以ε-CL-20(六硝基六氮杂异伍兹烷)为主体炸药,三元乙丙橡胶(EPDM)为胶粘剂,采用喷雾干燥法制备了ε-CL-20基PBX(聚合物粘接炸药)。研究结果表明:通过喷雾干燥法可使EPDM成功包覆在CL-20晶体表面,制得的包覆产物为ε-CL-20/EPDM复合炸药...以ε-CL-20(六硝基六氮杂异伍兹烷)为主体炸药,三元乙丙橡胶(EPDM)为胶粘剂,采用喷雾干燥法制备了ε-CL-20基PBX(聚合物粘接炸药)。研究结果表明:通过喷雾干燥法可使EPDM成功包覆在CL-20晶体表面,制得的包覆产物为ε-CL-20/EPDM复合炸药;与细化CL-20相比,ε-CL-20/EPDM的撞击感度明显降低,包覆样品的特性落高(H50)值从25.12 cm升至41.36 cm,表观活化能由182.58 k J/mol增至230.24 k J/mol,热爆炸临界温度由244.18℃增至245.60℃,说明ε-CL-20/EPDM复合炸药的热稳定性更好。展开更多
In order to improve the thermal stability of condensed polynuclear aromatic(COPNA) resin synthesized from vacuum residue, 1,4-benzenedimethanol was added to cure COPNA resin. The curing mechanism was investigated by p...In order to improve the thermal stability of condensed polynuclear aromatic(COPNA) resin synthesized from vacuum residue, 1,4-benzenedimethanol was added to cure COPNA resin. The curing mechanism was investigated by proton nuclear magnetic resonance spectrometry, solid carbon-13 nuclear magnetic resonance spectrometry and Fourier transform infrared spectroscopy. Microstructures of the uncured and the cured COPNA resins were studied by scanning electron microscopy and X-ray diffractometry. The thermal stability of COPNA resins before and after curing was tested by thermogravimetric analysis. The element composition of the cured COPNA resin heated at different temperatures was analyzed by an element analyzer. The results showed that the uncured COPNA resin reacted with the cross-linking agent during the curing process, and the curing mechanism was confirmed to be the electrophilic substitution reaction. Compared with the uncured COPNA resin, the cured COPNA resin had a smooth surface, well-ordered and streamlined sheet structure with more crystalline solids, better molecular arrangement and orientation. The weight loss process of the uncured and cured COPNA resins was divided into three stages. Carbon residue of the cured COPNA resin was 41.65% at 600 ℃, which was much higher than 25.02% of the uncured COPNA resin, which indicated that the cured COPNA resin had higher thermal stability.展开更多
Thermal stability and curing kinetics of polycarbosilane (PCS) fibers were studied by thermogravimetry (TG), Fourier transform infrared spectroscopy(FT-IR). Curing is an essential step in the preparation of SiC fibers...Thermal stability and curing kinetics of polycarbosilane (PCS) fibers were studied by thermogravimetry (TG), Fourier transform infrared spectroscopy(FT-IR). Curing is an essential step in the preparation of SiC fibers and the properties of SiC fibers are affected greatly by curing conditions. TG measurement performed in air shows that mass gain starts at approximately 200℃ and PCS fibers are sensitive to oxygen. Curing with oxygen, which results in crosslinking on the surface, enabled PCS fibers to retain its shape during high-temperature pyrolysis. The curing of PCS fibers is oxidation of Si─H and Si─CH3, then Si─O─Si and Si─O─C bonds are formed. This is a first order reaction, with activation energy of 79.27 kJ/mol, and the pre-exponential factor is calculated as 3.07×106. The kinetics model was obtained and the experimental data of PCS fibers show good agreement with the kinetics model.展开更多
Novel titanium-doped silicone resins were synthesized from low-cost silane monomers and tetrabutyl titanate as raw materials and hydrochloric acid as catalyst, with titanium element as dopant into principal chain of S...Novel titanium-doped silicone resins were synthesized from low-cost silane monomers and tetrabutyl titanate as raw materials and hydrochloric acid as catalyst, with titanium element as dopant into principal chain of Si-O-Si. The resins were characterized by means of FTIR, IH NMR and 13C NMR spectra, their thermal properties and curing properties were investigated and their corresponding films were determined. The results show that the thermal stability and storage stability of the resins were influenced by the types of silane monomers containing dif- ferent carbon atomicities of organic group. The thermal stability of the titanium-doped silicone resin with a molar ratio of silane monomer B(n-propyl triethoxysilane) to silane monomer C(n-octyl triethoxysilane) being 1:1 is superior to that of the resin with a molar ratio of silane monomer B to silane monomer C being 1:3. However, the storage stability of the former is inferior to that of the latter. This work also showed that the synthesized titanium-doped silicone resins have the highest thermal stability up to 450--500℃ with an atomicity molar ratio of 1:4 of titanium to silicon in the reactants. But the best storage stability of the resin prepared from the reactants with an atomicity molar ratio of 1:6[n(Ti):n(Si)] was obtained. The effect of the type and content of curing agent on the curing properties of the resin was also studied. Moreover, thermal mechanism and curing mechanism were proposed in this work.展开更多
