MACROMOLECULAR MATERIALS AND ENGINEERING
·
2021
·Vol. 306
·期 12
·2100569
·
IF 4.367
Junjun Zhang,Huajun Duan,Jiahao Zou,Jianfan Cao,Chao Wan,Chenhao Zhang,Huiru Ma
In order to eliminate the negative effect of traditional 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) -based flame retardants on heat resistance, mechanical properties, and curing process of epoxy resin (EP), a DOPO derivative (DST) constructed by sulfaguanidine and thiophene is designed and used as co-cured agent for EP. Compared with EP, the maximum decrease of glass transition temperature ( T g ) in all EP/DST samples is less than 5%, indicating EP modified by DST maintains good heat resistance. Encouragingly, DST shows satisfactory flame-retardant efficiency and excellent smoke suppressing effects. EP containing barely 5 wt% of DST (P content: 0.37 wt%) achieves a UL-94 V-0 rating and 32.8% limited oxygen index (LOI) value. Its peak heat release rate (PHRR), total heat release (THR), and total smoke production (TSP) are also decreased by 31.2%, 18.8%, and 30.2% . Further, DST significantly improves mechanical properties of the EP/DDM/DST system. The tensile strength and modulus increase by 37.2% and 14.6%, respectively, as DST content is 7.5 wt%. It is revealed that DST has positive quenching and diluting effects in the gas phase, as well as promoting the formation of a compact char layer in the condensed phase.
研究领域:
材料科学
·
化学工程
✓ 已验证
产品关联
DOI
高影响因子
POLYMER DEGRADATION AND STABILITY
·
2025
·
IF 7.4
Wei Liu,Xiaosui Chen,Yipei Zhang,Yuhang Huang,Shuzheng Liu,Aiqing Zhang,Shengchao Huang
To develop multifunctional epoxy (EP) composites integrating good flame retardancy, suitable mechanical performance, and superior antibacterial properties, a nanosphere-shaped flame retardant (PDA@KH560-DOPO) was fabricated by grafting 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) onto polydopamine (PDA) nanospheres via the bridging of silane coupling agent KH560. This additive exhibited two distinct degradation stages with low maximum degradation rates (1.79 and 1.52 %/min) and high charring ability (58.6 % at 700°C) under N 2 atmosphere. The EP composite containing 8 % PDA@KH560-DOPO achieved a limited oxygen index (LOI) of 31.8 % and a UL-94 V-0 rating, while maintaining good tensile and impact properties comparable to neat EP. The cone calorimeter test showed reductions in peak heat release rate (PHRR), total heat release (THR), and total smoke production (TSP) by 48.1, 32.1, and 19.0 % respectively. This is attributed to the cooperative flame-retarding mechanisms combining staged free-radical scavenging (phenoxy and P-containing radicals), inert gas dilution, and a reinforced char barrier (18.1 wt% in cone calorimeter test). Crucially, the composite also exhibited potent antibacterial activity, with over 94 % inhibition rate against Gram-positive bacteria (S. aureus). This work provides a practical pathway for expanding the applications of EP composites into domains that require fire-safe and hygienic standards.
研究领域:
高分子材料科学
·
阻燃化学
·
表面功能化
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生物医学材料
·
纳米复合材料
✓ 已验证
产品关联
DOI
高影响因子
CHEMICAL ENGINEERING JOURNAL
·
2024
·
IF 13.3
Ze-Tao Xiao,Guan-Long Wu,Tian-Mo Yang,Yu Li,Yuan Hu,Manfred Döring,Xin Wang
The flammability and brittleness of the diglycidyl ether of bisphenol A (DGEBA)-type epoxy resin greatly restrict its application in electronic appliances and structural materials. However, the synchronous improvement in the flame retardancy, mechanical strength, and toughness of DGEBA-type epoxy thermosets remains a significant challenge. To overcome this challenge, in this study, a sustainably sourced and DOPO-derived triol (DOPO-GL-DCDA) was synthesized from a bio-based material, glycerol 1, 3-diglycerolate diacrylate (GL-DCDA). A series of epoxy thermosets with different phosphorus contents were prepared by introducing DOPO-GL-DCDA into the DGEBA matrix. EP/DOPO-GL-DCDA demonstrated excellent flame retardancy and mechanical properties without compromising transparency. Specifically, EP/DOPO-GL-DCDA-1.0P exhibited a limit oxygen index (LOI) of 34.0 % and a UL-94 V-0 rating, and the total heat release (THR) and peak heat release rate (PHRR) of EP/DOPO-GL-DCDA-1.5P decreased by 36.6 % and 46.8 %, respectively, compared with those of pure EP. In addition, compared with those of pure EP, the tensile strength, impact strength, fracture toughness (K IC ), and fracture energy (G IC ) of EP/DOPO-GL-DCDA-1.5P increased by 62.8 %, 69.9 %, 62.9 %, and 99.0 %, respectively. Moreover, EP/DOPO-GL-DCDA had better dielectric properties than pure EP. Under the premise of maintaining transparency, this work provided a promising solution to synchronously improve the flame retardancy, mechanical strength, and toughness of epoxy thermosets.
