首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 312 毫秒
1.
To achive excellent fire resistance, new microcapsule flame retardants (DMCAD and DMPPD) were prepared using 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide combined with melamine cyanurate or melamine polyphosphate as the shell material and diatomite as the core material. The successful assembly of DMCAD and DMPPD was detailed characterized by Fourier transform infrared (FT‐IR) spectra, X‐ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Meanwhile, the flame retardancy and thermal stability of the unsaturated polyester resin (UPR)/DMCAD and UPR/DMPPD composites were also studied. The addition of DMCAD and DMPPD effectively improves the flame retardance properties of UPR, and the effect of DMPPD was better. The limiting oxygen index (LOI) of UPR/DMPPD‐3 increased by 11.6% when compared with that of UPR, and the sample achieved V‐0 rating. Moreover, the peak heat release rate (pHRR) and the total heat release (THR) rate of UPR/DMPPD‐3 were reduced by 67% and 26%, respectively. Under nitrogen condition and air condition, UPR/DMPPD showed better thermal stability and char‐forming ability from the thermogravimetric (TG) results. Residual char of the UPR composites was systematically analyzed with SEM and XPS. Finally, the flame retardant mechanism of DMPPD was proposed.  相似文献   

2.
Modified montmorillonite‐containing phytic acid (PA‐MMT) has been prepared by acid treatment and then introduced into unsaturated polyester resin (UPR) with an intumescent flame retardant (IFRs). The flame retardancy and thermal degradation of UPR/IFRs/PA‐MMT were evaluated by a limiting oxygen index (LOI) test, a vertical burning test (UL‐94), a thermogravimetric analysis (TGA), and a cone calorimeter test (CCT). Besides, the mechanical properties were studied by a universal testing machine. The LOI value of UPR/IFRs/PA‐MMT composites was increased to 29.2%. The CCT results indicated that the incorporation of PA‐MMT and IFRs significantly improved the combustion behavior of UPR. The results of the mechanical properties indicated that 1.5 wt% loading of PA‐MMT in UPR/IFRs showed the highest improvement in flexural strength and tensile strength. The flame‐retardant mechanism of PA‐MMT/IFRs was examined and discussed based on the results of combustion behavior and char analysis.  相似文献   

3.
In this work, phosphorylated chitosan‐coated carbon microspheres (PCH@CMS) was successfully synthesized. Obtained PCH@CMS used as flame retardant was added into unsaturated polyester resin (UPR). Fourier infrared spectroscopy (FTIR) and X‐ray electron spectroscopy (XPS) results indicated that C═O, P─O, and P═O appeared on the surface of PCH@CMS. Compared with UPR, the residues of UPR/PCH@CMS‐10 at 800°C under nitrogen and air atmospheres increased by 9.0 and 3.9 wt%, respectively, and the peak heat release rate (pHRR) and the peak smoke release rate (pSPR) of UPR/PCH@CMS‐3 decreased by 18.9% and 23.5%, respectively. Limiting oxygen index (LOI), thermogravimetric analyzer (TG), and cone calorimeter test (CCT) results showed that the addition of PCH@CMS could enhance the flame retardancy and smoke suppression of the UPR composites. Moreover, the residues after CCT were characterized by scanning electron microscopy (SEM), XPS, and laser Raman spectroscopy (LRS). Based on the above results, the flame retardant mechanism of PCH@CMS was proposed. The carbon layer produced by the UPR/PCH@CMS composites was tortuous and could suppress the heat and pyrolysis product exchange with UPR matrix.  相似文献   

4.
A phosphorus and silicon containing liquid monomer (9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene 10‐oxide–vinyltrimethoxysilane (DOPO–VTS)) was synthesized by the reaction between DOPO and VTS. DOPO–VTS and methacryloxypropyltrimethoxylsilane were introduced into unsaturated polyester resin to prepare flame retardant UPR/SiO2 (FR‐UPR/SiO2) hybrid materials by sol–gel method and curing process. DOPO–VTS contributes excellent flame retardancy to UPR matrix, which was confirmed by the limiting oxygen index and microscale combustion calorimeter results. The thermogravimetric analysis (TGA) results indicate that the FR‐UPR/SiO2 hybrid materials possess higher thermal stability and residual char yields than those of pure UPR at high temperature region. The thermal degradation of materials was investigated by TGA/infrared spectrometry (TG‐IR) and real‐time infrared spectrometry (RT‐IR), providing insight into the thermal degradation mechanism. Moreover, scanning electron microscopy (SEM) and X‐ray photoelectron spectroscopy (XPS) were used to explore the morphologies and chemical components of the residual char. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

