CN108978227A - A kind of phosphorous, nitrogen, the flame-retardant system of silicon and its flame-proof cotton fabric of preparation - Google Patents

A kind of phosphorous, nitrogen, the flame-retardant system of silicon and its flame-proof cotton fabric of preparation Download PDF

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CN108978227A
CN108978227A CN201810927184.4A CN201810927184A CN108978227A CN 108978227 A CN108978227 A CN 108978227A CN 201810927184 A CN201810927184 A CN 201810927184A CN 108978227 A CN108978227 A CN 108978227A
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cotton fabric
flame
sol
solution
pei
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任学宏
李杉杉
丁放
林兴焕
栗志广
刘颖
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Jiangnan University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/59Polyamides; Polyimides
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/61Polyamines polyimines
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

本发明公开了一种含磷、氮、硅的阻燃体系,该阻燃体系由聚阳离子溶胶、阴离子溶液组成;所述聚阳离子溶胶的制备方法为:将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2,继续磁力搅拌均匀,采用CH3COOH调节体系的pH,配制成聚阳离子溶胶;所述阴离子溶液的制备方法为:将PA溶于去离子水中,并用氢氧化钠溶液调节其pH,制成阴离子溶液,将棉织物浸于上述阻燃体系中,可层层组装成阻燃棉织物。本发明含磷、氮、硅的阻燃体系在阻燃效果上具有一定的协同作用,具有较好的阻燃效果。

The invention discloses a flame retardant system containing phosphorus, nitrogen and silicon. The flame retardant system is composed of polycation sol and anion solution; the preparation method of the polycation sol is: dissolving PEI in deionized water, Stir to make a PEI solution, then add nano-SiO 2 to the PEI solution, continue magnetic stirring evenly, use CH 3 COOH to adjust the pH of the system, and prepare a polycation sol; the preparation method of the anion solution is: dissolve PA in Ionized water, and adjust its pH with sodium hydroxide solution to make anion solution, soak the cotton fabric in the above flame retardant system, and assemble it into flame retardant cotton fabric layer by layer. The flame retardant system containing phosphorus, nitrogen and silicon of the present invention has a certain synergistic effect on the flame retardant effect, and has better flame retardant effect.

Description

一种含磷、氮、硅的阻燃体系及其制备的阻燃棉织物A flame retardant system containing phosphorus, nitrogen and silicon and the flame retardant cotton fabric prepared therefrom

技术领域technical field

本发明涉及棉织物阻燃技术领域,尤其是涉及一种通过层层自组装在棉织物表面构建含磷、氮、硅阻燃涂层的方法。The invention relates to the technical field of flame-retardant cotton fabrics, in particular to a method for constructing a flame-retardant coating containing phosphorus, nitrogen and silicon on the surface of cotton fabrics through layer-by-layer self-assembly.

背景技术Background technique

棉织物不仅具有优良的吸湿透气性,染色性和生物相容性,而且手感柔软,因此棉织物倍广泛用于装饰行业和纺织行业。但是棉纤维的极限氧指数(LOI)只有18%,容易燃烧而引起火灾,危害人类的生命财产安全。据统计表明,在家庭里由纺织品或家具引的火灾造成人员死亡率比其他原因引起的火灾人员死亡率高。为了阻止火灾发生,除采取防火措施外,还可使用具有阻燃性能的纺织品,以延缓火灾的扩大,使人们有时间撤离或采取措施进行灭火。为此,纺织品燃烧性技术法规逐渐成为各国技术性贸易壁垒的一个重要组成部分。Cotton fabric not only has excellent moisture absorption, breathability, dyeability and biocompatibility, but also has a soft hand, so cotton fabric is widely used in decoration industry and textile industry. However, the limiting oxygen index (LOI) of cotton fiber is only 18%, which is easy to burn and cause fire, endangering the safety of human life and property. According to statistics, the death rate caused by fires caused by textiles or furniture in the home is higher than that caused by fires caused by other causes. In order to prevent fires from happening, in addition to fire prevention measures, textiles with flame retardant properties can also be used to delay the expansion of fires, allowing people to have time to evacuate or take measures to extinguish the fire. For this reason, textile flammability technical regulations have gradually become an important part of technical barriers to trade in various countries.

