| Phosphorus flame retardant has excellent flame retardant properties and many varieties. It isthe main way to achieve non-halogenated flame retardant agent and be used widely. In which,the phosphate flame retardants have excellent thermal stability and compatibility. However,phosphorus flame retardant has many disadvantages, such as a large quantity of smoke andtoxicity, so its application has been somewhat restricted. In addition, as people continue toenhance environmental awareness and environmental regulations becoming more perfect,organic boron flame retardant are more and more people’s attentions by its non-toxic, noncorrosive, sterilization and smoke suppression and other features. However, it’s flame retardantand hydrolytic stability is generally worse than the phosphorus flame retardant. Therefore,developing the boron compound of phosphorus flame retardants of used the textile field will helpto combine the advantages of both, and reducing some defects. It has good research significance.The paper chooses P1and B1for the intermediate, making the new flame retardant BP-Fwhich is used to cotton fabrics. There are three parts in this research:Part one: Synthesis of intermediate P1and B1. There are a lot of problems existing intraditional synthesis process of P1, such as over products of phosphoryl chloride, high reactiontemperature and long reaction time. In this part, the synthesis process of P1was optimizd, theimpacts of the main factors on rate of production was studied. It is found that the best synthesisprocess of P1were gained when the catalyst of anhydrous aluminium vhloride dosage was1.2%,the amount of acetonitrile was12mL/g, the molar ratio of phosphorus oxychloride andpentaerythriol was2.6:1, the reaction temperature and time was80℃and8h, respectively. Theexperimental results showed that when the P1was synthesis by the optimal preparation, themolar ratio of phosphorus oxychloride and pentaerythriol was reduced from5.5:1to2.6:1, thereaction temperature was reduced from100℃to80℃, the reaction time was reduced from24hto8h, the production yields was increased from70%to83%. Therefore, this novel process wasmeeting the requirements of energy-saving and consumption reduction and environmentalrequirements. Meanwhile, the effects of individual factors on production yields of B1were analyzed, and the process condition of synthesis was optimized. The experimental results showedthat when the reaction temperature was130℃, the reaction time was3h, the catalystof p-toluene sulphonic acid was1.0%, the production yields of B1was up to92.9%.Part two: Synthesis and characterization of phosphorus-boron compound flame retardant. Inthis part, the B1and P1were used to synthesis novel phosphorus-boron compound flameretardant by bulk polymerization. The influence of the dosage of catalyst, reaction tempretureand time, and the molar ratio of intermediate on configuration and properties of the flameretardant were characterized. The experimental results showed that when the molar ratio of P1and B1was1:1.04, reaction temperature was110℃, reaction time was8h, the catalyst ofanhydrous aluminium vhloride dosage was0.6%, flame retardant BP-F yields is up to79.6%.Meanwhile, infrared spectroscopy analysis aslo confirmed the product as the goal of productBP-F.Part three: Application and performance test of phosphorus-boron compound flameretardant. In this part the application process of self-made flame retardant was studied. Theeffects of the flame retardant BP-F on flame retardancy, washing and other applicationperformance of cotton fabric was evaluated. The flame retardancy mechanism of BP-F flameretardant on cotton fabric was characterized by a variety of means of modern instrument analysis,such as thermal analysis, scanning electron microscopy, carbon formation analysis and infraredspectroscopy. It is found that the cotton fabric can be obtained good flame retardancy when theamount of flame retardant BP-F was250g/L, the melamine dosage was20g/l, the pH value ofadjustment liquid at6, the baking temperature and time was160℃and75s respectively. Afterflame retardant BP-F finishing, the limiting oxygen index was increased from19.4to32.1. Theunfavorable washing fastness and good dry cleaning resistance can be obtained. The mechanicalstrength, whiteness and shade of the cotton fabrics have decline after flame retardant BP-Ffinishing. BP-F has good catalytic role of carbon dehydration for the cotton fabrics and caninhibit the producing of the L-glucose and flammable gases when the cotton fabrics wereburning. These showed that BP-F has good effect when it flame-retardant the cotton fabrics, andthe flame-retardant finishing has the small influence for fabrics, and it has a good applicationvalue. |
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