Synergistic effects of layered double hydroxide (LDH) with intumescent flame retardanct (IFR) of phosphorusnitrogen (NP) compound in the polypropylene/ethylene-propylene-diene/IFR/LDH (PP/EPDM/IFR/LDH) nanocom...Synergistic effects of layered double hydroxide (LDH) with intumescent flame retardanct (IFR) of phosphorusnitrogen (NP) compound in the polypropylene/ethylene-propylene-diene/IFR/LDH (PP/EPDM/IFR/LDH) nanocomposites and related properties were studied by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), limiting oxygen index (LOI), UL-94 test, cone calorimeter test (CCT) and thermo-gravimetric analysis (TGA). The XRD and TEM results show that the intercalated and/or exfoliated nanocomposites can be obtained by direct melt-intercalation of PP/EPDM into modified LDH and that LDH can promote the IFR additive NP to disperse more homogeneously in the polymer matrix. The SEM results provide positive evidence that more compact charred layers can be obtained from the PP/EPDM/NP/LDH sample than those from the PP/EPDM/LDH and PP/EPDM/NP samples during burning. The LOI and UL-94 rating tests show that the synergetic effects of LDH with NP can effectively increase the flame retardant properties of the PP/EPDM/NP/LDH samples. The data from the CCT and TGA tests indicate that the PP/EPDM/NP/LDH samples apparently decrease the HRR and MLR values and thus enhance the flame retardant properties and have better thermal stability than the PP/EPDM/LDH and PP/EPDM/NP samples.展开更多
Aim of present work is to replace asbestos in thermal insulation by another percentage of non-toxic fillers such as silica. Different formulations of fillers were prepared and added to Nordel (Trade name assigned for ...Aim of present work is to replace asbestos in thermal insulation by another percentage of non-toxic fillers such as silica. Different formulations of fillers were prepared and added to Nordel (Trade name assigned for ethylene, propylene and 1, 4-hexadiene elastomers). The physical and mechanical properties (after and before aging), and thermal properties of the prepared samples were investigated. The objective was to choose a new formulation with properties that resemble as closely as possible those of the originally used in thermal insulation. After measuring the properties of tensile strength, elongation, hardness, specific gravity, compression set, rebound resilience, thermal conductivity, and initial and final decomposition temperatures, the sample that had values very close to those of the originally used in thermal insulation was chosen and recommended to be used. From comparison it was found that EPDM rubber with 50% silica gave the optimum properties closest to the originally used.展开更多
A kind of catalyst, ammonium molybdate was developed in this paper to promote the curing reaction of bisphthalonitrile resins with aromatic amine as curing agent, and the catalytic effect was studied by differential s...A kind of catalyst, ammonium molybdate was developed in this paper to promote the curing reaction of bisphthalonitrile resins with aromatic amine as curing agent, and the catalytic effect was studied by differential scanning calorimetry (DSC), rheometric measurements and thermogravimetric analysis (TGA). The results indicated that the catalyst could improve the curing rate and increase the curing degree, which could be regulated by the content of the catalyst used in the reaction.展开更多
The curing behavior of diglycidyl ether of bisphenol-A(DGEBA) with aromatic diamide-diimide-diamines having aryl ether,sulfone and methylene linkages was studied by differential scanning calorimetry(DSC).Nine diamide-...The curing behavior of diglycidyl ether of bisphenol-A(DGEBA) with aromatic diamide-diimide-diamines having aryl ether,sulfone and methylene linkages was studied by differential scanning calorimetry(DSC).Nine diamide-diimide-diamines of varying structure were synthesized by reacting 1 mole of dianhydride with 2 moles of L-cysteine(S) in a mixture of acetic acid and pyridine(3:2 V/V) followed by activation with thionyl chloride(SOCl_2) and then condensation with excess of diamines.Structural characterization...展开更多
