulp porridge by a sulfite method.
5. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 4, wherein the method comprises the following steps: when preparing alkali cellulose, 16% -20% sodium hydroxide solvent is added into the pulp porridge.
6. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 5, wherein the method comprises the following steps: the sodium hydroxide solvent is 18%.
7. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 6, wherein the method comprises the following steps: and in the yellowing reaction, the alkali cellulose and the carbon disulfide are processed.
8. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 7, wherein the method comprises the following steps: the flame retardant comprises phosphorus oxychloride, phenol and bisphenol A.
9. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 8, wherein the method comprises the following steps: during spinning, the content of cellulose in the spinning solution is 5% -11%.
10. The method for preparing the high-performance flame-retardant artificial viscose fiber according to claim 9, wherein the method comprises the following steps: during spinning, the weight ratio of the antibacterial agent to the spinning solution is 3-5: 100, the weight ratio of the flame retardant to the spinning solution is 3-10: 100.
CN202311297487.XA 2023-10-09 2023-10-09 Preparation method of high-performance flame-retardant artificial viscose fiber Pending CN117344396A (en)

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