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JOURNAL OF APPLIED POLYMER SCIENCE · 2024 ·Vol. 142 ·期 2 ·e56359 · IF 2.7

Lignin-based nitrogen and phosphorus-containing polylactic acid with flame-retardant performances

Guixin Zhang,Shuxian Weng,Jie Wang,Zhimin Kou,Meiting Liu,Guoqiang Zhu,Lihong Hu,Yonghong Zhou

Polylactic acid (PLA) is a new type of biodegradable material that has been applied in many fields such as extrusion, injection molding, film drawing, and spinning. In contrary, it does not have flame retardancy. In this paper, N-PCDL was synthesized by amidation reaction between  COOH of PCDL and  NH 2 of tetraethylenepentamine (TEPA), followed by an Atherton-Todd reaction of unreacted  NH 2 at the other end of TEPA with P  H of DOPO to prepare a novel lignin-based flame retardant containing nitrogen and phosphorus (NP-PCDL). The Fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic hydrogen spectroscopy ( 1 H NMR) analysis results showed that proton peaks of  CO  NH  , P  N  , and  NH  appeared in the NP-PCDL spectrum, while the characteristic absorption peak of P  H bond disappeared in DOPO, the X-ray photoelectron spectroscopy (XPS) results showed that the degraded lignin consisted of elements C and O, while NP-PCDL consisted of elements C, O, N and P. The above results indicated that NP-PCDL was successfully prepared. NP-PCDL accounted for 3% (mass percentage, the same below), 5% and 10% of PLA, then lignin based flame-retardant PLA composites were prepared by internal mixing and injection molding. Thermogravimetric analysis (TGA) showed that the residual carbon of PLA/3% NP-PCDL, PLA/5% NP-PCDL and PLA/10% NP-PCDL at 800°C were higher than that of pure PLA, with the increase of 56.56%, 97.54%, and 301.64%, respectively; The analysis of SEM, XPS, and Raman showed that PLA/NP-PCDL formed dense, regular and highly graphitized residual carbon with phosphorus nitrogen structure during the combustion process. At the same time, NH 3 , H 2 O and PO˙ free radicals were released, which could dilute combustible gases, destroy free radical chain reaction, isolate combustible gases and heat, so as to play a flame-retardant role.

CAS / MDL: 6066-82-6
研究领域: 材料科学 · 化学工程
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MATERIALS RESEARCH INNOVATIONS · 2024 · IF 0

Preparation and properties of halogen-free flame retardant PE based wood-plastic composite materials

Hongdan Hu,Yaowen Wang

The experiment carried out halogen-free flame retardant modification treatment on polyethylene-based wood-plastic composite materials. The results showed that after adding flame retardant, the ignition time of the material increased to 76 seconds, an increase of 22 seconds. At combustion temperatures above 530°C, only a small amount of the material’s residue continues to evaporate. When the temperature rises to 800°C, the difference in the residual carbon content of the samples gradually becomes larger. The residual carbon content of sample 1# is only 10.1%. At this time, the residual carbon content of samples 7#, 8# and 9# are respectively Reaching 27.12%, 27.09% and 25.60%. The above results show that the thermal stability of composite materials has been greatly improved after adding nano-flame retardants, providing new ideas and methods for the application of flame retardant and halogen-free flame retardant materials of wood-plastic composites.

CAS / MDL: 7631-86-9
研究领域: 材料科学 · 高分子化学
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JOURNAL OF ENVIRONMENTAL MANAGEMENT · 2023 · IF 8.7

Recovery of residual carbon from coal gasification fine slag by a combined gravity separation-flotation process