In this work,Epoxidized natural rubber/sawdust short fiber(ENR-50/SD)composites at different fiber content(5,10,15 and 20 phr)and size(fine size at 60–100μm and coarse size at 10–20 mm)were prepared using two-roll ...In this work,Epoxidized natural rubber/sawdust short fiber(ENR-50/SD)composites at different fiber content(5,10,15 and 20 phr)and size(fine size at 60–100μm and coarse size at 10–20 mm)were prepared using two-roll mill and electrical-hydraulic hot press machine respectively.Curing characteristics,water uptake,tensile,morphological,physical,and thermal properties of the composites were investigated.Results indicated that the scorch time and cure time became shorter whereas torque improved as SD content increase.Though the decline of tensile strength and elongation at break values,modulus,hardness and crosslinking density have shown enhancements with the increasing of SD content.The water uptake percentage of all samples has shown an increasing as SD content increase.However,the low SD content,particularly fine size have presented lower water uptake.The temperature of weight%loss(5 and 50 wt%loss)of 5 phr SD(low content)have recorded higher temperature compared to 20 phr SD(high content)in the rubber composites,which indicated higher thermal stability.The fine size of SD has recorded better overall properties than SD coarse size at same loading in the rubber composites.展开更多
Technological aspects of modifying the operational characteristics of cold cured silicate rubbers have been developed. The effect of chromium oxide on the resistance of cold-curing silicone compounds to thermal aging,...Technological aspects of modifying the operational characteristics of cold cured silicate rubbers have been developed. The effect of chromium oxide on the resistance of cold-curing silicone compounds to thermal aging, as well as on the physic mechanical properties and dielectric characteristics has been studied. The various content of ultrafine chromium oxide in cold-cured silicone compositions has been investigated, it’s optimal content in an amount of 2 - 5 mass at 100 mass, including low molecular weight rubber. Chromium oxide has been proven to improve the thermal stability of cold-cured silicone compositions. The manufacturing technology and component composition of the composition with high performance.展开更多
文摘以ε-CL-20(六硝基六氮杂异伍兹烷)为主体炸药,三元乙丙橡胶(EPDM)为胶粘剂,采用喷雾干燥法制备了ε-CL-20基PBX(聚合物粘接炸药)。研究结果表明:通过喷雾干燥法可使EPDM成功包覆在CL-20晶体表面,制得的包覆产物为ε-CL-20/EPDM复合炸药;与细化CL-20相比,ε-CL-20/EPDM的撞击感度明显降低,包覆样品的特性落高(H50)值从25.12 cm升至41.36 cm,表观活化能由182.58 k J/mol增至230.24 k J/mol,热爆炸临界温度由244.18℃增至245.60℃,说明ε-CL-20/EPDM复合炸药的热稳定性更好。
基金supported by the National Natural Science Foundation of China(51172285 and 51372277)the Fundamental Research Funds for the Central Universities(14CX02060A,15CX02084A)the Natural Science Foundation of Shandong Province(ZR2011EL030)
文摘In order to improve the thermal stability of condensed polynuclear aromatic(COPNA) resin synthesized from vacuum residue, 1,4-benzenedimethanol was added to cure COPNA resin. The curing mechanism was investigated by proton nuclear magnetic resonance spectrometry, solid carbon-13 nuclear magnetic resonance spectrometry and Fourier transform infrared spectroscopy. Microstructures of the uncured and the cured COPNA resins were studied by scanning electron microscopy and X-ray diffractometry. The thermal stability of COPNA resins before and after curing was tested by thermogravimetric analysis. The element composition of the cured COPNA resin heated at different temperatures was analyzed by an element analyzer. The results showed that the uncured COPNA resin reacted with the cross-linking agent during the curing process, and the curing mechanism was confirmed to be the electrophilic substitution reaction. Compared with the uncured COPNA resin, the cured COPNA resin had a smooth surface, well-ordered and streamlined sheet structure with more crystalline solids, better molecular arrangement and orientation. The weight loss process of the uncured and cured COPNA resins was divided into three stages. Carbon residue of the cured COPNA resin was 41.65% at 600 ℃, which was much higher than 25.02% of the uncured COPNA resin, which indicated that the cured COPNA resin had higher thermal stability.
