Preparation and characterization of durable flame retardant cotton fabrics using phosphorylation reaction of cellulose with ammonium etidronate

IF 2.4 3区化学 Q3 POLYMER SCIENCE

Iranian Polymer Journal Pub Date : 2024-03-02 DOI:10.1007/s13726-024-01287-9

Won-Guk Choe, Wi-Phyong Kung, Yong-Man Jang, Pom Choe, Chung-Guk Choe, Chol-Jun Yu

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Abstract

Developing an effective flame retardant for cotton is urgently needed to minimize the life and property loss caused by fire hazard. Here, diphosphonate system flame retardant, the ammonium salt of 1-hydroxyethylidene-1,1-diphosphonic acid (AHEDPA) is obtained by reacting urea with etidronic acid (or HEDPA), which is newly synthesized from acetic acid, phosphorus oxychloride and phosphorous acid. We predicted the suitable conditions of phosphorylation reaction for enhancing grafting rate of AHEDPA on cotton fibers, and revealed the mechanism of reaction using dicyandiamide as an accelerant. Through the Fourier transform infrared spectra and scanning electron microscopy analysis, it was found that AHEDPA with P = O(ONH₄⁺)₂ functional groups could be combined with –OH groups of cellulose, creating the P−O−C and P−NH₂ bonds. Limiting oxygen index, vertical flame test and cone calorimetric measurements were carried out on the untreated and treated cotton fabric samples with AHEDPA at different concentrations, demonstrating that the flame retardant cotton fabric with excellent washing durability were successfully obtained. Through the thermogravimetric analysis, it was confirmed that the cotton fabrics treated with AHEDPA exhibited a promotion of dehydration in cellulose and thus an increase of char formation rate, thereby protecting the substrate (cotton) from heat and fuel. The newly proposed method could enhance the grafting rate of cotton and remarkably improved the flame retardancy and durability of cotton fabrics, highlighting a wide prospect in production of flame retardant clothes.

Graphical abstract

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利用纤维素与依替膦酸铵的磷化反应制备耐用阻燃棉织物并确定其特性

为了最大限度地减少火灾造成的生命和财产损失，迫切需要开发一种有效的棉花阻燃剂。本文通过尿素与乙酸、氧氯化磷和磷酸新合成的乙烯膦酸（或 HEDPA）反应，得到了二膦酸盐体系阻燃剂--1-羟基亚乙基-1,1-二膦酸铵盐（AHEDPA）。我们预测了磷化反应的适宜条件，以提高 AHEDPA 在棉纤维上的接枝率，并以双氰胺为促进剂揭示了反应机理。通过傅立叶变换红外光谱和扫描电子显微镜分析发现，带有 P = O(ONH4+)2 官能团的 AHEDPA 能与纤维素的 -OH 基团结合，生成 P-O-C 和 P-NH2 键。对未经处理和经不同浓度 AHEDPA 处理的棉织物样品进行了极限氧指数、垂直燃烧试验和锥形量热测定，结果表明成功获得了具有优异洗涤耐久性的阻燃棉织物。通过热重分析，证实了经 AHEDPA 处理的棉织物具有促进纤维素脱水的作用，从而提高了成炭率，从而保护了基材（棉花）免受热量和燃料的影响。新提出的方法可提高棉花的接枝率，显著改善棉织物的阻燃性和耐久性，在生产阻燃服装方面具有广阔的前景。

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来源期刊

Iranian Polymer Journal 化学-高分子科学

CiteScore

4.90

自引率

9.70%

发文量

107

审稿时长

2.8 months

期刊介绍： Iranian Polymer Journal, a monthly peer-reviewed international journal, provides a continuous forum for the dissemination of the original research and latest advances made in science and technology of polymers, covering diverse areas of polymer synthesis, characterization, polymer physics, rubber, plastics and composites, processing and engineering, biopolymers, drug delivery systems and natural polymers to meet specific applications. Also contributions from nano-related fields are regarded especially important for its versatility in modern scientific development.