Bo Lv,Xiaoman Chai,Xiaowei Deng,Feishuo Jiao,Chaojun Fang,Baolin Xing

Recovering inner residual carbon is important for fully utilizing coal gasification fine slag (CGFS) resources. In this study, we adopted a combined gravity-separation and flotation process to efficiently recover residual carbon by considering the characteristics of the CGFS and optimizing the operating factors of the process. CGFS is principally a mixture of residual carbon and ash, with low-density particles containing more of the former. Accordingly, residual carbon is preliminarily enriched by gravity separation, in which gas velocity ( v g ) and water velocity ( v w ) significantly impact separation efficiency, followed by feed volume ( m ). The residual carbon in the initial concentrate was preliminarily enriched (i.e., loss on ignition ( LOI ): 55.90%; combustible recovery ( R o ): 72.36%) under appropriate operating conditions (i.e., v w  = 0.04 m/s, v g  = 3 m/s, m  = 150 g). Moreover, the quality of the flotation concentrate was most influenced by collector dosage ( m c ), followed by aeration rate ( η ), frother dosage ( m f ), stirring speed ( w ), and grinding time ( t ) during flotation of the primary concentrate. The flotation concentrate exhibited LOI and R o values of 90.95% and 50.34%, respectively, under the optimal flotation conditions (i.e., m c  = 20 kg/t, m f  = 15 kg/t, w  = 2600 rad/min, η  = 200 L/h, t  = 360 s); it has a high residual carbon content and is an ideal raw material for preparing fuels or carbon materials.

CAS / MDL: 8008-20-6
研究领域: 矿物加工工程 · 资源与环境科学
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HIGH PERFORMANCE POLYMERS · 2024 · IF 1.8

Bio-based flame retardants containing a biphenyl unit for enhancing mechanical properties and fire safety of epoxy resins

Bin Ren,Chenchen Wang,Rui Ma,Ying Huang,Xiuyun Li

A reactive flame retardant containing biphenyl structure (DEU-2DOPO) was prepared from the bio-based raw material eugenol. The incorporation of DEU-2DOPO into the epoxy resin serves to enhance the ring-opening reaction of the epoxy. Furthermore, the inclusion of DEU-2DOPO has been found to have a positive impact on the glass transition temperature and residual carbon rate of the epoxy resin. This additive also significantly improves the mechanical properties of the epoxy resin, leading to a 49.3% increase in tensile strength, an 81.9% increase in breaking elongation, and a 15.8% increase in flexural strength. Notably, when DEU-2DOPO is introduced at a concentration of 5 wt%, it not only achieves a V-0 rating in the UL-94 test but also exhibits an impressive ultimate oxygen index of 34.5%. Additionally, the cone calorimetric testing revealed that the presence of DEU-2DOPO results in lower combustion metrics compared to pure epoxy, as evidenced by a reduction of 15.1% in total heat release (THR) and 10.8% in total smoke release (TSR). An analysis of the flame retardant mechanism elucidates that DEU-2DOPO promotes the formation of a stable and dense residual carbon, thereby impeding gas and heat exchange. Furthermore, the decomposition of DEU-2DOPO generates PO· and PO2· radicals, which effectively neutralize reactive radicals.

研究领域: 材料科学 · 化学工程
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MOLECULES · 2021 ·Vol. 26 ·期 20 ·6116 · IF 4.412

Synthesis of Porous Material from Coal Gasification Fine Slag Residual Carbon and Its Application in Removal of Methylene Blue

Yixin Zhang,Rumeng Wang,Guofeng Qiu,Wenke Jia,Yang Guo,Fanhui Guo,Jianjun Wu

A large amount of coal gasification slag is produced every year in China. However, most of the current disposal is into landfills, which causes serious harm to the environment. In this research, coal gasification fine slag residual carbon porous material (GFSA) was prepared using gasification fine slag foam flotation obtained carbon residue (GFSF) as raw material and an adsorbent to carry out an adsorption test on waste liquid containing methylene blue (MB). The effects of activation parameters (GFSF/KOH ratio mass ratio, activation temperature, and activation time) on the cation exchange capacity (CEC) of GFSA were investigated. The total specific surface area and pore volume of GSFA with the highest CEC were 574.02 m2/g and 0.467 cm3/g, respectively. The degree of pore formation had an important effect on CEC. The maximum adsorption capacity of GFSA on MB was 19.18 mg/g in the MB adsorption test. The effects of pH, adsorption time, amount of adsorbent, and initial MB concentration on adsorption efficiency were studied. Langmuir isotherm and quasi second-order kinetic model have a good fitting effect on the adsorption isotherm and kinetic model of MB.

