Biobased Furfurylated Poplar Wood for Flame-Retardant Modification with Boric Acid and Ammonium Dihydrogen Phosphate

Furfurylated wood exhibits excellent dimensional stability and corrosion resistance,making it a promising material for constructing buildings,but it is highly flammable.Herein,flame-retardant furfurylated poplar wood was produced via a two-step process utilizing boric acid(BA)and ammonium dihydrogen phosphate(ADP)as flame-retardant components,and biomass-derived furfuryl alcohol(FA)as a modifier.The acidity of BA and ADP allowed them to catalyze the polymerization of FA,which formed a cross-linked network that immobilized BA and ADP inside the wood.The addition of BA/ADP substantially delayed the time to ignition from 10 to 385 s and reduced the total heat release and total smoke release by 58.75%and 77.31%,respectively.Analysis of the pyrolysis process showed that the decomposition products of BA and ADP protected the underlying furfurylated wood and diluted combustible gases.This method significantly improved the fire retardancy and smokeless properties of furfurylated wood,providing promising prospects for its application as an engineering material.

Rapid Determination of Cd in Squilla by Mixed Acid Leaching-flame Atomic Absorption Method

[Objective] This study was conducted to find a method for rapid determi-nation of Cd in squil a. [Method] Cd in squil a was determined by mixed acid leach-ing-flame atomic absorption method by digesting samples with HNO3-HSO4 （5：1） and determining Cd in the samples by a flame atomic absorption spectrophotometer. [Results] The Cd contents in squil a were 1.0-2.0 mg/kg, and the recoveries of Cd were 86%-109%, and the relative standard deviations were 0-6%. [Conclusion] The method is simple and rapid with strong operability, good reproducibility and high ac-curacy.

Synergistic effect of MXene on the flame retardancy and thermal degradation of intumescent flame retardant biodegradable poly(lactic acid)composites

The effect of Ti3C2 MXene nanosheets on the intumescent flame retardant(IFR)poly(lactic acid)(PLA)composites was investigated among a series of PLA/IFR/MXene,which were prepared by melt blending 0-2.0 wt%MXene,10.0 wt%-12.0 wt%IFR and PLA together.The results of limiting oxygen index(LOI)and vertical burning(UL-94)discover that the combination of 0.5 wt%MXene and 11.5 wt%IFR synergistically improves the fire safety of PLA to reach UL-94 V-0 rating with LOI value of 33.0%.The PLA/IFR/MXene composites perform an obvious reduction in peak of heat release rate(HRR)in cone calorimeter tests(CCTs).Furthermore,the carbon residues after CCTs were characterized by scanning electron microscope(SEM),laser Raman spectroscopy(LRS),X-ray diffraction(XRD)and X-ray photoelectron spectroscopy(XPS).It is demonstrated that both the titanium composition of the MXene structure and the characteristics of the two-dimensional material enhance the PLA/IFR/MXene composite materials’ability to produce a dense barrier layer to resist burnout during thermal degradation.

Novel Bio-based Flame Retardant Systems Derived from Tannic Acid

In this study,tannic acid(TA)was investigated as flame retardant agent for PLA.Different strategies to modify its thermal degradation pathway have been explored in order to improve its charring effect.The first one consists in combining TA with organomodified montmorillonite(oMMT),and enables limiting the thermo-oxidative degradation of TA and promoting the formation of an effective char layer.Flame-retardant(FR)behavior of PLA-based composition has been found to be positively impacted by this combination since a reduction of the peak of Heat Release Rate(PHRR),more important than the value recorded when oMMT and tannic acid are used separately,has been obtained.The second strategy,in which tannic acid was associated with a biosourced phosphorousbased compounds,i.e.metallic phytate salt,evidenced another alternative allowing enhancing TA flame retardant effect at 30 wt%loading content.The third and last strategy explored aims to chemically modify TA via a chemical grafting of phosphoric acid groups.This phosphorylated TA was shown to present the most effective flame-retardant(FR)effect.However,an important reduction of PLA molecular weight was observed.

Determination of Iron in Layered Crystal Sodium Disilicate and Sodium Silicate by Flame Atomic Absorption Spectrometry with Boric Acid as a Matrix Modifier

The effects of matrix silicate and experimental conditions on the determination of iron in flame atomic absorption spectrometry （FAAS） were investigated. It was found that boric acid as a matrix modifier obviously eliminated silicate interference. Under the optimum operating conditions, the determination results of iron in layered crystal sodium disilicate and sodium silicate samples by FAAS were satisfactory. The linear range of calibration curve is 0-10.5 μg.mL^-1, the relative standard deviation of method is 1.2%-2.2%, the recovery of added iron is 96.0%- 101%, the sensitivity is 0.19 μg.mL^-l and the detection limit is 77 ng.mL^-1. The effect of the determination of iron of the standard curve method, standard addition calibration and colorimetry method was the same, but the first has the merits of rapid sample preparation, reduced contamination risks and fast analysis.