研究领域:
材料科学
·
化学工程
✓ 已验证
产品关联
DOI
高影响因子
POLYMERS FOR ADVANCED TECHNOLOGIES
·
2024
·Vol. 35
·期 4
·e6358
·
IF 3.1
Qinqin Luo,Yulin Sun
A novel organic salt containing DOPO and pyrimidine (AD) was successfully synthesized through a simple acid–base neutralization reaction. The salt was used as a reactive flame retardant for epoxy resin. Non-isothermal DSC tests disclosed that the epoxy resin displayed a lower temperature of onset curing and exothermic peak in the presence of AD. By using only 3 wt% AD, the epoxy resin achieved a UL-94 V-0 rating and a limited oxygen index value of 27.4%, revealing the high flame-retardant efficiency of AD. AD inhibited the release of heat and smoke. The analysis of the flame-retardant mode of action indicated that AD was able to impede combustion not only by the dilution and quenching effects in the gas phase but also by the charring effect in the condensed phase. During UL-94 testing, 3 wt% AD gave the epoxy resin good flame retardancy due to the charring and blowing-out effects formed by adding AD. The blowing-out effect was that the release of strong airflows suppressed or even blew out the flame based on the dilution and quenching effects of phosphorous-containing radicals and numerous non-combustible gases produced by the degradation of AD and epoxy resin matrix. Additionally, the incorporation of AD slightly increased the glass transition temperature and the tensile and flexural strengths of the epoxy resin. This study provided a meaningful attempt to improve the flame retardance of epoxy resin by introducing a reactive pyrimidine-organophosphonic acid salt.
研究领域:
材料科学
·
化学工程
✓ 已验证
DOI
高影响因子
JOURNAL OF APPLIED POLYMER SCIENCE
·
2021
·Vol. 139
·期 17
·52036
·
IF 3.125
Jiahao Zou,Huajun Duan,Junjun Zhang,Jianfan Cao,Chenhao Zhang,Chao Wan,Huiru Ma
In order to comply with the environmentally friendly flame retardant requirements of epoxy resin and strive to maintain the comprehensive performance of the epoxy resin matrix, a P/N/S-containing heterocyclic halogen-free reactive flame retardant (VAP) was constructed. Vanillin (VA), 2-amino-5-mercapto-1,3,4-thiadiazole, and 9,10-dihydro-9-oxa-10-phosphaphenanthrene10-oxide (DOPO) were chosen as raw materials to prepare VAP through a simple one-pot reaction. The addition of VAP slightly decreased the curing activity of the system while the transparency of the samples was maintained well. Moreover, the maximum degradation rate of VAP modified samples dropped by 47.26% and the amount of char residue at 800°C increased. When 10 wt% VAP (0.66 wt% P) was added, EP-10 passed UL-94 V-0 rating and the limited oxygen index value reached 30.3%. In contrast to pure EP, the peak heat release rate, total heat release, and total smoke production of EP-10 were reduced by 36.87%, 25.61%, and 29.07%, representing good smoke and heat suppression effect. Besides, the glass transition temperature ( T g ) of the samples remained above 165°C, showing a slight drop. Due to the existence of heteroatoms and the introduction of heterocyclic structure, the enhancement of intermolecular force in the system counteracted the deterioration of mechanical properties caused by the reduction of crosslinking density, maintaining the excellent mechanical properties of epoxy resin.
