Synthesis And Application Of A Novel Fluorine-bromine-sulphur Diamine

Polymer material has become an indispensable material, which is widely used incutting-edge technology, national defense and national economy, because of itsincomparable performance. However, polymeric materials are flammable, with highburning velocity and difficulty in stopping their burning, thereby endangering thesafety of people’s lives and property. Improving the flame retardancy of polymer hasbecome an issue of concern. Research and development of new flame retardants arealso very necessary.In this study, a novel diamine4,4’-((sulfonylbis(2,6-dibromo-4,1-phenylene))bis(-oxy))bis(3-(trifluoromethyl)aniline)(SPBFA) containing both fluorine, bromine andsulfur was synthesized and was used to prepare a series of BSFPUEs. In addition, twonovel flame retardants: expandable graphite and ammonium polyphosphate flameretardant microcapsules were prepared as with SPBFA capsule timber material, andthey were used to prepare a series of PPEGs and PPAPPs, respectively. Theperformance of the materials above was also investigated.1. The SPBFA was synthesized by nitration reaction and hydrazine reduction basedon5-nitro-o chlorobenzotrifluoride and tetrabromobisphenol S and characterized byfourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance(NMR). The above characterizations were in good agreement with the chemicalstructure of SPBFA.2. SPBFA was utilized as chain extender to prepare a series of polyurethaneelastomers (BSFPUEs) with different structures. The BSFPUEs were investigated bymicroscale combustion colorimeter (MCC), thermo-gravimetric analysis (TGA),cone calorimeter and contact angle. The results showed that: BSFPUEs had goodflame retardant properties. Compared with ordinary polyurethane elastomer PUE, thethermal stability of BSFPUEs decreased, but the char yield increased significantly bynearly12times. The peak heat release rate(PHRR) and total heat release(THR) of theBSFPUE3with dense surface carbon residue were decreased by49.7%and46.8%，respectively. And the same for the cone calorimeter. Meanwhile, BSFPUEs had goodhydrophobic and oleophobic low surface energy, and BFPUE3’s contact angle with water was92.8°, their contact angle with ethylene glycol was79.9°, and theirsurface tension was20.0mN/m.3. PUEG and PUBEG were successfully prepared with3,3-dichloro-4,4-diamino diphenyl methane (MOCA) and SPBFA raw material for the capsule，respectively. They were characterized by FTIR, scanning electron microscope (SEM)and volume expansion, and the results showed that PUEG and PUBEG werecompletely packaged.4. PPEGs composites were prepared with EG, PUEG and PUBEG as flameretardants, respectively. The effects on the flame retardancy, thermal stability andcompatibility impact of the PPEGs with different contents of EG, PUEG and PUBEGwere investigated by cone calorimeter, MCC, TGA and microscopic characterizationmethods. The results showed that: with the increase of the content of flame retardant,PHRR and THR of PPEGs were reduced, and carbon residue increased. Thecomparison of PPEGs mixed with PUBEG, PUEG and EG indicated that the formerhad lower PHRR and higher char residue, with better fire safety.5. Ammonium polyphosphate (APP) microcapsules (PUAPP and PUBAPP) weresuccessfully prepared with MOCA and SPBFA as capsules，respectively. They werecharacterized by FTIR, SEM, TGA and contact angle, and the results showed thatPUAPP and PUBAPP were completely packaged.6. The effects of APP, PUAPP and PUBAPP on the thermal stability, flameretardancy and mechanical properties of PP composites were studied. TGA analysisshowed microencapsulated APP could decrease PP/APP composites’ thermaldegradation. Analysis of cone calorimetric data showed that compared with the samecontents of the flame retardant, the PPAPPs mixed with microcapsulated APP hadbetter flame retardancy performance, and higher fire safety. MCC analysis showedPPAPP-8had the best flame retardant properties due to the sulfur-containing fluorinebromine flame retardant elements in PUBAPP. The SEM of the cross-sectiondiagram dealing with hot water immersion showed that microencapsulation coulddramatically reduce the water solubility of APP, and improve its compatibility,because the polyurethane shell effectively prevented the APP from being affected bywater erosion.