Preparation and Properties of Bio-Based Flame Retardant L-APP/Poly(L-lactic acid)Composites

Poly(L-lactic acid)(PLLA)is a thermoplastic material with complete degradability,high biocompatibility and excellent mechanical properties.It can replace petroleum-based polymers are currently being used in the fields of packaging,agriculture,textiles,medical and so on.However,PLLA’s extremely flammability greatly limits its wider application.An bio-based flame retardant L-APP/PLLA composites was prepared by melt blending of the L-APP and PLLA.The morphology,impact properties,thermal properties and flame retardant properties of composites were investigated by field emission scanning electron microscope(SEM),impact tester,differential scanning calorimeter(DSC),thermogravimetric analyzer(TGA),limiting oxygen indexer(LOI)and horizontalvertical burning tester.The results showed that the degree of crystallization(X_(c))and LOI of L-APP/PLLA composites increased as increasing of L-APP content.What’s more,the impact strength first increased and then decreased,the glass transition temperature(T_(g))and melting temperature(T_(m))do not changed significantly.The impact strength of composites was 9.1 kJ/m^(2) at a 5 wt%loading for L-APP,which was the highest level.When the content of L-APP was 20%,the LOI was 30.8%,the Xc was 42.3%and the UL-94 level was V-0.This research can promote the value-added utilization of lignin and the application of PLLA in the fields of flame retardant materials.

On-line Preconcentration and Determination of Trace Metals in Water Samples by Flow Injection Combined with Flame Atomic Absorption Spectrometry via Calix[4]arene Carboxylic Acid Packed Micro-column

An adsorbent calix[4]arene carboxylic acid was employed as the adsorption material for on-line flow in jection（FI） micro-column preconcentration coupled with flame atomic absorption spectrometry（FAAS） determination of trace heavy metals（Cu, Pb, Co, Ni and Cd）. Parameters such as the pH, loading time and flow rate of sample, and the concentration, volume and flow rate of eluent were optimized. The enrichment factors are 50.0, 56.5, 11.6, 12.1 and 19.1 for Cu, Pb, Co, Ni, and Cd, respectively, and a sample throughput of 20 h–1 was obtained. The limits of de tection for Cu, Pb, Co, Ni, and Cd were in a range of 1.56―3.91 μg/L, and the relative standard deviations（RSDs） were less than 2.76%（n=7）. Furthermore, the proposed method was successfully applied to the determination of Cu, Pb, Co, Ni, and Cd in certified reference materials and various water samples.

Halogen-Free Flame Retarded Poly(Lactic Acid)with an Isosorbide-Derived Polyphosphonate

Fabrication of flame retardants from renewable biomass has aroused extensive interest over the past decade.This work reported a synthesis of isosorbide-derived polyphosphonate(PICPP)as an anti-flammable agent for poly(lactic acid)(PLA).The presence of PICPP notably declined the storage modulus of PLA/PICPP owing to the declined molecular weight of PLA catalyzed by the presence of PICPP.PLA and PLA/PICPP thermally degraded in one stage under either air or nitrogen atmosphere.With increasing the amount of PICPP,the onset thermal decomposition temperature of PLA/PICPP was decreased gradually,owing to the earlier decomposition of PICPP.With only 10 wt%of PICPP,PLA/PICPP-10 achieved a high limiting oxygen index of 30.0%and UL-94 V-0 classification,manifesting that PICPP was an efficient anti-flammable agent for PLA.The inclusion of 15 wt%PICPP also caused 33%and 16%decline in PHRR and THR of PLA,respectively.TG-IR results clarified that PLA/PICPP produced the less typical pyrolysis products especially flammable carbonyls than PLA,which may account for the suppressed PHRR and THR values of PLA/PICPP.