基金Project (59972042) supported by the National Natural Science Foundation of China
文摘Thermal stability and curing kinetics of polycarbosilane (PCS) fibers were studied by thermogravimetry (TG), Fourier transform infrared spectroscopy(FT-IR). Curing is an essential step in the preparation of SiC fibers and the properties of SiC fibers are affected greatly by curing conditions. TG measurement performed in air shows that mass gain starts at approximately 200℃ and PCS fibers are sensitive to oxygen. Curing with oxygen, which results in crosslinking on the surface, enabled PCS fibers to retain its shape during high-temperature pyrolysis. The curing of PCS fibers is oxidation of Si─H and Si─CH3, then Si─O─Si and Si─O─C bonds are formed. This is a first order reaction, with activation energy of 79.27 kJ/mol, and the pre-exponential factor is calculated as 3.07×106. The kinetics model was obtained and the experimental data of PCS fibers show good agreement with the kinetics model.
基金Supported by the Science and Technology Project of Guangdong Province, China(No.2009B011000012)
文摘Novel titanium-doped silicone resins were synthesized from low-cost silane monomers and tetrabutyl titanate as raw materials and hydrochloric acid as catalyst, with titanium element as dopant into principal chain of Si-O-Si. The resins were characterized by means of FTIR, IH NMR and 13C NMR spectra, their thermal properties and curing properties were investigated and their corresponding films were determined. The results show that the thermal stability and storage stability of the resins were influenced by the types of silane monomers containing dif- ferent carbon atomicities of organic group. The thermal stability of the titanium-doped silicone resin with a molar ratio of silane monomer B(n-propyl triethoxysilane) to silane monomer C(n-octyl triethoxysilane) being 1:1 is superior to that of the resin with a molar ratio of silane monomer B to silane monomer C being 1:3. However, the storage stability of the former is inferior to that of the latter. This work also showed that the synthesized titanium-doped silicone resins have the highest thermal stability up to 450--500℃ with an atomicity molar ratio of 1:4 of titanium to silicon in the reactants. But the best storage stability of the resin prepared from the reactants with an atomicity molar ratio of 1:6[n(Ti):n(Si)] was obtained. The effect of the type and content of curing agent on the curing properties of the resin was also studied. Moreover, thermal mechanism and curing mechanism were proposed in this work.
