Three thermal analytical techniques such as differential scanning calorimetry(DSC), thermal gravimetric analysis(TGA) using five heating rates, and DSC-Fourier Transform Infrared(DSCFTIR) microspectroscopy using one h...Three thermal analytical techniques such as differential scanning calorimetry(DSC), thermal gravimetric analysis(TGA) using five heating rates, and DSC-Fourier Transform Infrared(DSCFTIR) microspectroscopy using one heating rate, were used to determine the thermal characteristics and the dehydration process of aspartame(APM) hemihydrate in the solid state.The intramolecular cyclization process of APM anhydrate was also examined. One exothermic and four endothermic peaks were observed in the DSC thermogram of APM hemihydrate,in which the exothermic peak was due to the crystallization of some amorphous APM caused by dehydration process from hemihydrate to anhydride. While four endothermic peaks were corresponded to the evaporation of absorbed water, the dehydration of hemihydrate, the diketopiperazines(DKP) formation via intramolecular cyclization, and the melting of DKP, respectively. The weight loss measured in TGA curve of APM hemihydrate was associated with these endothermic peaks in the DSC thermogram. According to the Flynn–Wall–Ozawa(FWO)model, the activation energy of dehydration process within 100–150 °C was about 218 ± 11 kJ/mol determined by TGA technique. Both the dehydration and DKP formation processes for solid-state APM hemihydrate were markedly evidenced from the thermal-responsive changes in several specific FTIR bands by a single-step DSC-FTIR microspectroscopy.展开更多
In order to reduce the influence of impurities in hemihydrate phosphogypsum(HPG)on the environment and improve the workability of HPG,the effects of the content of quicklime and types of biopolymer(hydroxypropyl methy...In order to reduce the influence of impurities in hemihydrate phosphogypsum(HPG)on the environment and improve the workability of HPG,the effects of the content of quicklime and types of biopolymer(hydroxypropyl methylcellulose,xanthan gum,sodium polyacrylate(PAANa))on the compressive strength,softening coefficient and ultrasonic velocity of HPG were evaluated.When the content of quicklime was 1.5%and the content of PAA-Na was 0.2%,HPG had the best mechanical properties and workability,its water retention rate can be increased by 5.8%,and unconfined compressive strength of 3 days increased by 10.3%and 7 days increased by 13.1%.Through the analysis of scanning electron microscope and X-ray diffraction,it was found that the hydration reac-tion of HPG was more sufficient,the pores size and number decreased,the number of impurities on the crystal surface decreased obviously,and CaF2 and other substances were formed by the reaction after the addition of quicklime.After adding quicklime and PAANa,the indicators of gypsum self-leveling mortar prepared by HPG meet the requirements of the standard.展开更多
The objective of this study was to assess the feasibility of using the plant-source polymer of the matcha powder as a composite admixture for hemihydrate gypsum. Hemihydrate gypsum was mixed with different contents of...The objective of this study was to assess the feasibility of using the plant-source polymer of the matcha powder as a composite admixture for hemihydrate gypsum. Hemihydrate gypsum was mixed with different contents of matcha powder, and then the water requirement for the normal consistency, setting times, density, strength, hydration and microstructure of the hardened mixture were evaluated. The experimental results showed that it increased the water requirement for the normal consistency, and it regulated the setting times and reduced the density. Hemihydrate gypsum with more matcha powder had the higher water requirement, longer setting times and lower density. Less than 1% matcha powder had slight impact on the strength of hardened paste, but more than 1% matcha powder had a remarkable one. Matcha powder changed the hydration process and prolonged the induction and acceleration period. Small needlelike crystals were transformed into longer, larger and thicker ones as more matcha powder was mixed. This case is closely related to the prolongation of the induction and acceleration period. Besides, more and larger pores were observed in the hardened paste with more matcha powder. It is attributed to the appearances of the tea polyphenol in matcha powder and the larger and longer crystal morphology in hardened paste as well as the high water requirement for the normal consistency. These results are important to the application of matcha powder as a composite admixture for the hemihydrate gypsum as well as the prosperity and development of the tea industry.展开更多