研究领域:
材料科学
·
化学工程
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF APPLIED POLYMER SCIENCE
·
2023
·Vol. 140
·期 36
·e54373
·
IF 3
Zhengbiao Liu,Yijun Zhang,Zhiwei Jia,Hua Liu,Zuozhen Liu
9,10-dihydro-9-oxo-10-phosphaphenanthrene-10-oxide (DOPO) and special tetra functional epoxy resin (EP) AG-601 were combined to synthesize a reactive flame retardant (FREP) and then incorporated into EP, obtaining the flame retardant material EP/FREP. To achieve EPs with higher flame retardancy and mechanical properties, a new intrinsically flame retardant EP system named EP/FRDM was produced by modifying EP/FREP with high thermal resistance bismaleimide (BDM). In the presence of a distinct FRDM structure comprising phosphaphenanthrene/nitrogen, the EP possessed superior flame retardancy and impact toughness. The curing process of EP/FRDM was investigated using Real-Time Fourier-transform Infrared. In terms of fire performance, the limiting oxygen index of the EP/FRDM-3 was raised from 31.4% to 38.2%, and the vertical burning rating was improved after BDM was added to the EP/FREP system. It was discovered that EP/FRDM exhibited a classic two-phase flame retardant influence by analyzing the residual carbon morphology and pyrolysis behavior. Simultaneously, the glass transition temperature ( T g ) of EP/FRDM remained essentially stable, and the char residue yield rose markedly, which indicated that the system had outstanding thermal stability, according to the results of the dynamic mechanical analysis and thermogravimetric analysis tests. Notably, the EP/FRDM experienced an internal chain expansion reaction when BDM was added, giving flame retardant materials excellent flexural and impact strengths and promising future application opportunities.
研究领域:
材料科学
·
化学工程
✓ 已验证
产品关联
DOI
高影响因子
POLYMER DEGRADATION AND STABILITY
·
2025
·
IF 7.4
Mingxing Wang,Zhaoqi Zhu,Chenchen Cheng,Hanxue Sun,Jiyan Li,Rui Jiao,An Li
The development of new materials with heat-insulating and flame-retardant properties is particularly important in the development of various fields such as construction, electric power, transportation, and aerospace. In this study, two kinds of conjugated microporous polymer (CMPs) nanospheres with hollow structures (H CMPs) were prepared by Sonogashira-Hagihara cross-coupling reaction using 1,3,5-triethynylbenzene and 1,4-diethynylbenzene as the monomers and SiO 2 nanospheres as the hard templates, respectively. Then 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide (DOPO) and chitosan (CTS) were loaded on the surface of H CMPs using a layer-by-layer assembly method to obtain the composite flame retardant H CMPs@CTS@DOPO. H CMP1@CTS@DOPO, H CMP2@CTS@DOPO and ammonium polyphosphate (APP) were introduced into the flammable epoxy resin (EP) in different ratios to obtain EP1, EP2, EP3, EP4 and EP5, which were compared with pure EP to evaluate their thermal insulation and flame retardant properties. The thermal conductivity of EP2, EP3 was measured to be 0.0359 W m -1 K -1 and 0.0170 W m -1 K -1 , respectively, which has excellent thermal insulation performance. The peak heat release rate (pHRR) of EP4, EP5 was reduced by 57.3 % and 64.8 %, and the peak CO 2 production (CO 2 P) was reduced by 72.7 % and 77.3 %, respectively, compared with that of pure EP, as measured by conical calorimetry (CC), which has an excellent flame retardant effect. Therefore, H CMPs@CTS@DOPO, as a new class of heat-insulating and flame-retardant materials, has great potential for application in the fields of construction, electronics and transportation.
研究领域:
材料科学
·
化学工程
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF COLLOID AND INTERFACE SCIENCE
·
2022
·
IF 9.965
Xin Jiang,Fukai Chu,Xia Zhou,Xingjun Li,Pengfei Jia,Xiaoyu Luo,Yuan Hu,Weizhao Hu
It’s known that the application of bismaleimide resins (BMI) is limited due to its brittleness and poor flame retardancy. A novel type of BMI monomer (MADQ) based on the typical phosphorus series flame retardant DOPO is designed to improve the fire safety of BMI. Besides, aliphatic long chain structure is introduced in MADQ, which is supposed to be conducive to reducing the rigidity of the BMI cross-linked network and thus to improve the toughness of BMI. It’s seen that with the incorporation of 5.24 wt% MADQ, the peak of heat release rate (PHRR) and total heat release (THR) of resultant BMI/MADQ-5 is reduced by 37.7% and 33.9%, respectively. Meanwhile, with modification of 1.07 wt% MADQ, BMI/MADQ-1 possesses UL-94V-0 rating. The relevant mechanism analysis reveals that the phosphaphenanthrene group in MADQ can exert flame retardancy effect both in condensed and gas phase. Besides, the impact strength of the BMI/MADQ is maximally increased by nearly 90.1%. Furthermore, the BMI/MADQ still maintains high tensile strength and thermal stability, which indicates the modification of MADQ did not deteriorate other properties of BMI. An innovative research idea and research basis for the preparation of intrinsic flame-retardant and toughened BMI is provided in this work.