文摘Synergistic effects of layered double hydroxide (LDH) with intumescent flame retardanct (IFR) of phosphorusnitrogen (NP) compound in the polypropylene/ethylene-propylene-diene/IFR/LDH (PP/EPDM/IFR/LDH) nanocomposites and related properties were studied by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), limiting oxygen index (LOI), UL-94 test, cone calorimeter test (CCT) and thermo-gravimetric analysis (TGA). The XRD and TEM results show that the intercalated and/or exfoliated nanocomposites can be obtained by direct melt-intercalation of PP/EPDM into modified LDH and that LDH can promote the IFR additive NP to disperse more homogeneously in the polymer matrix. The SEM results provide positive evidence that more compact charred layers can be obtained from the PP/EPDM/NP/LDH sample than those from the PP/EPDM/LDH and PP/EPDM/NP samples during burning. The LOI and UL-94 rating tests show that the synergetic effects of LDH with NP can effectively increase the flame retardant properties of the PP/EPDM/NP/LDH samples. The data from the CCT and TGA tests indicate that the PP/EPDM/NP/LDH samples apparently decrease the HRR and MLR values and thus enhance the flame retardant properties and have better thermal stability than the PP/EPDM/LDH and PP/EPDM/NP samples.
文摘Aim of present work is to replace asbestos in thermal insulation by another percentage of non-toxic fillers such as silica. Different formulations of fillers were prepared and added to Nordel (Trade name assigned for ethylene, propylene and 1, 4-hexadiene elastomers). The physical and mechanical properties (after and before aging), and thermal properties of the prepared samples were investigated. The objective was to choose a new formulation with properties that resemble as closely as possible those of the originally used in thermal insulation. After measuring the properties of tensile strength, elongation, hardness, specific gravity, compression set, rebound resilience, thermal conductivity, and initial and final decomposition temperatures, the sample that had values very close to those of the originally used in thermal insulation was chosen and recommended to be used. From comparison it was found that EPDM rubber with 50% silica gave the optimum properties closest to the originally used.
文摘A kind of catalyst, ammonium molybdate was developed in this paper to promote the curing reaction of bisphthalonitrile resins with aromatic amine as curing agent, and the catalytic effect was studied by differential scanning calorimetry (DSC), rheometric measurements and thermogravimetric analysis (TGA). The results indicated that the catalyst could improve the curing rate and increase the curing degree, which could be regulated by the content of the catalyst used in the reaction.
文摘The curing behavior of diglycidyl ether of bisphenol-A(DGEBA) with aromatic diamide-diimide-diamines having aryl ether,sulfone and methylene linkages was studied by differential scanning calorimetry(DSC).Nine diamide-diimide-diamines of varying structure were synthesized by reacting 1 mole of dianhydride with 2 moles of L-cysteine(S) in a mixture of acetic acid and pyridine(3:2 V/V) followed by activation with thionyl chloride(SOCl_2) and then condensation with excess of diamines.Structural characterization...
文摘In this work,Epoxidized natural rubber/sawdust short fiber(ENR-50/SD)composites at different fiber content(5,10,15 and 20 phr)and size(fine size at 60–100μm and coarse size at 10–20 mm)were prepared using two-roll mill and electrical-hydraulic hot press machine respectively.Curing characteristics,water uptake,tensile,morphological,physical,and thermal properties of the composites were investigated.Results indicated that the scorch time and cure time became shorter whereas torque improved as SD content increase.Though the decline of tensile strength and elongation at break values,modulus,hardness and crosslinking density have shown enhancements with the increasing of SD content.The water uptake percentage of all samples has shown an increasing as SD content increase.However,the low SD content,particularly fine size have presented lower water uptake.The temperature of weight%loss(5 and 50 wt%loss)of 5 phr SD(low content)have recorded higher temperature compared to 20 phr SD(high content)in the rubber composites,which indicated higher thermal stability.The fine size of SD has recorded better overall properties than SD coarse size at same loading in the rubber composites.
文摘Technological aspects of modifying the operational characteristics of cold cured silicate rubbers have been developed. The effect of chromium oxide on the resistance of cold-curing silicone compounds to thermal aging, as well as on the physic mechanical properties and dielectric characteristics has been studied. The various content of ultrafine chromium oxide in cold-cured silicone compositions has been investigated, it’s optimal content in an amount of 2 - 5 mass at 100 mass, including low molecular weight rubber. Chromium oxide has been proven to improve the thermal stability of cold-cured silicone compositions. The manufacturing technology and component composition of the composition with high performance.