α-calcium sulfate hemihydrate (α-HH) is known to be suitable for application as bone void filler. High percentage of α-HH is obviously needed for medical applications, especially for implantation. Three commerciall...α-calcium sulfate hemihydrate (α-HH) is known to be suitable for application as bone void filler. High percentage of α-HH is obviously needed for medical applications, especially for implantation. Three commercially available calcium sulfate dihydrates (DH, CaSO4·2H2O) with different sizes and surface morphologies were used as starting materials to synthesize high percentage α-HH via a hydrothermal method. The median particle sizes of the three types of DH were 946.7 μm, 162.4 μm and 62.4 μm, respectively. They were named as DH-L, DH-M and DH-S in this paper. The particle size distribution, morphology and phase composition of the raw materials were evaluated before synthesis. SEM results revealed that DH-L consisted of irregular large particles, while DH-M and DH-S were composed of plate-like particles with some small ones. High percentage HH can be obtained with proper synthesis parameters by hydrothermal method, specifically, 105 °C/90 min for DH-L (achieving 98.8% HH), 105°C/30 min for DH-M (achieving 96.7% HH) and 100°C/45 min for DH-S (achieving 98.4% HH). All the synthesized HH were hexagonal columns, demonstrating that they were α-phase HH. The particle size and morphology of starting material (DH) have significant influences on not only the rate of phase transition but also the morphology of the synthesized α-HH. Calcium sulfate dihydrate cements were prepared by the synthesized α-HH. The highest compressive strength of calcium sulfate dihydrate cement was 17.2 MPa. The results show that the preparation of high percentage α-HH is feasible via a hydrothermal method and the process can be further scaled up to industrial scale production.展开更多
Objective:To prepare a bone repair material with certain mechanical strength and biological activity,this paper used calcium sulfate hemihydrate(CSH)powder compounded with calcium hydroxide(Ca(OH)2)powder to prepare a...Objective:To prepare a bone repair material with certain mechanical strength and biological activity,this paper used calcium sulfate hemihydrate(CSH)powder compounded with calcium hydroxide(Ca(OH)2)powder to prepare a bone repair scaffold material for physicochemical property characterization and testing.Methods:The physical and chemical properties and characterization of the dried and cured bone repair materials were determined by Fourier infrared spectroscopy(FT-IR),X-ray diffraction(XRD),and scanning electron microscopy;Universal material testing machine to determine the mechanical and mechanical strength of composite materials.Results:XRD showed that the structure of the composite material phase at 5%concentration was calcium sulfate hemihydrate and calcium hydroxide after hydration.The FT-IR and XRD analyses were consistent.Scanning electron microscopy(SEM)results showed that calcium hydroxide was uniformly dispersed in the hemihydrate calcium sulfate material.0%,1%,5%,and 10%specimen groups had compressive strengths of 3.86±3.1,5.27±1.28,8.22±0.96,and 14.4±3.28 MPa.10%addition of calcium hydroxide significantly improved the mechanical strength of the composites,but also reduced the the porosity of the material.Conclusion:With the addition of calcium hydroxide,the CSH-Ca(OH)2 composite was improved in terms of mechanical material and is expected to be a new type of bone repair material.展开更多
Objective:The as-providedα-calcium sulfate hemihydrate bone repair material exhibits superior degradation properties and osteogenic property to the traditional calcium sulfate bone repair materials. Its effects on th...Objective:The as-providedα-calcium sulfate hemihydrate bone repair material exhibits superior degradation properties and osteogenic property to the traditional calcium sulfate bone repair materials. Its effects on the blood and the biocompatibility were studied to ensure its safety for the bone implantation application.Method: The hemolytic tests were conducted to evaluate the blood compatibility of theα-calcium sulfate hemihydrate. The extracts ofα-calcium sulfate hemihydrate with different concentration reacted with 2% rabbit red blood cell suspension. The existence and morphology of the red blood were observed through naked eye observation and microscope observation. The hemolytic ratios were calculated through the absorbances using a ultraviolet spectrophotometer.Result:It was observed by naked eye that the red blood accumulated at the bottom of the test tubes and the upper liquids were clear, colorless and transparent in the experimental sample. The microscope observation exhibited that the cells of the experimental samples had the normal morphology, no deformed and broken blood sell existed. The hemolytic ratios of the experimental sample were all less than 5%. The hemolytic ratios were increased with the increase of the concentration of the extracts. Conclusions: The hemolytic ratios of the medical -calcium sulfate hemihydrate accorded with the standard ISO/TR7405-1984(E). It could be concluded the material would not cause acute hemolysis. The osteogenic property exhibited dose dependence.展开更多
