论文总字数：24713字

摘 要

我国近十几年来，平均每年发生的纺织品火灾约3-4万起，死亡人数达3千人左右，火灾损失超过2亿元。不仅如此，即便起火源头是电气等其他原因，纺织品也因为是室内最主要装修装饰材料而快速传递火焰与热量，使得救援与扑灭都更加困难。如2015年西宁纺织品大楼火灾，克拉玛依友谊宾馆幕布起火等事件，都是源于纺织品起火并快速在室内蔓延，致使发烟量过大，温度过高而难以逃生或救援。而棉纺织品是应用最广泛的纺织品之一，且具有高度易燃性，因此提升棉织物的阻燃性能就成为了一件具有研究意义的工作。本文选用溶胶-凝胶法，制备阻燃剂，将其以浸渍烘焙法涂覆于棉织物上，增强其阻燃性能。

本文选用DOPO（9，10-二氢-9-氧杂-10-磷杂菲-10-氧化物）的衍生物DOPO-CH₂OH作为阻燃剂，将其引入SiO₂单一溶胶和SiO₂-KH560复合溶胶进行杂化，分析此溶胶-凝胶体系是否对棉织物阻燃性的改性有可观的作用。

首先，观察作为对照组的纯棉织物的外观与制备好的各溶胶-凝胶、溶液等，并用相机记录；与此同时，对制备好的溶胶与其他溶液等进行酸碱度、固含量及粒径分布进行实验测试并记录；然后，将制备好的各改性溶胶-凝胶体系使用浸渍烘焙法对纯棉织物进行改性整理；最后，对各改性棉织物与原始棉织物进行极限氧指数测试（LOI）、热失重测试（TG）和扫描电子显微镜分析（SEM）测试并记录，对各改性织物根据实验结果进行阻燃性能的合理推测；与此同时，记录LOI实验中各棉织物的燃烧情况，如火焰大小，是否熔融滴落和烟尘情况等。

实验显示，经杂化SiO₂-KH560-DOPO-CH₂OH溶胶-凝胶整理的棉织物LOI值由17%增至22.5%，增幅达到 32.4 %；TG实验则表明后整理棉织物的残碳率由 3 %提升至近 30 %，为原有数值的十倍；而SEM实验的图像则表明改性后的棉织物微观形态有一定变化，杂化SiO₂-KH560-DOPO-CH₂OH溶胶作用下，棉纤维形成致密炭层，且在燃烧后仍能较好的保持，对火焰有较强的抵抗作用。

结果表明，相对于单一DOPO-CH₂OH溶液等，杂化SiO₂-KH560-DOPO-CH₂OH溶胶-凝胶能有效加强棉织物的阻燃能力与热稳定性。

关键词：溶胶-凝胶 DOPO衍生物 棉织物 阻燃性能

Abstract

Fire accidents are one of the most frequent and most dangerous accidents in today's man-made accidents. The flammability of textiles is one of the main reasons for the rapid spread of fire and the ignition of fire. According to statistics, more than one-fifth of the fires are caused by the flammability of textiles. Moreover, even if the source of the fire is electrical and other reasons, the textiles quickly transmit flames and heat because they are the most important decoration materials in the room, making it difficult to rescue and fight. For example, the Xining Textile Building Fire in 2015, the Karamay Friendship Hotel Fire and other events were caused by the fire of textiles and the rapid spread of indoors, resulting in excessive smoke, high temperatures and difficulty in escape or rescue. Cotton textiles are one of the most widely used textiles and are highly flammable, so improving the flame retardant properties of cotton fabrics has become a research issue. In this paper, the sol-gel method was used to prepare the flame retardant, which was coated on cotton fabric by immersion baking method to enhance its flame retardant property.

In this paper, DOPO-CH₂OH, a derivative of DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), was selected as a flame retardant and introduced into SiO₂ single sol and SiO₂-KH560 composite sol. Hybridization was carried out to analyze whether the sol-gel system has a considerable effect on the modification of the flame retardancy of cotton fabrics.

First, the appearance of the cotton fabric as a control group was visually observed and tested for softness. Secondly, the prepared hybrid SiO₂-KH560-DOPO-CH₂OH sol gel system and other single solutions, sols, etc. were visually observed and recorded by a camera. At the same time, the acidity and alkalinity, solid content and particle size distribution of the prepared sol and other solutions were tested and recorded; then, the prepared modified sol-gel system was immersed and baked to the pure cotton fabric. Modified finishing; finally, the modified cotton fabric and the original cotton fabric were tested by limiting oxygen index test (LOI), thermogravimetric test (TG) and scanning electron microscopy (SEM), and recorded, according to each modified fabric. The experimental results were reasonably speculated for the flame retardant performance; at the same time, the burning conditions of the cotton fabrics in the LOI experiment, such as the size of the flame, whether the melt dripping and the soot were recorded, were recorded.

The experiment showed that the LOI value of the cotton fabric finished by hybrid SiO₂-KH560-DOPO-CH₂OH sol gel increased from 17% to 22.5%, which increased by 32.4%. The TG experiment showed that the residual carbon ratio of the finished cotton fabric increased from 3% to near30%, which is ten times the original value; while the SEM experiment shows that the modified cotton fabric has a certain change in microscopic morphology. Under the action of hybrid SiO₂-KH560-DOPO-CH₂OH sol, the cotton fiber forms a dense carbon layer.  And it can be better maintained after burning, and has a strong resistance to flame.

The results show that the hybrid SiO₂-KH560-DOPO-CH₂OH sol gel can effectively enhance the flame retardancy and thermal stability of cotton fabrics compared with single DOPO-CH₂OH solution.

Key Words：Sol-gel；DOPO derivative；cotton fabric；flame-retardant property

目 录

摘要 I

ABSTRACT II

第一章 绪论 1

1.1织物火灾事故及危害 1

1.1.1 源头性可燃性 1

1.1.2 过程可燃性 1

1.2 易燃纺织品处理措施 1

1.2.1 对纺织材料进行阻燃后处理而达到阻燃目的 1

1.2.2 后整理织物法 2

1.3 阻燃剂/溶胶-凝胶技术后整理阻燃织物研究进展 3

1.4 本文技术路线 4

第二章 杂化溶胶改性织物实验过程 5

2.1 实验用品和器材 5

2.2 实验前期准备 6

2.2.1 硅烷偶联剂的作用机理、选取及水解 6

2.2.2 复合SiO₂-KH560溶胶体系 6

2.2.3 杂化SiO₂-DOPO-CH₂OH溶胶体系 7

2.2.4 纯棉织物的预处理 7

2.2.5 渗透剂的选择实验 7

2.3 实验过程 7

2.3.1 阻燃整理 7

2.3.2 整理品性能测试 8

2.4 本章小结 9

第三章 DOPO溶胶-凝胶体系理化性质 10

3.1 杂化溶胶-凝胶外观 10

3.2 酸碱性 11

3.3 固含量 11

3.4 粒径分布 12

3.5 本章小结 13

第四章 DOPO杂化溶胶后整理棉织物阻燃特性分析 14

4.1 改性后织物的形貌 14

4.2 燃烧行为分析 14

4.3 极限氧指数（LOI）测试及分析 15

4.3.1 整理后目标织物的LOI值 15

4.3.2 △LOI/△m分析 16

4.4 改性后织物热解特性分析 16

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