Improved flame resistance properties of unsaturated polyester resin with TiO2-MXOY solid superacid

Five SO4^2-/TiO2-MXOY solid super acids(SSA:Cu@Ti:SSA,Zr@Ti:SSA,Fe@Ti:SSA,Mn@Ti:SSA,Mo@Ti:SSA)were successfully prepared by sol-gel method,and its chemical structure and element content were characterized by X-ray diffraction(XRD)analysis,Fourier transform infrared spectroscopy(FHIR)and energy dispersive spectroscopy(EDS).Then,a compound flame retardant system containing SSA and ammonium polyphosphate/montmorillonite(AM)were was introduced into an unsaturated polyester resin(UPR)to enhance the flame retardance.The effect of SSA on the flammability and thermal stability of the UPR was evaluated by the limiting oxygen index(LOI),cone calorimeter te st(CCT)and thermogravimetric analysis(TGA).The LOI results showed that the flame retardance of the UPR composites was significantly improved with the addition of SSA.Moreover,their heat release rate(HRR),total heat release(THR),the smoke production rate(SPR)and CO and CO2 yield were much decreased.In addition,the initial decomposition temperature of UPR/AM/S SA was delayed,indicating that their thermal stability was increased,and the residual char of UPR/AM/SSA was also increa sed due to strong catalytic of SSA ability for esterification and dehydration.Furthermore,the microstructure of the residual char after combustion of the UPR composites was studied by the scanning electron microscopy(SEM),and it was found that the char layer structure was more continuous and dense after the addition of the SSA.In sum up,the synergistic effect between SSA and AM was the main factor for the great improvement of flame retardant of UPR composites.

植酸铵包覆微晶纤维素的制备及结构表征

以生物基微晶纤维素(MCC)为原料,通过逐步加入三聚氰胺(MEL)和植酸(PA)对MCC进行包覆改性,制备了植酸胺包覆微晶纤维素(MEL-PA-MCC)生物基杂化结构。利用傅里叶变换红外光谱仪、热重分析仪、差示扫描量热仪、扫描电子显微镜、X射线光电子能谱仪、能谱分析仪、X射线衍射仪等对MEL-PA-MCC的结构、元素组成和形貌进行了表征。结果表明,经MEL-PA改性后的MCC分别在1624,1328,785cm^(-1)处表现出了C=N,P=O和P—O的特征吸收峰,且最大热分解速率显著降低,残炭率增加;MEL-PA-MCC杂化结构的表面密集地附着圆形颗粒,同时N,P元素明显提升,结晶行为也显著改变。上述结果共同表明植酸胺成功实现对MCC的包覆改性。利用MEL-PA-MCC对聚己二酸/对苯二甲酸丁二酯(PBAT)进行改性,当MEL-PA-MCC添加质量分数为5%时,该复合材料可达到垂直燃烧UL-94测试V-1等级,极限氧指数提高到25.5%,抗熔滴性能显著改善。此外,PBAT/5%MEL-PA-MCC复合材料的拉伸强度和拉伸弹性模量比纯PBAT分别提高了87.31%和41.30%。因此,通过引入制备的MEL-PA-MCC阻燃杂化结构可显著改善PBAT的阻燃效果、提高材料的拉伸性能。

An Approach to the Flame Retardancy of EVA Copolymer by Plasma Treatmentc2

An attempt was made in the paper aiming at imparting flame retardancy to polymers by plasma grafting technique Based on EVA copolymers with different VA contents the author tried to use the Ar plasma followed by grafting with/without subsequent saponification and metal ion exchange expediting the charring of polymers upon heationg Characterization of the flammability of the plasma treated EVA copolymers grafted with acrylic monomers(MAA,AA and AAm)indicates that this approach turns out to be a promising way and worthy doing whatever in research and/or applications

植酸基阻燃剂对泡桐木材燃烧性能和热稳定性的影响

以植酸为主要原料,分别通过层层组装法、两步法、溶胶-凝胶法3种方式,合成植酸基阻燃剂(植酸-壳聚糖全生物质阻燃剂、植酸铵-环糊精膨胀型阻燃剂、植酸铵-硅溶胶环保阻燃剂);通过表面涂覆的方式在泡桐(Paulownia)木材表面构建阻燃涂层,研究3种阻燃剂对试件点燃时间、热释放速率、总热释放量、总烟释放量、一氧化碳和二氧化碳产量、残余物质量和热稳定性的影响。结果表明:与天然木材相比,植酸铵-环糊精阻燃木材、植酸铵-硅溶胶阻燃木材的点燃时间均延长一倍以上,3种阻燃剂对降低木材的热释放速率、总热释放量、二氧化碳产量均具有促进作用,残余物质量增加量的提高超过6.89%,但总烟释放量、一氧化碳产量有所增加;阻燃木材的热分解速率明显下降,植酸-壳聚糖阻燃木材、植酸铵-环糊精阻燃木材、植酸铵-硅溶胶阻燃木材的残炭量分别提高163.24%、58.04%、121.77%,热稳定性显著提高。