研究领域:
材料科学
·
高分子化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2022
·
IF 8.025
Xinyu Lu,Xiaoli Gu
In this study, lignin-based epoxy resins (EP) were fabricated using lignin, phenol and glyoxal as crosslinking reagents. For improving the flame retardancy, a bi-DOPO compound with bi-hydroxyl structure was successfully synthesized, containing excellent quenching and charring capacities. Good pyrolysis behaviors of as-synthesized flame retardant resulted in significant quenching effect via structure decomposition to release PO and PO 2 free radicals for capturing reactive H and OH radicals produced from epoxy combustion. With addition of 0.18 wt% phosphorus, epoxy composite (10% LPG-ER-4) passed V-0 rating with high limited oxygen index (LOI) value of 35.2%. Cone calorimeter tests showed that heat release (including heat release rate (HRR) and total heat release (THR)) from combustion was reduced with assistance of flame retardant. Char residue analyses illustrated that bi-hydroxyl structure in DOPO-based flame retardant benefited the formation of char layer with higher compactness and integrity to serve as a protective shell of interior epoxy matrix. Furthermore, exterior pore size of char residue was narrowed or blocked to avoid the release of heat and volatiles generated from combustion. This study provided a feasible method to improve flame retardancy of lignin-based EP and proposed flame-retardant mechanism both in gaseous and solid phases.
研究领域:
材料科学
·
化学工程
✓ 已验证
产品关联
DOI
PubMed
高影响因子
POLYMER DEGRADATION AND STABILITY
·
2024
·
IF 6.3
Ruiyang Cheng,Hao Chen,Yuhan Chen,Chunhui Shen,Shanjun Gao
In this study, a phosphorus-nitrogen flame retardant (DOPO-DABP) was synthesized by 9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 4,4′-diaminobenzophenone (DABP). Then, polylactic acid (PLA), polybutylene adipate terephthalate (PBAT), ammonium polyphosphate (APP), DOPO-DABP, Joncryl ADR-4370F(ADR), azodicarbonamide (ADC) and nano-SiO 2 were used as raw materials to prepare flame-retardant modified PLA foamed materials by hot pressing. The synergistic effect of APP and DOPO-DABP not only effectively improves the flame retardancy of PLA foamed material, but also promotes their mechanical properties. The experimental results showed that when APP/DOPO-DABP=10/10, the vertical combustion grade (UL-94) of the material reached the V-0 level, the limiting oxygen index (LOI) was 34.4 %. The tensile strength of the material was 25.35 MPa, bending strength was 32.14 MPa. The cell diameter of the material was reduced to 46.72 μm, and the cell density of the material was 2.25×10 6 /cm 3 .
研究领域:
材料科学
·
高分子化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF WUHAN UNIVERSITY OF TECHNOLOGY-MATERIALS SCIENCE EDITION
·
2025
·Vol. 40
·期 4
·946-952
·
IF 1.1
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
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF APPLIED POLYMER SCIENCE
·
2025
·
IF 2.8
Ke Liu,Junjie Qu,Yanfei Zhou,Yanlu Sun,Bohan Liang,Junming Dai,Wenxing Chen,Wangyang Lu
To enhance the flame retardancy of polyamide 66 (PA66), this study developed a macromolecular flame retardant (PA–DDP) using nylon 66 salt and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DDP). The mechanical property, flame retardancy, and flame retardant mechanism of flame retardant PA66 (FRPA66) were characterized. In a vertical combustion test, FRPA66 with a P concentration of 4000 ppm performs well in terms of flame retardancy, receiving a V-0 grade (UL-94). The cone calorimeter results indicate significantly lower heat release of FRPA66 than from pure PA66. The peak heat release rate and total heat release of FRPA66 with 6000 ppm P are 47.8% and 21.5% lower, respectively, than those of PA66. Moreover, PA–DDP exhibits flame retardant properties in gas and condensed phases. Phosphorus-containing radicals in the pyrolysis product of PA–DDP capture active radicals, thereby interrupting the combustion chain reaction and playing a flame-retardant role in the gas phase. The break of the P–C bond in PA–DDP promotes the droplet drop to carry away heat of combustion timely in the condensed phase, rather than forming a carbon layer to cut off heat transfer and oxygen supply.
研究领域:
高分子科学
·
材料工程
·
消防安全工程
·
化学合成
✓ 已验证
产品关联
DOI
高影响因子