A large amount of coal gangue from coal mining and processing is regarded as waste and usually stockpiled directly. In order to recycle the valuable elements from the coal gangue, an integrated process is proposed. Th...A large amount of coal gangue from coal mining and processing is regarded as waste and usually stockpiled directly. In order to recycle the valuable elements from the coal gangue, an integrated process is proposed. The process consists of three steps: 1concentrating alumina from the coal gangue via activation roasting followed by alkali leaching of Si O2 which produces alumina concentrate for alumina extraction by the Bayer process; 2) synthesizing tobermorite whiskers from the filtrated alkali liquo containing silicate via a hydrothermal method and reusing excess caustic liquor; and 3) enriching titanium component from the Baye process residue by sulfuric acid leaching. Alumina concentrate with 69.5% Al_2O_3 and mass ratio of alumina to silica(A/S) of 5.9pure 1.1 nm tobermorite whisker and TiO_2-rich material containing 33% TiO_2 are produced, respectively, with the optimal parameters Besides, the actual alumina digestion ratio of alumina concentrate reaches 80.4% at 270 oC for 40 min in the Bayer process.展开更多
The high-temperature phase transition of tobermofite was investigated by TGA/DSC, X-ray diffraction and Infrared spectroscopy (IR), respectively. The experimental results showed that Si-OH bonds were cleaved at 724...The high-temperature phase transition of tobermofite was investigated by TGA/DSC, X-ray diffraction and Infrared spectroscopy (IR), respectively. The experimental results showed that Si-OH bonds were cleaved at 724℃ and dehydroxylation occured at the same time, implying that the crystal structure of tobermorite was broken. As a result, the dehydroxylatiun tobermorite was metastable state, exhibiting obviously hydrolysis activity. The suspension was alkaline and Ca^2+ ions content reached a maximum value 4.76% after heat treatment at 724℃. The dehydroxylation tobermorite had potential reactive activity due to the strong hydrolysis activity. The disordered structure recombined to wollastonite, and the crystal structure became ordering and stable at 861℃. Finally, 2M-wollastonite structure can be found in the sample as the temperature reached up to 1 000℃.展开更多
This article presents the thermal transitions of a tobermorite-bearing sample when heated from 30℃ up to 1200℃,both in vacuum and in static air,including tobermorite transforming to wollastonite,aragonite to calcite...This article presents the thermal transitions of a tobermorite-bearing sample when heated from 30℃ up to 1200℃,both in vacuum and in static air,including tobermorite transforming to wollastonite,aragonite to calcite and calcite to lime.Characteristics obtained by in situ high temperature X-ray diffraction,field emission scanning electron microscopy and scanning transmission electron microscopy analyses jointly indicate that the investigated tobermorite is anomalous.The variations along the a,b,c axes and the volume changes of tobermorite with increasing temperature are described,and its thermal shrinkage coefficients therefore determined.The comparison between the refined structures at 30℃ and 800℃ demonstrates that the shrinkage degree(Δa/a0)along the a axis is higher than those(Δb/b0,Δc/c0)along the b and c axes.The wollastonite is formed in two ways:Tobermorite converting to wollastonite and lime reacting with quartz to form wollastonite.展开更多
The difference between the systems of CaO-SiO2,-H2O and CaO-SiO2-Al(OH)3,-H2O, was studied, especially the effect of Al3+on the crystallinity of tobermorite was focussed. As a result, in the system of CaO-SiO2-H2O, to...The difference between the systems of CaO-SiO2,-H2O and CaO-SiO2-Al(OH)3,-H2O, was studied, especially the effect of Al3+on the crystallinity of tobermorite was focussed. As a result, in the system of CaO-SiO2-H2O, tobermorite formed early, however, withreaction time forward, tobermorite was replaced by xonotlite. So far as CaO-SiO2-Al(OH)3,-H2O was concemed, hydrothermal reactionwas cdried out under the same condition as CaO-SiO2-H2O to study the morphological changes of tobermorite crystals. It was found thatAl3+ accelefated the crystal growth of tobermorite to some extent and was in faVor ofplaty crystals. Moreovef, with the Al3+ content in-creasing in the starting material, the morphology of tobermorite did not change magnificently, but platy crystals became more and moreeminent. As soon as the Al2O3 content was over 15.6%, synthetic mineral greatly changed in smicthe and haled into hibschite differentfrom 1 .1 nm tobermorite. Obviously, xonotlite was not apt to form in the presence of Al3+.展开更多
The objective of the present work was to investigate the transition reaction of the calcium silicate hydrate tobermorite into xonotlite under influence of additives. Tobermorite is the main binding agent in steam hard...The objective of the present work was to investigate the transition reaction of the calcium silicate hydrate tobermorite into xonotlite under influence of additives. Tobermorite is the main binding agent in steam hardened building materials and the appearance of xonotlite indicates the progress of hardening and an overcuring of the material. Hydrothermal experiments under addition of sucrose, calcium formate and calcium chloride dihydrate to the main components quartz and lime were done using temperatures of 220°C and a reaction time of 40.5 h. All experiments were performed with powders as well as with pressed educts. The products of all syntheses were analyzed with XRD, SEM/EDX and FTIR. The references as well as the syntheses with calcium chloride dihydrate led to the formation of 11 Å tobermorite and xonotlite. The former showed the best results and even synthesis with pressed educts and calcium chloride dihydrate revealed an accelerating effect of the additive. In contrast syntheses with sucrose had the worst reactivity and led to the formation of calcite beside the CSH-phase scawtite. The additive calcium formate was only slightly oppressing the crystallization of tobermorite and favouring the formation of xonotlite. Syntheses with pressed pellets and sucrose or calcium formate showed generally worse results.展开更多