The synthesis of α-calcium sulfate hemihydrate (α-CSH) from flue gas desulfurization (FGD)gypsum is a good way to realize the comprehensive utilization of FGD gypsum. To obtainα-CSH with the satisfactory performanc...The synthesis of α-calcium sulfate hemihydrate (α-CSH) from flue gas desulfurization (FGD)gypsum is a good way to realize the comprehensive utilization of FGD gypsum. To obtainα-CSH with the satisfactory performances, a facile hydrothermal-aging pretreatment process for FGD gypsum raw materials was proposed, where FGD gypsum was firstly hydrothermally converted to α-CSH whiskers, and α-CSH whiskers were further hydrated to synthesize CaSO4·2H2O (CSD) by aging under the regulation of N,N'-methylenebisacrylamide (MBA). The effects of aging time, MBA addition, aging temperature, and pH on the morphology of the synthesized CSD were investigated. The synthesized CSD crystals exhibit highly uniform prismatic morphology with the length of ca 100μm and the whiteness of 91.56%. The regulation mechanism of MBA was also illustrated. The synthesized CSD crystals with prismatic morphology were further used as raw materials to synthesize the short columnar α-CSH. The absolute dry compressive strength of paste prepared from the short columnar α-CSH is 40.85 MPa, which reaches α40 strength grade.展开更多
Alpha-calcium sulfate hemihydrate (α-HH) has been prepared from flue gas desulfurization (FGD) gypsum with salt solution method under atmospheric pressure. X-ray diffraction (XRD),thermogra-vimetry and differential s...Alpha-calcium sulfate hemihydrate (α-HH) has been prepared from flue gas desulfurization (FGD) gypsum with salt solution method under atmospheric pressure. X-ray diffraction (XRD),thermogra-vimetry and differential scanning calorimetry (TG-DSC),optical micrograph,X-ray photoelectron spec-troscopy (XPS),energy dispersive spectrometry (EDS),and scanning electron microscopy (SEM) have been employed to characterize the α-HH crystals,based on which the formation and growth mecha-nisms of the α-HH crystals have been discussed. The results show that FGD gypsum can be success-fully transformed into high purity α-HH in salt solution under mild conditions,and that a dissolu-tion-recrystallization route is most probably adopted by this transition. The growth of α-HH crystals in salt solution demonstrates a preferred direction along [001] and results in a bundle-of-sheets or bun-dle-of-raphide texture. The characteristics revealed in this study can help to understand and control the growth of the α-HH crystal from solution.展开更多
文摘Three thermal analytical techniques such as differential scanning calorimetry(DSC), thermal gravimetric analysis(TGA) using five heating rates, and DSC-Fourier Transform Infrared(DSCFTIR) microspectroscopy using one heating rate, were used to determine the thermal characteristics and the dehydration process of aspartame(APM) hemihydrate in the solid state.The intramolecular cyclization process of APM anhydrate was also examined. One exothermic and four endothermic peaks were observed in the DSC thermogram of APM hemihydrate,in which the exothermic peak was due to the crystallization of some amorphous APM caused by dehydration process from hemihydrate to anhydride. While four endothermic peaks were corresponded to the evaporation of absorbed water, the dehydration of hemihydrate, the diketopiperazines(DKP) formation via intramolecular cyclization, and the melting of DKP, respectively. The weight loss measured in TGA curve of APM hemihydrate was associated with these endothermic peaks in the DSC thermogram. According to the Flynn–Wall–Ozawa(FWO)model, the activation energy of dehydration process within 100–150 °C was about 218 ± 11 kJ/mol determined by TGA technique. Both the dehydration and DKP formation processes for solid-state APM hemihydrate were markedly evidenced from the thermal-responsive changes in several specific FTIR bands by a single-step DSC-FTIR microspectroscopy.
基金This study was financially supported by National Natural Science Foundation of China(GrantNo.51834001)Fundamental Research Funds for the Central University(Grant No.FRF-BD-20-01B).
文摘In order to reduce the influence of impurities in hemihydrate phosphogypsum(HPG)on the environment and improve the workability of HPG,the effects of the content of quicklime and types of biopolymer(hydroxypropyl methylcellulose,xanthan gum,sodium polyacrylate(PAANa))on the compressive strength,softening coefficient and ultrasonic velocity of HPG were evaluated.When the content of quicklime was 1.5%and the content of PAA-Na was 0.2%,HPG had the best mechanical properties and workability,its water retention rate can be increased by 5.8%,and unconfined compressive strength of 3 days increased by 10.3%and 7 days increased by 13.1%.Through the analysis of scanning electron microscope and X-ray diffraction,it was found that the hydration reac-tion of HPG was more sufficient,the pores size and number decreased,the number of impurities on the crystal surface decreased obviously,and CaF2 and other substances were formed by the reaction after the addition of quicklime.After adding quicklime and PAANa,the indicators of gypsum self-leveling mortar prepared by HPG meet the requirements of the standard.