纺织品经过阻燃处理后,能不同程度地降低可燃性,在燃烧过程中可显著延缓其燃烧效率,并在离开火源后能迅速自熄,从而不易燃烧。棉织物的易燃性在很大程度上限制的棉织物的应用。因此,棉织物的阻燃整理极为重要。传统的棉用阻燃剂是含卤阻燃剂,但由于其在燃烧的过程中会产生有毒的气体而逐渐被磷系阻燃剂所取代。但是含磷阻燃剂在单独使用时,很难达到需要的阻燃效果。磷-氮-硅阻燃体系不含卤素,燃烧过程中不产生有毒气体和烟雾,与物质的相容性好,不容易迁移,且在燃烧的过程中能够发挥协同阻燃的效果。织物的整理多以传统的轧烘焙工艺为主,然而这种工艺也具有一定的局限性和缺点,例如,在焙烘过程中,由于温度过高,对设备有一定的要求,并且高温也会导致织物强力的降低。近年来,新型的加工技术,电子束辐射技术、层层自组装技术在纺织品的改性加工中得到了越来越多的应用。相对于轧烘焙工艺,层层自组装技术具有制备简单、厚度可控、可以组合控制不同的生物分子等优点。After flame-retardant treatment, textiles can reduce their flammability to varying degrees, significantly delay their combustion efficiency during the combustion process, and quickly self-extinguish after leaving the fire source, so they are not easy to burn. The flammability of cotton fabrics largely limits the application of cotton fabrics. Therefore, the flame retardant finishing of cotton fabrics is extremely important. Traditional cotton flame retardants are halogen-containing flame retardants, but they are gradually replaced by phosphorus-based flame retardants because they produce toxic gases during combustion. However, when phosphorus-containing flame retardants are used alone, it is difficult to achieve the desired flame retardant effect. The phosphorus-nitrogen-silicon flame retardant system does not contain halogen, does not produce toxic gas and smoke during combustion, has good compatibility with substances, is not easy to migrate, and can exert a synergistic flame retardant effect during combustion. The finishing of fabrics is mainly based on the traditional padding and baking process. However, this process also has certain limitations and disadvantages. For example, in the baking process, due to the high resulting in a decrease in fabric strength. In recent years, new processing technologies, such as electron beam radiation technology and layer-by-layer self-assembly technology, have been applied more and more in the modification and processing of textiles. Compared with the rolling and baking process, the layer-by-layer self-assembly technology has the advantages of simple preparation, controllable thickness, and the ability to combine and control different biomolecules.

发明内容Contents of the invention

针对现有技术存在的上述问题,本发明申请人提供了一种含磷、氮、硅的阻燃体系及其制备的阻燃棉织物。本发明含磷、氮、硅的阻燃体系在阻燃效果上具有一定的协同作用,反应条件温和,工艺简单,操作方便,绿色无污染。In view of the above-mentioned problems in the prior art, the applicant of the present invention provides a flame-retardant system containing phosphorus, nitrogen, and silicon and the flame-retardant cotton fabric prepared therefrom. The flame retardant system containing phosphorus, nitrogen and silicon of the invention has a certain synergistic effect on the flame retardant effect, mild reaction conditions, simple process, convenient operation, green and pollution-free.

本发明的技术方案如下:Technical scheme of the present invention is as follows:

一种含磷、氮、硅的阻燃体系,所述阻燃体系由聚阳离子溶胶、阴离子溶液组成;A flame retardant system containing phosphorus, nitrogen and silicon, the flame retardant system is composed of polycation sol and anion solution;

所述聚阳离子溶胶的制备方法为:将PEI(聚醚酰亚胺树脂)溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2,继续磁力搅拌均匀,采用CH3COOH调节体系的pH,配制成聚阳离子溶胶;The preparation method of the polycation sol is as follows: PEI (polyetherimide resin) is dissolved in deionized water, and the PEI solution is made by magnetic stirring, then nano - SiO is added to the PEI solution, and the magnetic stirring is continued to be uniform. CH 3 COOH adjusts the pH of the system and prepares polycation sol;

所述阴离子溶液的制备方法为:将PA(植酸)溶于去离子水中,并用氢氧化钠溶液调节其pH,制成阴离子溶液。The preparation method of the anion solution is as follows: dissolving PA (phytic acid) in deionized water, and adjusting its pH with sodium hydroxide solution to prepare the anion solution.