5.
Metal‐organic framework MIL‐53 (Fe)@C/graphite carbon nitride hybrid (MFeCN), a novel flame retardant, was synthesized by hydrothermal reaction and subsequently added into unsaturated polyester resin (UPR). The structure, morphology, and thermal stability of MFeCN were characterized by Fourier transform infrared spectroscopy (FTIR), X‐ray diffraction (XRD), X‐ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDS), and thermogravimetric analysis (TG). The thermal stability and flammability of the UPR composites were characterized by TG and cone calorimeter tests (CCT). The results of CCT demonstrated that the peak heat release rate (pHRR), total heat release (THR), peak smoke production rate (pSPR), and total smoke production (TSP) of UPR/MFeCN‐4 were reduced by 39.8%, 10.2%, 33.3%, and 14.5%, respectively, comparing with UPR. The results of TG and CCT indicated that MFeCN could improve the thermal stability, flame retardancy, and smoke suppression properties of the UPR composites. The residues after CCT were then characterized by laser Raman spectroscopy (LRS), XPS, and SEM. Finally, based on the above experimental results and analysis, the flame retardancy mechanism of MFeCN was proposed.  相似文献   

6.
A transparent flame‐retardant unsaturated polyester resin (FR‐UPR) was obtained by reacting propylene glycol (PG) with maleic anhydride (MA), phthalic anhydride (PA), and 9,10‐dihydro‐10[2,3‐di(hydroxy carbonyl)propyl]‐10‐phosphaphenanthrene‐10‐oxide (DDP) synthesized from 9,10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene 10‐oxide (DOPO) and itaconic acid (ITA). The chemical structure of the resulting FR‐UPR was confirmed by FTIR, 1H‐NMR and 31P‐NMR. The average molecular weight and viscosity of the FR‐UPR were determined by gel permeation chromatography (GPC) and viscometer, respectively. Thermal stability was studied by thermogravimetric analysis (TGA) both in air and nitrogen to determine the thermal decomposition mechanism, and the apparent activation energy (Ea) was calculated by both the Kissinger and Ozawa methods. Compared to unsaturated polyester resin (UPR), the higher Ea of FR‐UPR3 implied an improved thermal stability. According to variations of the limited oxygen index (LOI) values, the UL 94 rating of vertical burning test and scanning electron microscopy (SEM) photographs of char residues, the flame retardance of cured FR‐UPR was enhanced with increasing DDP content. The study of fire reaction tests, using a cone calorimeter, suggested that there was a significant reduction of flammability in the FR‐UPR. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

7.

Unsaturated polyester resin (UPR) is a widely applied engineering material with drawbacks of high fire risks and brittleness. In this paper, low-cost diethylene glycol (DEG) was used as one of diols to react with saturated and unsaturated anhydrides for unsaturated polyester pre-polymers. Fourier transform infrared spectroscopy, nuclear magnetic resonance spectroscopy, gel permeation chromatograph were used for studying their structures and differential scanning calorimetry, thermogravimetric analysis (TG) for studying their thermal properties. Incorporated DEG comonomer improves limited oxygen index values of cross-linked UPR from 20 to 26% as the mole proportion of DEG increases from 0 to 50 mol% in diols. Combustion test indicates that the UPR sample with 70 mol% DEG in diols is self-extinguishing with none drop, referring to nonflammable burning grade. What is more, mechanical properties are also increased greatly by comparing with typical UPR base. Pyrolysis behaviors of UPR in nitrogen atmosphere suggest that the polyesters incorporated with DEG will produce more char and residues during the degradation process. By comparing the pyrolysis behaviors of UPR having DEG with those of UPR adding ammonium polyphosphate in TG curves, the flame-retarding mechanism of DEG incorporation is probably due to residual char forming in temperature range of 500–800 °C, which is close to the burning temperature. This study suggests that DEG element increases effectively and environmental friendly the fire safety of UPR materials.

  相似文献   

8.
The organo-montmorillonite (MT), combined with a DOPO-based oligomer (PDAP), was used to improve the flame retardancy of epoxy thermoset. The thermal stabilities and flame-retardant properties of thermosets were investigated by thermogravimetric analysis, limiting oxygen index (LOI) and UL-94 tests. The synergistic effect of MT and PDAP was studied by Py–GC/MS, Fourier transform infrared spectroscopy, elemental analysis, laser Raman spectroscopy and scanning electron microscope. Results revealed that 0.5 mass% MT combined with 4 mass% PDAP showed obvious synergistic effect on enhancing the flame retardancy of thermoset. The corresponding thermoset achieved an LOI value of 35.5% and V-0 rating in UL-94 test, which was attributed to the intense blowing-out effect during combustion. The synergistic mechanism was probably ascribed to the formation of silicoaluminophosphate (SAPO) originating from the reaction between MT and PDAP. The SAPO serving as a solid acidic catalyst, coupled with the acid sites from the decomposition of organomodifier in MT, could promote the charring process. With the further increase in MT content, the charring process was strongly promoted and more phosphorus element was retained in the condensed phase, which inevitably resulted in the remarkable decrease of the amount of pyrolytic gases containing phosphorus-based radicals and nonflammable gases. These factors were responsible for the diminished blowing-out effect during combustion, which was adverse to the further improvement of flame retardancy.  相似文献   