A NEW SYNERGIST FOR INTUMESCENT FLAME RETARDANT POLYPROPYLENE

The synergistic effects of silicotungstic acid (SiW12) as a catalyst in the phosphorus-nitrogen compounds AM-based intumescent flame-retardant (IFR) polypropylene (PP) were studied using the limiting oxygen index (LOI), the UL-94 test, thermogravimetric analysis (TGA), real time Fourier transform infrared (FTIR), laser Raman spectroscopy (LRS). The LOI data show that SiW12 added to PP/IFR systems has a synergistic FR effect with an IFR additive named AM. The TGA data show that SiW12 apparently increases the thermal stability of the PP/IFR systems at high temperature (T > 500degreesC). The FTIR results provide the positive evidence that IFR can improve the thermal stability of PP and SiW12 can induce a higher rate of formation of phosphoric acid and its derivatives. The LRS measurements provide useful information on the carbonaceous microstructures. In short, a suitable amount of SiW12 (1.5 wt%) exerts synergistic effects with the IFR by increasing the LOI value and the thermal stability at high temperature and promoting the formation of charred structures on the burning PP surface.

Development of a Derivatization-free GC-FID Method for Evaluation of Free Fatty Acid Levels in Plasma of Diabetic Nephropathy Patients

Metabolism of free fatty acids（FFAs） is related to several important physiological events and therefore their quantitaion in biological samples arouses extensive interest and efforts.Existing gas chromatography with flame ionization detector（GC-FID） methods for the analysis of FFAs normally require derivatization of them in order to lower boiling points.But this extra procedure tends to induce additional error and it is laborious and time-consuming.A derivatization-free method was therefore established in the present investigation to determine FFAs in human plasma by capillary（GC-FID）.After extraction of FFAs from plasma,a highly polar FFAP（free fatty acid in plasma） column was employed to directly quantitate FFAs concentration,free from derivatization reaction.All sample pretreatments were carried out at room temperature,improving recovery of short-chain FFAs.Heptadecanoic acid（C17：0） was employed as internal standard,and the proposed method was validated for recovery,precision,sensitivity,stabi-lity,and linearity.Validation data show that it is suitable for clinical study that has been applied to the evaluation of FFAs levels in plasma of diabetic nephropathy（DN） patients during the course of treatment.Forty-seven patients diagnosed with DN were admitted to the double-blind experiment.Control group（n=17） underwent solely basic treatment and the patients did not show significant change in FFAs concentration during six months of treatment.Experiment group（n=30） was supplied with traditional Chinese medicine besides basic treatment.After six months of medication,their plasma concentration of palmitic acid（C16：0）,stearic acid（C18：0） and oleic acid（C18：1n-9） decreased while linolenic acid（C18：3n-3） increased significantly（P〈0.05）.These four compounds could be served as biomar-kers in the evaluation of drug efficacy,and their quantitation in plasma may provide additional information for disease progression in DN patients.

Effect of MMT on Flame Retardancy of PLA/IFR/LDH Composites

Nano filler synergistic intumescent flame retardant(IFR)system is an effective way to improve the flame retardant properties of polymer.In this study,the effects of montmorillonite(MMT)on the flame retardant properties of polylactic acid/layered double hydroxides(PLA/LDH)and PLA/IFR/LDH were investigated.The results show that both LDH and LDH/IFR can reduce the peak heat release rate(HRR)of PLA and prolong the combustion time of PLA;When a proportionate MMT is introduced into PLA/LDH and PLA/IFR/LDH systems,respectively,MMT will not only affect the degradation process of PLA composites during combustion,but also the PLA composites can form a more stable carbon layer during combustion,which could decrease the peak HRR and prolong combustion time of PLA composite.Furthermore,when 0.5 wt%MMT is incorporated,the peak HRR of LDH/IFR/LDH composite is reduced by 16.17%and the combustion time is prolonged by about 70 s.This study can provide an opportunity to further optimize the properties of intumescent flame retardant polymer.

全生物质单组份膨胀型阻燃剂的制备与性能研究实验设计

该文以生物质材料作为原料制备了单组分膨胀型阻燃剂,并将其加入聚乳酸中制备了复合材料。实验结果表明,该阻燃剂能够显著提高聚乳酸的阻燃性能和抗熔滴性能,且热稳定性良好。该实验涉及高分子材料配方设计、成型加工、性能测试、结构表征等专业知识,可使学生掌握高分子材料阻燃机理,熟练使用相关仪器设备进行测试与分析,有利于他们提高综合运用知识的能力,并针对高分子材料与工程领域的复杂工程问题设计解决方案。