所述聚阳离子溶胶中SiO2与PEI的质量比为1:2~10。The mass ratio of SiO 2 to PEI in the polycation sol is 1:2-10.

所述聚阳离子溶胶的pH为5。The pH of the polycation sol is 5.

所述阴离子溶液中PA的质量浓度为0.5~2wt%;所述阴离子溶液的pH为4~9。The mass concentration of PA in the anion solution is 0.5-2 wt %; the pH of the anion solution is 4-9.

所述氢氧化钠溶液的浓度为4mol/L。The concentration of the sodium hydroxide solution is 4mol/L.

一种含有所述阻燃体系的阻燃棉织物,所述阻燃棉织物的制备方法为:A flame-retardant cotton fabric containing the flame-retardant system, the preparation method of the flame-retardant cotton fabric is:

(1)配制1wt%的SiO2-PEI聚阳离子溶胶,SiO2与PEI的质量比为1:2~10,用醋酸溶液调节pH为5;(1) Prepare 1wt% SiO 2 -PEI polycation sol, the mass ratio of SiO 2 to PEI is 1:2-10, adjust the pH to 5 with acetic acid solution;

(2)配制0.5~2wt%的PA溶液,用4mol/L的氢氧化钠溶液调节pH为4~9;(2) prepare the PA solution of 0.5~2wt%, adjust pH with the sodium hydroxide solution of 4mol/L to be 4~9;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到2~7层。(7) Repeat the above steps (5) and (6) until the number of assembled layers reaches 2-7 layers.

本发明有益的技术效果在于:The beneficial technical effects of the present invention are:

本发明采用的亲水型纳米二氧化硅尺寸小,比表面积大,表面带有负电荷,聚乙烯亚胺(PEI)是一种水溶性高分子聚合物,无色或淡黄色黏稠状液体,聚乙烯亚胺大分子链上有反应性很强的伯胺和仲胺,在水中以聚合阳离子存在,可以中和和吸附所有阴离子物质,还能螯化重金属离子;当纳米二氧化硅与PEI大分子混合时,纳米二氧化碳表面会吸附带有正电荷的PEI大分子,形成稳定的溶胶,由于二氧化硅的比表面积大,易于吸附在基材表面,故当织物浸渍到聚阳离子溶胶中时,可以增加聚阳离子组份在织物表面的吸附量,提高组装的效率。The hydrophilic nano-silica used in the present invention is small in size, large in specific surface area, and has a negative charge on the surface. Polyethyleneimine (PEI) is a water-soluble polymer, a colorless or light yellow viscous liquid, There are highly reactive primary and secondary amines on the macromolecular chain of polyethyleneimine, which exist as polymerized cations in water, which can neutralize and adsorb all anionic substances, and can also chelate heavy metal ions; when nano-silica and PEI When the macromolecules are mixed, the surface of the nano-carbon dioxide will adsorb the positively charged PEI macromolecules to form a stable sol. Due to the large specific surface area of silica, it is easy to adsorb on the surface of the substrate, so when the fabric is immersed in the polycation sol , can increase the adsorption amount of the polycation component on the surface of the fabric, and improve the efficiency of assembly.

本发明采用的植酸(PA)是一种天然食品,无毒,安全性高,含磷量高(28%),可作为一种绿色的阻燃剂。The phytic acid (PA) used in the invention is a natural food, non-toxic, high in safety, high in phosphorus content (28%), and can be used as a green flame retardant.