9.
The thermal degradation and combustion behaviour of an interpenetrating network (IPN) structure of unsaturated polyester UP resin and a resole type of phenolic resin was studied. Thermal gravimetric analysis (TGA) was used to monitor the degree of thermal decomposition for the UP/phenol IPN structure and the change of the oxygen index (OI) was used to describe the variation of the combustion behaviour. The smoke density was measured via a non-flaming process to detect the amount of smoke generated during the combustion. A homemade cone calorimetric dynamic flammability evaluation system was assembled to analyse the gas evolved and to measure the heat release rate (HRR) during the combustion. Under simulated conditions of a burning field at the temperature of 757°C, the variation of the concentration of carbon monoxide (CO) and the HRR of the UP/phenol IPN structure were studied. The results show that modification of the essentially flammable UP resin by the phenol structure to form an IPN system cannot only remarkably improve the heat resistance but also help to suppress the smoke, toxic gas and heat release during the combustion.  相似文献   

10.
采用原位聚合法制备了蜜胺树脂(MF)和环氧树脂(EP)双层包裹聚磷酸铵(APP),得到一种新型核壳结构的微胶囊阻燃剂(EMFAPP).用傅里叶红外光谱(FTIR)和扫描电镜(SEM)对微胶囊的核壳结构进行了表征;用极限氧指数(LOI)、垂直燃烧等级测试(UL 94)对EMFAPP在EP中的阻燃性能进行了研究.EMFAPP在EP基体中阻燃性能优异,当其添加量大于7%时EP/EMFAPP均通过UL 94 V-0级,LOI值达27.0%以上.与未包裹APP相比,EMFAPP耐水性明显提高;经水处理(75℃,6天)后,EMFAPP/EP仍可保持良好的阻燃性能.采用热重分析对EMFAPP及其阻燃复合物的热降解行为进行了研究,EMFAPP能够促进成炭,EP/EMFAPP(8 wt%)在700℃残炭率达16.2%,但其低温稳定性有所下降.此外,利用热失重-红外联用对EMFAPP/EP的热降解行为进行了研究,探讨相关阻燃机理.  相似文献   

11.
Phosphorus/nitrogen‐containing advanced epoxy resins were obtained by chain‐extension of the diglycidyl ether of bisphenol‐A epoxy (DGEBA) resin with phosphorus‐modified triglycidyl isocyanurate (TGICP). The structure of TGICP was characterized by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR). Differential scanning calorimetry revealed that the EP/TGICP composites possessed higher glass transition temperatures than that of phosphorus free EP. The thermal stability and flame retardant properties of the epoxy resin/TGICP systems were investigated by thermogravimetric analysis (TGA), limiting oxygen index (LOI), and vertical burning test (UL‐94) test. When the TGICP content was 10 wt%, the LOI value of epoxy resin system was as high as 35.0% and it can obtain the V‐0 grade in UL‐94 protocol. From microscale combustion calorimetry (MCC) measurement, it was found that the addition of TGICP reduced the value of peak heat release rate and total heat release. The thermal degradation process of EP and EP/TGICP composite was monitored by real time FTIR. Moreover, scanning electron microscopy (SEM) and X‐ray photoelectron spectroscopy (XPS) were used to explore the morphology and chemical components of the char residues. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

12.
Two original art installations constructed from unsaturated polyester resins (UPR) and four different reference UPR products (before and after UVB aging) were analyzed by high-resolution 1D and 2D nuclear magnetic resonance (NMR) spectroscopy. Breaking strain studies were also conducted for the four UPR model products before and after different aging procedures (moisture, UVB exposure, melt/freeze). NMR analysis of the chemical composition of the UPR resin extracts showed they contain several low MW organic compounds and oligomers rich in polar -OH groups that play a significant role in the degradation behavior of the composite UPR materials. Statistical analysis of the NMR compositional data showed that styrene and benzaldehyde contents can be used to differentiate between fresh and aged UPR samples. The phthalate and propylene glycol unit speciation (esterified, primary or secondary -OH) of the extracts provided evidence that UPR resin C was used in the construction of the two art installations, and direct comparison of (1)H and (13)C NMR spectra verified this compositional similarity. UPR resin C was shown by both NMR and breaking strain studies to be the reference UPR most susceptible to degradation by different aging procedures, a characteristic attributed to the lower styrene content of resin C.  相似文献   