基金Funded by the National Natural Science Foundation of China(Nos.51678442,51578412,51478348,51508404,51878480,and 51878479)the National High-speed Train Union Fund(U1534207)+1 种基金Key Project of the Shanghai Committee of Science and Technology(No.15DZ1205003)the Fundamental Research Funds for the Central Universities
文摘The objective of this study was to assess the feasibility of using the plant-source polymer of the matcha powder as a composite admixture for hemihydrate gypsum. Hemihydrate gypsum was mixed with different contents of matcha powder, and then the water requirement for the normal consistency, setting times, density, strength, hydration and microstructure of the hardened mixture were evaluated. The experimental results showed that it increased the water requirement for the normal consistency, and it regulated the setting times and reduced the density. Hemihydrate gypsum with more matcha powder had the higher water requirement, longer setting times and lower density. Less than 1% matcha powder had slight impact on the strength of hardened paste, but more than 1% matcha powder had a remarkable one. Matcha powder changed the hydration process and prolonged the induction and acceleration period. Small needlelike crystals were transformed into longer, larger and thicker ones as more matcha powder was mixed. This case is closely related to the prolongation of the induction and acceleration period. Besides, more and larger pores were observed in the hardened paste with more matcha powder. It is attributed to the appearances of the tea polyphenol in matcha powder and the larger and longer crystal morphology in hardened paste as well as the high water requirement for the normal consistency. These results are important to the application of matcha powder as a composite admixture for the hemihydrate gypsum as well as the prosperity and development of the tea industry.
基金financial support from the Swedish Innovation Agency(VINNOVA)and China Scholarship Council(CSC).
文摘α-calcium sulfate hemihydrate (α-HH) is known to be suitable for application as bone void filler. High percentage of α-HH is obviously needed for medical applications, especially for implantation. Three commercially available calcium sulfate dihydrates (DH, CaSO4·2H2O) with different sizes and surface morphologies were used as starting materials to synthesize high percentage α-HH via a hydrothermal method. The median particle sizes of the three types of DH were 946.7 μm, 162.4 μm and 62.4 μm, respectively. They were named as DH-L, DH-M and DH-S in this paper. The particle size distribution, morphology and phase composition of the raw materials were evaluated before synthesis. SEM results revealed that DH-L consisted of irregular large particles, while DH-M and DH-S were composed of plate-like particles with some small ones. High percentage HH can be obtained with proper synthesis parameters by hydrothermal method, specifically, 105 °C/90 min for DH-L (achieving 98.8% HH), 105°C/30 min for DH-M (achieving 96.7% HH) and 100°C/45 min for DH-S (achieving 98.4% HH). All the synthesized HH were hexagonal columns, demonstrating that they were α-phase HH. The particle size and morphology of starting material (DH) have significant influences on not only the rate of phase transition but also the morphology of the synthesized α-HH. Calcium sulfate dihydrate cements were prepared by the synthesized α-HH. The highest compressive strength of calcium sulfate dihydrate cement was 17.2 MPa. The results show that the preparation of high percentage α-HH is feasible via a hydrothermal method and the process can be further scaled up to industrial scale production.
基金National Natural Science Foundation of China(No.82060347)Postgraduate innovation research project of Hainan Medical College(No.HYYS2020-38)。
文摘Objective:To prepare a bone repair material with certain mechanical strength and biological activity,this paper used calcium sulfate hemihydrate(CSH)powder compounded with calcium hydroxide(Ca(OH)2)powder to prepare a bone repair scaffold material for physicochemical property characterization and testing.Methods:The physical and chemical properties and characterization of the dried and cured bone repair materials were determined by Fourier infrared spectroscopy(FT-IR),X-ray diffraction(XRD),and scanning electron microscopy;Universal material testing machine to determine the mechanical and mechanical strength of composite materials.Results:XRD showed that the structure of the composite material phase at 5%concentration was calcium sulfate hemihydrate and calcium hydroxide after hydration.The FT-IR and XRD analyses were consistent.Scanning electron microscopy(SEM)results showed that calcium hydroxide was uniformly dispersed in the hemihydrate calcium sulfate material.0%,1%,5%,and 10%specimen groups had compressive strengths of 3.86±3.1,5.27±1.28,8.22±0.96,and 14.4±3.28 MPa.10%addition of calcium hydroxide significantly improved the mechanical strength of the composites,but also reduced the the porosity of the material.Conclusion:With the addition of calcium hydroxide,the CSH-Ca(OH)2 composite was improved in terms of mechanical material and is expected to be a new type of bone repair material.