植酸-胞嘧啶对DL-蛋氨酸粉尘爆燃火焰抑制特性研究

饲料及其添加剂粉尘具有较高的燃烧热,在生产过程中存在一定的爆燃风险,威胁生命财产安全,预混抑制剂是目前应用最为广泛的一种抑爆手段,但传统抑制剂不可食用,无法加入至饲料类粉尘实现抑爆。因此,以饲料主要添加剂DL-蛋氨酸(DLM)粉尘为研究对象,采用自主合成的营养价值高、绿色可食用生物质基植酸-胞嘧啶(PA-CY),研究了PA-CY对DLM粉尘爆燃火焰传播特性的影响,通过高速摄影和可视化竖直管道记录爆燃火焰传播过程并计算火焰速度,采用热电偶监测火焰温度变化。结果表明:随PA-CY质量分数的升高DLM爆燃火焰亮度持续下降,严重破坏了火焰结构,加入20%PA-CY后火焰峰值速度、平均速度和峰值温度由27.66 m/s、14.39 m/s、1014℃分别下降至13.83 m/s、6.88 m/s、540℃,下降比重达50.0%、52.2%和46.7%,且PA-CY质量分数达30%后粉尘无法被点燃,说明PA-CY抑制效果显著。此结果可为饲料类粉尘爆燃的防治提供理论支持。

二苯基磷酸改性酚醛树脂的制备及耐热阻燃性能研究

以苯酚、甲醛水溶液、二苯基磷酸为原料,制备了二苯基磷酸改性酚醛树脂(PPR)。通过傅里叶变换红外光谱(FT-IR)、核磁共振氢谱(1H-NMR)表征了PPR的结构。通过差示扫描量热法(DSC)对PPR的固化过程进行了研究,得到PPR的最佳固化工艺为100℃固化2h,130℃固化2h,150℃固化1h。通过热重分析(TG)、维卡软化点测试了PPR的耐热性能,通过极限氧指数、UL94垂直燃烧测试了PPR的阻燃性能。测试了PPR的拉伸剪切强度和冲击强度。结果表明:当二苯基磷酸用量为苯酚质量的14%时,PPR的综合性能最优,残炭率、极限氧指数、维卡软化点、拉伸剪切强度相比于普通酚醛树脂(PR)分别提高了17.4%、5%、29.5%、54.7%,UL94垂直燃烧达到V-0级。

水性丙烯酸阻燃涂料的研究进展

水性丙烯酸树脂涂料是一类近年来发展迅速的水性涂料,由于具有耐光性、耐候性、耐热性良好且环保无毒的特点,在汽车、家具、建筑等行业得到了广泛应用。其中利用水性丙烯酸树脂制备阻燃涂料的研究呈快速增长的态势,得到了木材、家具、建筑、钢材阻燃等领域有关学者的高度关注。简述了水性丙烯酸阻燃涂料的阻燃机理,从原料配比、原料种类、反应温度三方面阐述了水性丙烯酸阻燃涂料的制备工艺及其应用,并对其研究发展方向提出了建议。

界面阻燃化玻璃纤维协同聚磷酸铵增强阻燃聚乳酸

采用3-氨丙基三乙氧基硅烷(KH550)对短切玻璃纤维(GF)进行氨基化处理,得到表面富含氨基的GF-KH550,以三乙胺为缚酸剂和催化剂、POCl_(3)和4,4-二氨基二苯甲烷为反应单体,在GF-KH550表面原位聚合,获得超支化聚磷酰胺界面阻燃化玻璃纤维(GF@HBPN),采用FTIR、XPS、SEM、TGA对其进行了表征。GF-KH550、GF@HBPN单独或与聚磷酸铵(APP)作为阻燃剂用于聚乳酸(PLA)复合材料(GF-KH550/PLA、GF@HBPN/PLA、APP/GF@HBPN/PLA)的制备。对复合材料的热稳定性、力学和阻燃性能进行了测试。结果表明,与PLA相比,GF-KH550/PLA的拉伸强度明显提高,但GF的“烛芯效应”严重恶化了其燃烧性能;GF@HBPN/PLA复合材料的拉伸强度也有提高,且燃烧过程中GF表面形成的界面残炭抑制其“烛芯效应”,改善了其燃烧性能(UL-94V-2),但不足以达到理想阻燃效果。当APP质量分数10%、GF@HBPN质量分数为30%时,制备的复合材料10%APP/30%GF@HBPN/PLA的极限氧指数达到26.8%±0.2%、垂直燃烧等级为UL-94V-0级,且热释放速率峰值、总热释放量和平均有效燃烧热比PLA分别下降了31.39%、23.57%和18.80%,显示出优异的火安全性能。