研究领域: 环境科学 · 材料科学 · 化学工程
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JOURNAL OF WUHAN UNIVERSITY OF TECHNOLOGY-MATERIALS SCIENCE EDITION · 2025 ·Vol. 40 ·期 4 ·946-952 · IF 1.1

New DOPO-based Flame Retardants: Synthesis and Flame-retardant Properties of Modified Epoxy Resin

Guo Jiahua,Wei Tao,Huagn Zhixiong,Deng Zongyi,Shi Minxian

We aimed to enhance the flame retardancy of epoxy resin (EP) by synthesizing a novel, halogen-free flame retardant through a one-pot method. The synthesis utilized 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), furfurylamine (FA), and benzene propionaldehyde (BPA) as raw materials. We conducted differential scanning calorimetry (DSC) analysis to investigate the effects of FPD on the curing process and thermal properties of EP. Our findings reveal that incorporating FPD into EP can facilitate a faster curing process and increase the carbon residue post-combustion. Specifically, the FPD/EP-7 composite demonstrates a limiting oxygen index (LOI) of 34.9% and achieves a UL-94V-0 rating with a phosphorus content of 0.91wt%. These results indicate that FPD significantly enhances the thermal stability and charring rate of EP, thereby improving its flame retardancy. Although the addition of FPD slightly reduces the mechanical properties of EP, the composite material maintains excellent performance.

研究领域: 材料科学 · 高分子科学 · 消防安全工程 · 化学合成
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JOURNAL OF HAZARDOUS MATERIALS · 2021 · IF 10.588

Conversion of phenolic mixture to refractory resins: A resourcezation strategy for phenolic distillation residues

Jing Zhou,Xingang Li,Jinze Du,Lin He,Chengyang Wang,Hong Sui

A new resourcezation way has been proposed to address the treatment challenges of the light phenolic distillation residue (LPDR) from the coal-based phenolic distillation residue. Herein, the LPDR, which was collected at 20 kPa and 220 °C from the phenolic distillation residue, has been further used to synthesize the phenolic resin (named as RPF) for MgO-C refractories. It is found that the conversion efficiency of crude phenol mixture to RPF is 71.3%, which is lower than that of pure phenol. To increase the conversion efficiency and improve the properties of RPF, the crude phenolic mixture was blended with pure phenol for the synthesis. The optimal addition mass ratio of phenol in the crude phenol mixture (phenol/total phenolic compounds) is determined to be 0.8, where the obtained RPF could satisfy or even better than the national standard. Further addition of 10 wt% of urotropine (HMTA) as curing agent and 9 wt% of ferrocene (Fc) as modifier (named as MRPF) are found to significantly improve the graphitization of RPF. Under these conditions, the DTG at temperature of maximum mass lose rate (T max ) of MRPF was lower than that of commercial resin. The graphitization level was as high as 61.6% with the residual carbon rate up to 41.4%, which are higher than those of national standard. These findings provide insights for the resourcezation of the phenolic distillation residue.

CAS / MDL: 108-68-9
研究领域: 化学工程 · 材料科学 · 环境科学
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ENERGY · 2023 · IF 9

Stable and highly efficient HMDS terminated m-Cresol inhibitor for inhibiting coal spontaneous combustion

Wei Lu,Ao Gao,Yuntao Liang,Zhenglong He,Jinliang Li,Yong Sun,Shuanglin Song,Shaocong Meng

A stable and highly efficient 1, 1, 3, 3, 3-hexamethyldisilazane (HMDS) terminated m-Cresol inhibitor was synthesized based on the protection-deprotection strategy. The inhibitory effect of HMDS terminated m-Cresol inhibitor on spontaneous combustion of lignite was explored through temperature-programmed oxidation tests, in-situ infrared analysis and thermogravimetric analysis. Results show that, the oxidation of active phenolic hydroxyl groups in the m-Cresol inhibitor can be hindered by the protection of HMDS. After encountering coal, the HMDS terminated inhibitor can be gradually deprotected to regenerate the m-Cresol inhibitor that contains massive active phenolic hydroxyl groups, thus improving the chemical inhibition efficiency of coal spontaneous combustion. For the coal sample inhibited with HMDS terminated m-Cresol inhibitor, the initial contents of the active functional groups are lower and more stable during heating, and the inhibition rate reaches 70% at 130 °C. Moreover, the crossing-point temperature rises by 32.4 °C–181.2 °C. The activation energy increases by 11 kJ/mol and 18 kJ/mol at below and above 130 °C respectively. The peak temperature at maximum weight loss rate rises by 65 °C–431.2 °C, and the corresponding residual carbon rate increased by 31.3%–61.6%. The inhibition mechanism of the HMDS terminated m-Cresol inhibitor on coal spontaneous combustion was deduced.

CAS / MDL: 108-39-4
研究领域: 化工工程 · 材料科学 · 煤化学 · 热分析
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