13.
Calcium alginate fibers were prepared by wet spinning of sodium alginate into a coagulating bath containing calcium chloride.The thermal degradation and flame retardancy of calcium alginate fibers were investigated with thermal gravimetry(TG),X-ray diffraction(XRD),limiting oxygen index(LOI) and cone calorimeter(CONE).The results show that calcium alginate fibers are inherently flame retardant with a LOI value of 34,and the heat release rate(HRR),total heat release(THR),CO and CO_2 concentrations during ...  相似文献   

14.
A novel phosphorus‐containing monomer, (6‐oxido‐6H‐dibenzo[c,e][1,2]oxaphosphinin‐6‐yl)methyl acrylate (DOPO‐AA), is first synthesized and characterized by Fourier transform infrared spectra (FTIR), 1H nuclear magnetic resonance (NMR) and 31P NMR. The monomer is then introduced into poly (methyl methacrylate) (PMMA) matrix via in situ copolymerization to produce a new PMMA based copolymer (PMMA/DOPO‐AA). From UV–vis spectra, microscale combustion calorimeter (MCC) and thermogravimetric analyses (TGA) results, the as‐fabricated PMMA/DOPO‐AA copolymers not only keep relatively high transparency, but also exhibit remarkable improvements in the flame retardancy and thermal stability, such as increased T0.5 by 60.2°C and limited oxygen index (LOI) by 4.1, and decreased peak heat released rate (PHRR) by 34.7%. Thermal degradation behaviors investigated by real time Fourier transform infrared spectra (RTIR), char structure analysis studied by scanning electron microscope (SEM) and pyrolysis gaseous products studied by TGA coupled with FTIR (TGA‐FTIR) demonstrate that the catalytic charring function of DOPO‐AA in condensed phase and DOPO flame retardant systems in the gas phase are two key factors for the property enhancements. This work not only provides a promising flame‐retardant monomer for polymers, but also will stimulate more efforts on the development of DOPO‐containing flame‐retardant monomers. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

15.
A phosphorus-nitrogen containing flame retardant additive of poly(phosphoric acid piperazine),defined as PPAP,was synthesized by the salt-forming reaction between anhydrous piperazine and phosphoric acid,and the dehydration polymerization under heating in nitrogen atmosphere.Its chemical structure was well characterized by Fourier transform infrared (FTIR) spectroscopy,13C and 31p solid-state nuclear magnetic resonance measurements.The synthesized PPAP and curing agent m-phenylenediamine were blended into epoxy resin (EP) to prepare flame retardant EP thermosets.The effects of PPAP on the fire retardancy and thermal degradation behavior of cured EP/PPAP composites were investigated by limiting oxygen index (LOI),vertical burning (UL-94),thermogravimetric analysis/infrared spectrometry (TG-IR) and cone calorimeter tests.The morphologies and chemical compositions of char residues for cured epoxy resin were investigated by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS),respectively.The results demonstrated that the flame retardant EP thermosets successfully passed UL-94 V-0 flammability rating and the LOI value was as high as 30.8% when incorporating 5wt% PPAP into the EP thermosets.The TGA results indicated that the synthesized PPAP flame retardant additive possessed high thermal stability and excellent charring capability.Meanwhile,the incorporation of PPAP stimulated the epoxy resin matrix to decompose and charring ahead of time due to its catalytic decomposition effect,which led to a higher char yield at high temperature.The morphological structures and the analysis results of XPS for char residues of EP thermosets revealed that the introduction of PPAP benefited the formation of a sufficient,more compact and homogeneous char layer containing phosphorus-nitrogen flame retardant elements on the material surface during combustion.The formed char layer with high quality effectively prevented the heat transmission and diffusion,limited the production of combustible gases,and inhibited the emission of smoke,leading to the reduction of heat and smoke release.  相似文献   

16.
以芝麻秸秆粉、水稻秸秆粉、玉米芯秆粉、菠萝叶粉、甘蔗渣粉五种不同植物纤维粉为填充体、不饱和聚酯树脂(UPR)为基体制作植物纤维粉/UPR复合材料,对比研究了秸秆种类对复合材料密度、力学性能及吸水性能的影响。结果表明,植物纤维粉粒径为100目、添加量为UPR用量的10%时,芝麻秸秆粉/UPR复合材料的综合力学性能最好,拉伸强度、弯曲强度和冲击强度分别为41.320 MPa、67.467 MPa和2.815 KJ/m^2,且每一浸泡阶段吸水率均最低。  相似文献   