本发明采用SiO2-PEI与PA通过层层自组装整理到棉织物上,在棉织物表面表面构建含磷、氮、硅的阻燃涂层,制备了阻燃棉织物。当整理的棉织物燃烧时,织物表面的整理剂会先于棉织物分解,发挥阻燃作用。与以往的组装体系相比,该体系的主要优点在于组装效率高(当组装层数达到7层时,增重率可达到27.7%)、交叉污染少、阻燃效率高(LOI可达33.7%)。同时,由于在组装的过程中聚阴阳离子会在织物表面反应形成致密的薄膜使得棉织物的空隙减少,透光率降低,UPF值升高。故自组装整理后的棉织物既具有优异的阻燃性能又具有一定的抗紫外性能。The invention uses SiO 2 -PEI and PA to self-assemble layer by layer on the cotton fabric, constructs a flame-retardant coating containing phosphorus, nitrogen and silicon on the surface of the cotton fabric, and prepares the flame-retardant cotton fabric. When the finished cotton fabric is burned, the finishing agent on the surface of the fabric will decompose before the cotton fabric and play a flame-retardant role. Compared with the previous assembly system, the main advantages of this system are high assembly efficiency (when the number of assembly layers reaches 7 layers, the weight gain rate can reach 27.7%), less cross-contamination, and high flame retardant efficiency (LOI can reach 33.7% ). At the same time, since the polyanions and cations will react on the surface of the fabric to form a dense film during the assembly process, the voids of the cotton fabric will be reduced, the light transmittance will be reduced, and the UPF value will be increased. Therefore, the self-assembled cotton fabric has both excellent flame retardancy and certain UV resistance.

附图说明Description of drawings

图1为实施例1、2、3中制备的阻燃棉织物的垂直燃烧图。Fig. 1 is the vertical combustion diagram of the flame-retardant cotton fabric prepared in embodiment 1, 2, 3.

图2为实施例2、4、5中制备的阻燃棉织物的垂直燃烧图。Fig. 2 is the vertical combustion figure of the flame-retardant cotton fabric prepared in embodiment 2, 4, 5.

图3为实施例6、7、8中制备的阻燃棉织物的垂直燃烧图。Fig. 3 is the vertical combustion figure of the flame-retardant cotton fabric prepared in embodiment 6, 7, 8.

图4为实施例8、9、10中制备的阻燃棉织物的垂直燃烧图。Fig. 4 is the vertical burning graph of the flame-retardant cotton fabric prepared in embodiment 8, 9, 10.

具体实施方式Detailed ways

下面结合附图和实施例,对本发明进行具体描述。The present invention will be specifically described below in conjunction with the accompanying drawings and embodiments.

实施例1Example 1

一种含有所述阻燃体系的阻燃棉织物,所述阻燃棉织物的制备方法为:A flame-retardant cotton fabric containing the flame-retardant system, the preparation method of the flame-retardant cotton fabric is:

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:2),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:2) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为4,制成2wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 4 with 4mol/L sodium hydroxide solution to make a 2wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到7层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 7 layers.

实施例2Example 2

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:6),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:6) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为4,制成2wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 4 with 4mol/L sodium hydroxide solution to make a 2wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到7层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 7 layers.

实施例3Example 3

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:10),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:10) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为4,制成2wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 4 with 4mol/L sodium hydroxide solution to make a 2wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到7层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 7 layers.

实施例4Example 4

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:6),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:6) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为7,制成2wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 7 with 4mol/L sodium hydroxide solution to make a 2wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到7层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 7 layers.

实施例5Example 5

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:6),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:6) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为9,制成2wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 9 with 4mol/L sodium hydroxide solution to make a 2wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到7层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 7 layers.

实施例6Example 6

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:6),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:6) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为6,制成0.5wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 6 with 4mol/L sodium hydroxide solution to make a 0.5wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到7层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 7 layers.

实施例7Example 7

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:6),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:6) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为6,制成1wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 6 with 4mol/L sodium hydroxide solution to make a 1wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到7层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 7 layers.

实施例8Example 8

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:6),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:6) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为6,制成2wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 6 with 4mol/L sodium hydroxide solution to make a 2wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Immerse the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到7层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 7 layers.

实施例9Example 9

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:6),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:6) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为6,制成2wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 6 with 4mol/L sodium hydroxide solution to make a 2wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Soak the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;制得自组装层数为2层的阻燃棉织物。(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in sol with deionized water for 3 times, and then place it in an oven at 45°C. Drying; the flame-retardant cotton fabric with 2 self-assembled layers was obtained.