文摘Objective:The as-providedα-calcium sulfate hemihydrate bone repair material exhibits superior degradation properties and osteogenic property to the traditional calcium sulfate bone repair materials. Its effects on the blood and the biocompatibility were studied to ensure its safety for the bone implantation application.Method: The hemolytic tests were conducted to evaluate the blood compatibility of theα-calcium sulfate hemihydrate. The extracts ofα-calcium sulfate hemihydrate with different concentration reacted with 2% rabbit red blood cell suspension. The existence and morphology of the red blood were observed through naked eye observation and microscope observation. The hemolytic ratios were calculated through the absorbances using a ultraviolet spectrophotometer.Result:It was observed by naked eye that the red blood accumulated at the bottom of the test tubes and the upper liquids were clear, colorless and transparent in the experimental sample. The microscope observation exhibited that the cells of the experimental samples had the normal morphology, no deformed and broken blood sell existed. The hemolytic ratios of the experimental sample were all less than 5%. The hemolytic ratios were increased with the increase of the concentration of the extracts. Conclusions: The hemolytic ratios of the medical -calcium sulfate hemihydrate accorded with the standard ISO/TR7405-1984(E). It could be concluded the material would not cause acute hemolysis. The osteogenic property exhibited dose dependence.
基金Funded by National Natural Science Foundation of China(No.22008049)Natural Science Foundation of Hebei Province,China (Nos.B2020202081 and B2018202330)+1 种基金Key Laboratory of Gas Hydrate,Guangzhou Institute of Energy Conversion,Chinese Academy of Sciences,China (No.E029kf1601)Research Fund Program of Science and Technology of Colleges and Universities of Hebei Province,China (No.QN2019012)。
文摘The synthesis of α-calcium sulfate hemihydrate (α-CSH) from flue gas desulfurization (FGD)gypsum is a good way to realize the comprehensive utilization of FGD gypsum. To obtainα-CSH with the satisfactory performances, a facile hydrothermal-aging pretreatment process for FGD gypsum raw materials was proposed, where FGD gypsum was firstly hydrothermally converted to α-CSH whiskers, and α-CSH whiskers were further hydrated to synthesize CaSO4·2H2O (CSD) by aging under the regulation of N,N'-methylenebisacrylamide (MBA). The effects of aging time, MBA addition, aging temperature, and pH on the morphology of the synthesized CSD were investigated. The synthesized CSD crystals exhibit highly uniform prismatic morphology with the length of ca 100μm and the whiteness of 91.56%. The regulation mechanism of MBA was also illustrated. The synthesized CSD crystals with prismatic morphology were further used as raw materials to synthesize the short columnar α-CSH. The absolute dry compressive strength of paste prepared from the short columnar α-CSH is 40.85 MPa, which reaches α40 strength grade.
基金Supported by the National High-Tech Research & Development Program of China (Grant No. 2006AA06Z385)New Century Excellent Talents in University (Grant No. NCET-04-0549)the Project of Science and Technology Plan of Zhejiang Province (Grant No. 2007C23055)
文摘Alpha-calcium sulfate hemihydrate (α-HH) has been prepared from flue gas desulfurization (FGD) gypsum with salt solution method under atmospheric pressure. X-ray diffraction (XRD),thermogra-vimetry and differential scanning calorimetry (TG-DSC),optical micrograph,X-ray photoelectron spec-troscopy (XPS),energy dispersive spectrometry (EDS),and scanning electron microscopy (SEM) have been employed to characterize the α-HH crystals,based on which the formation and growth mecha-nisms of the α-HH crystals have been discussed. The results show that FGD gypsum can be success-fully transformed into high purity α-HH in salt solution under mild conditions,and that a dissolu-tion-recrystallization route is most probably adopted by this transition. The growth of α-HH crystals in salt solution demonstrates a preferred direction along [001] and results in a bundle-of-sheets or bun-dle-of-raphide texture. The characteristics revealed in this study can help to understand and control the growth of the α-HH crystal from solution.