17.
以聚苯氧基磷酸联苯二酚酯(PBPP)与聚磷酸铵(APP)组成复合阻燃剂,对环氧树脂(EP)进行阻燃改性.通过氧指数(LOI)、垂直燃烧(UL-94)、热失重(TGA)、锥形量热(CONE)和扫描电镜(SEM)等方法研究改性环氧树脂的阻燃性能和阻燃机理.结果表明,PBPP/APP体系对EP具有较好的阻燃性能,阻燃剂添加量为10%时能使环氧树脂的氧指数提高到29.6%,垂直燃烧等级达到UL94 V-0级,残炭量大大增加;平均热释放速率下降45.7%,热释放速率峰值下降51.0%,有效燃烧热平均值下降21.1%;TGA、CONE、SEM等综合分析显示了PBPP/APP改性后的环氧树脂比纯环氧树脂具有更高的热稳定性,燃烧后能够形成连续、致密、封闭、坚硬的焦化炭层,在聚合物表面产生有效覆盖、隔绝了氧气,改善了环氧树脂的燃烧性能.  相似文献   

18.
A flame-retardant epoxy resin (EP) was synthesized based on a novel reactive phosphorus-containing monomer, 4-[(5,5-dimethyl-2-oxide-1,3,2-dioxaphosphorinan-4-yl)oxy]-phenol (DODPP), and its structures were characterized by FTIR, 1H NMR and 31P NMR spectra. The DODPP-EP3/LWPA (low molecular weight polyamide), which contains 2.5% phosphorus, can reach UL-94 V-0 rating and a limiting oxygen index (LOI) value of 30.2%. The thermal properties and burning behaviours of cured epoxy resins were investigated by differential scanning calorimeter (DSC), thermogravimetry (TG), LOI, UL-94 tests and cone calorimetry. The morphologies of residues of cured epoxy resins were investigated by scanning electron microscopy (SEM). DSC shows that the glass-transition temperatures of cured epoxy resins decrease with increasing phosphorus content. TGA shows that the onset decomposition temperatures and the maximum-rate decomposition temperatures decrease, while char yields increase, with the increase of phosphorus content. The data from the cone calorimeter tests give the evidence that heat release rate (HRR), peak heat release rate (PHRR), average heat release rate (Av-HRR), average mass loss rate (Av-MLR) and the fire growth rate index (FIGRA) decrease significantly for DODPP-EP3/LWPA. SEM shows that the DODPP-EP3/LWPA forms lacunaris and compact charred layers which inhibit the transmission of heat during combustion.  相似文献   

19.
A novel flame retardant curing agent for epoxy resin (EP), i.e., a DOPO (9,10-dihydro-9-oxa-10-phosphaphenan-threne-10-oxide)-containing 4,4'-bisphenol novolac (BIP-DOPO) was synthesized and characterized by Fourier transform infrared (FTIR), 1H NMR, 31P NMR spectroscopy, and gel permeation chromatography. The epoxy resin cured by BIP-DOPO itself or its mixture with a commonly used bisphenol A-formaldehyde novolac resin (NPEH720) was prepared. The flame retardancy of the cured EP thermosets were studied by limiting oxygen index (LOI), UL 94 and cone calorimeter test (CCT), and the thermal properties by thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). The results show that the cured epoxy resin EPNP/BI/3/1, which contains 2.2% phosphorus, possesses a value of 26.2% and achieves the UL 94 V-0 rating. The data from cone calorimeter test demonstrated that the peak release rate, average heat release rate, total heat release decline sharply for the flame retarded epoxy resins, compared with those of pure ones. DSC results show that the glass-transition temperatures of cured epoxy resins decrease with increasing phosphorus content. TGA indicates that the incorporation of BIP-DOPO promotes the decomposition of epoxy resin matrix ahead of time and leads to higher char yield. The surface morphological structures of the char residues reveal that the introduction of BIP-DOPO benefits to the formation of a continuous and solid char layer on the epoxy resin material surface during combustion.  相似文献   

20.
不饱和聚酯的改性   总被引:6,自引:0,他引:6  
综述了不饱和聚酯树脂的合成、性能以及改性方向。介绍了不饱和树脂功能化、精细化、高性能化的研究 ,并着重介绍了有机 /无机纳米复合不饱和聚酯的制备和性能  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号