实施例10Example 10

(1)将PEI溶解在去离子水中,在磁力搅拌制成PEI溶液,之后向PEI溶液中加入纳米SiO2(SiO2:PEI质量比为1:6),继续磁力搅拌均匀,采用CH3COOH调节体系的pH为5,配制成1wt%的SiO2-PEI聚阳离子溶胶;(1) Dissolve PEI in deionized water, stir magnetically to make PEI solution, then add nano-SiO 2 (SiO 2 : PEI mass ratio is 1:6) to PEI solution, continue magnetic stirring evenly, use CH 3 COOH Adjust the pH of the system to 5, and prepare 1wt% SiO 2 -PEI polycation sol;

(2)将PA溶于去离子水中,并用4mol/L氢氧化钠溶液调节其pH为6,制成2wt%的PA溶液;(2) PA is dissolved in deionized water, and its pH is adjusted to 6 with 4mol/L sodium hydroxide solution to make a 2wt% PA solution;

(3)将煮练过的棉织物浸渍到步骤(1)中制备的溶胶中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(3) Soak the scoured cotton fabric into the sol prepared in step (1). After 10 minutes, rinse the cotton fabric soaked in the sol three times with deionized water, and then dry it in an oven at 45°C. ;

(4)将步骤(3)中制备的棉织物浸渍在步骤(2)制备的溶液中,10min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干,完成第一层的组装循环;(4) Soak the cotton fabric prepared in step (3) in the solution prepared in step (2). After 10 minutes, rinse the cotton fabric soaked in the sol with deionized water for 3 times, and then place it in an oven at 45 ° C. Dry to complete the assembly cycle of the first layer;

(5)将步骤(4)中制备的棉织物浸渍到步骤(1)中制备的溶胶中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(5) Immerse the cotton fabric prepared in step (4) into the sol prepared in step (1). After 1 min, rinse the cotton fabric soaked in the sol three times with deionized water, and then place it in an oven at 45°C. medium drying;

(6)将步骤(5)中制备的棉织物浸渍在步骤(2)制备的溶液中,1min后,将浸渍过溶胶的棉织物用去离子水漂洗3次,然后放在45℃的烘箱中烘干;(6) Soak the cotton fabric prepared in step (5) in the solution prepared in step (2). After 1 min, rinse the cotton fabric soaked in sol with deionized water for 3 times, and then place it in an oven at 45°C. drying;

(7)重复上述步骤(5)、(6)的操作,直到组装层数达到4层。(7) Repeat steps (5) and (6) above until the number of assembled layers reaches 4 layers.

测试例1test case 1

将实施案例1~10制备得到的整理棉织物及原棉织物按照GB/T 5455-1997《纺织品燃烧性能测试垂直法》,在YG815型垂直法织物燃烧性能测试仪上对织物进行垂直燃烧测试,测试的标准样品大小为300×80mm。垂直燃烧后织物的图像如图1、2、3、4所示。由图1可以直观的看出,随着Si2O与PEI质量比的增加,阻燃整理的棉织的炭长先减小后有所增加。图2直观的展示出了在弱酸性条件组装整理的棉织物的阻燃效果明显较在弱碱性条件下的阻燃棉织物。由图3可以直观的看出,随着PA溶液浓度的增加,阻燃整理棉织物的阻燃效果逐渐增加。由图4可知,随着组装层数的增加织物垂直燃烧的损毁长度逐渐减小,阻燃性能逐渐变好。According to GB/T 5455-1997 "Vertical Method for Testing the Flammability of Textiles", the finished cotton fabrics and raw cotton fabrics prepared in Cases 1 to 10 were tested for vertical combustion on the YG815 Vertical Fabric Flammability Tester. The standard sample size is 300×80mm. The images of the fabric after vertical burning are shown in Figures 1, 2, 3, and 4. It can be seen intuitively from Figure 1 that as the mass ratio of Si 2 O to PEI increases, the char length of the flame-retardant finished cotton fabric first decreases and then increases. Figure 2 intuitively shows that the flame-retardant effect of the cotton fabric assembled and finished under weakly acidic conditions is significantly higher than that of the flame-retardant cotton fabric under weakly alkaline conditions. It can be seen intuitively from Figure 3 that with the increase of the concentration of the PA solution, the flame retardant effect of the flame retardant finished cotton fabric gradually increases. It can be seen from Figure 4 that with the increase of the number of assembled layers, the damage length of the vertical burning of the fabric gradually decreases, and the flame retardancy performance gradually improves.

表1Table 1

测试例2test case 2

按照GB/T 5454-1997《纺织品燃烧性能测试氧指数法》,将实施案例9、10、8制备得到的整理棉织物及原棉织物至少裁剪成5块,样品规格约为25×6cm2,在氧氮混合气流中,用百分含量来表示维持其燃烧所需的最低氧浓度值。结果见表2所示,由表2可以看出随着组装层数的增加,阻燃整理棉织物的LOI值由原棉的18.2%增加到33.7%。According to GB/T 5454-1997 "Oxygen Index Method for Testing the Combustion Performance of Textiles", the finished cotton fabrics and raw cotton fabrics prepared in Cases 9, 10, and 8 were cut into at least 5 pieces, and the sample size was about 25×6cm 2 . In the oxygen-nitrogen mixed flow, the percentage content is used to express the minimum oxygen concentration value required to maintain its combustion. The results are shown in Table 2. It can be seen from Table 2 that as the number of assembled layers increases, the LOI value of the flame-retardant finished cotton fabric increases from 18.2% to 33.7% of the raw cotton.

表2Table 2

实施例Example 原棉raw cotton 99 1010 88 LOI/%LOI/% 18.218.2 26.026.0 29.129.1 33.733.7

测试例3Test case 3

采用紫外防护因子(UPF)来评价实施案例9、10、8制备得到的整理棉织物及原棉织物的抗紫外性能。测试结果见表3。根据澳大利亚/新西兰标准AS/NZS4399:1996的测试方法对织物样品进行测试,实验仪器为美国VARIAN技术有限公司的Cary50纺织品紫外防护因子测试仪。结果如表3所示,由表3可以看出随着组装层数的增加,阻燃棉织物的UPF值由原棉的6.76增加到35.78,表明经自组装整理后的棉织物既具有较好的阻燃性同时具有良好的抗紫外性能。The UV protection factor (UPF) was used to evaluate the UV resistance of the finished cotton fabrics and raw cotton fabrics prepared in Examples 9, 10, and 8. The test results are shown in Table 3. The fabric samples were tested according to the test method of Australia/New Zealand Standard AS/NZS4399:1996, and the experimental instrument was the Cary50 textile UV protection factor tester of American VARIAN Technology Co., Ltd. The results are shown in Table 3. It can be seen from Table 3 that with the increase of the number of assembled layers, the UPF value of the flame-retardant cotton fabric increases from 6.76 to 35.78 of the raw cotton, indicating that the cotton fabric after self-assembly finishing has better Flame retardant and good UV resistance.

表3table 3

实施例Example 原棉raw cotton 99 1010 88 UPFUPF 6.766.76 15.3615.36 23.6723.67 35.7835.78

Claims (6)

1. the flame-retardant system of a kind of phosphorous, nitrogen, silicon, which is characterized in that the flame-retardant system is molten by polycation colloidal sol, anion Liquid composition;
The polycation colloidal sol the preparation method comprises the following steps: by PEI dissolution in deionized water, PEI solution is made in magnetic agitation, Backward PEI solution in Nano-meter SiO_2 is added2, continuation magnetic agitation is uniform, using CH3The pH of COOH regulation system is configured to gather Cationic sol;
The anion solutions the preparation method comprises the following steps: PA is dissolved in deionized water, and adjust its pH with sodium hydroxide solution, make At anion solutions.
2. flame-retardant system according to claim 1, which is characterized in that SiO in the polycation colloidal sol2With the quality of PEI Than for 1:2~10.
3. flame-retardant system according to claim 1, which is characterized in that the pH of the polycation colloidal sol is 5.
4. flame-retardant system according to claim 1, which is characterized in that the mass concentration of PA is in the anion solutions 0.5~2wt%;The pH of the anion solutions is 4~9.
5. flame-retardant system according to claim 1, which is characterized in that the concentration of the sodium hydroxide solution is 4mol/L.
6. a kind of flame-proof cotton fabric containing flame-retardant system described in claim 1, which is characterized in that the system of the flame-proof cotton fabric Preparation Method are as follows:
(1) SiO of 1wt% is prepared2- PEI polycation colloidal sol, SiO2Mass ratio with PEI is 1:2~10, with acetum tune Saving pH is 5;
(2) the PA solution for preparing 0.5~2wt%, adjusting pH with the sodium hydroxide solution of 4mol/L is 4~9;
(3) cotton fabric of kiering is impregnated into the colloidal sol prepared in step (1), after 10min, the cotton for impregnating colloidal sol is knitted Object is rinsed 3 times with deionized water, is then placed in 45 DEG C of baking oven and is dried;
(4) cotton fabric prepared in step (3) is immersed in the solution of step (2) preparation, after 10min, colloidal sol will be impregnated Cotton fabric with deionized water rinse 3 times, be then placed in 45 DEG C of baking oven and dry, complete first layer assembling circulation;
(5) cotton fabric prepared in step (4) is impregnated into the colloidal sol prepared in step (1), after 1min, colloidal sol will be impregnated Cotton fabric with deionized water rinse 3 times, be then placed in 45 DEG C of baking oven and dry;
(6) cotton fabric prepared in step (5) is immersed in the solution of step (2) preparation, after 1min, colloidal sol will be impregnated Cotton fabric is rinsed 3 times with deionized water, is then placed in 45 DEG C of baking oven and is dried;
(7) repeat the above steps the operations of (5), (6), until the assembling number of plies reaches 2~7 layers.
CN201810927184.4A 2018-08-15 2018-08-15 A kind of phosphorous, nitrogen, the flame-retardant system of silicon and its flame-proof cotton fabric of preparation Pending CN108978227A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113186727A (en) * 2021-05-08 2021-07-30 兰州大学 Inorganic-bio-based anti-photoaging flame retardant and application thereof in textiles
CN114703667A (en) * 2022-01-18 2022-07-05 北京理工大学 A method for preparing flame-retardant cotton fabric based on attapulgite soil layer-by-layer self-assembly technology

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103951920A (en) * 2014-05-07 2014-07-30 浙江理工大学 Preparation method of polyelectrolyte complex flame-retardant polyvinyl alcohol containing phosphorus and nitrogen
CN105256554A (en) * 2015-11-17 2016-01-20 浙江理工大学 Method for improving durability of color of electrostatic self-assembly bionic structure color generating textiles
CN105484017A (en) * 2015-11-23 2016-04-13 浙江理工大学 Electrostatic self-assembly deepening method for fabric
CN106752055A (en) * 2017-01-05 2017-05-31 南京林业大学 A kind of preparation method of LBL self-assembly flame-retardant wood-plastic composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103951920A (en) * 2014-05-07 2014-07-30 浙江理工大学 Preparation method of polyelectrolyte complex flame-retardant polyvinyl alcohol containing phosphorus and nitrogen
CN105256554A (en) * 2015-11-17 2016-01-20 浙江理工大学 Method for improving durability of color of electrostatic self-assembly bionic structure color generating textiles
CN105484017A (en) * 2015-11-23 2016-04-13 浙江理工大学 Electrostatic self-assembly deepening method for fabric
CN106752055A (en) * 2017-01-05 2017-05-31 南京林业大学 A kind of preparation method of LBL self-assembly flame-retardant wood-plastic composite material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113186727A (en) * 2021-05-08 2021-07-30 兰州大学 Inorganic-bio-based anti-photoaging flame retardant and application thereof in textiles
CN114703667A (en) * 2022-01-18 2022-07-05 北京理工大学 A method for preparing flame-retardant cotton fabric based on attapulgite soil layer-by-layer self-assembly technology

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Application publication date: 20181211