Calcium-Silicate-Hydrate-phases (CSH-phases) are important binding agents of building materials. The synthesis of CSH phases and their structural characterization was done to investigate the crystallization in depende...Calcium-Silicate-Hydrate-phases (CSH-phases) are important binding agents of building materials. The synthesis of CSH phases and their structural characterization was done to investigate the crystallization in dependence of an increasing CaO/SiO2 ratio (C/S ratios) from 0.41 up to 1.66 at temperatures in the crossover region of tobermorite to xonotlite (180℃ and 230℃). Parallel runs with the same C/S ratio but on the one hand with constant mass of quartz and variation of lime and on the other hand under reverse conditions (constant mass of lime but variable amounts of quartz) were performed at both temperatures. The aim was to clarify the connections of crystallization mechanism and kinetics of phase formation with structure, crystallinity and morphology of the CSH’s in the mentioned C/S ratio for both temperatures in the tobermorite-xonotlite crossover region. The parallel experiments with different mass ratios of the educts are important to study the influence of time evaluation of supersaturation within the solution under the peculiarities of the retrograde solubility of lime but accelerated solubility of quartz. The products were characterized by XRD, SEM/EDX, FTIR and 29Si MAS NMR spectroscopy (using the Q-site nomenclature [1]). The experiments could clarify some important connections of crystallization process and the reaction pathway.展开更多
The measures of steam curing and early-strengthening agents to promote the precast components to reach the target strength quickly can bring different degrees of damage to the concrete.Based on this,the new nanomateri...The measures of steam curing and early-strengthening agents to promote the precast components to reach the target strength quickly can bring different degrees of damage to the concrete.Based on this,the new nanomaterial CSH-the hydration product of cement effectively solves these measures’disadvantages,such as excessive energy consumption,thermal stress damage,and the introduction of external ions.In this paper,the effect of CSH on the early strength of precast fly ash concrete components was investigated in terms of setting time,workability,and mechanical properties and analyzed at the microscopic level using hydration temperature,XRD,and SEM.The results showed that under the same workability,CSH could significantly reduce the amount of admixture,shorten the final setting time,almost not affect the initial setting time,and accelerate the hydration of cement.At the optimum dose of 5%,the mechanical properties of the specimens were improved by more than 98%within 12 h of hydration,resulting in an earlier release time of 12 h and no risk of strength inversion later.The results of this paper give theoretical support to the behavior of precast components under steam-free curing.展开更多
Synthesis of autoclaved aerated concrete (AAC) has been carried out with carbide slag addition, and the carbide slag could be used as a main material to produce the AAC with the compressive strength about 2 MPa and ...Synthesis of autoclaved aerated concrete (AAC) has been carried out with carbide slag addition, and the carbide slag could be used as a main material to produce the AAC with the compressive strength about 2 MPa and the density below 0.6 g.cm-3. In this study, quartz sand acted as frame structure phase in the matrix, and quartz addition also influenced the Si/Ca of starting material. Tobermorite and CSH gel were formed readily at 62%, which seemed to enhance the compressive strength of samples. Curing time seemed to affect the morphology of phase produced, and specimen with the plate-like tobermorite formed at 10 h appeared to have a better compressive strength development than the fiber-like one at 18 h. The higher curing temperature seemed to favor the tobermorite and CSH gel formation, which also exerted a significant effect on the strength development of the samples. On the micro-scale, the formed CSH gel was filled in the interface of the matrix, and the tobermorite appeared to grow in internal-surface of the pores and interstices. The tobermorite or/and CSH formation seemed to densify the matrix, and therefore enhanced the strength of the samples.展开更多
To meet the commercial requirements of inorganic heat insulators,the mixture of diatomite and Ca(OH)2 are evenly dispersed,mold-compacted,and then hydrothermally solidified due to the formation of tobermorite under an...To meet the commercial requirements of inorganic heat insulators,the mixture of diatomite and Ca(OH)2 are evenly dispersed,mold-compacted,and then hydrothermally solidified due to the formation of tobermorite under an autoclaved process.Systematic investigations of the preparation conditions(including mix ratio,autoclaved factors,mold pressure,etc)were carried out to optimize the serving properties of such tobermorite-based products.As a result,a compressive strength of more than 30 MPa was realized for the specimen in high density(about 1.30(g·cm-3)).On the contrary,the specimen in light weight for example 0.63(g·cm-3)typically showed a thermal conductivity of around 0.12(W·m-1·K-1).The present work developed a feasible way to produce and to control the serving properties of diatomite-based heat insulators by a process of hydrothermal solidification,in which the optimized value of Ca/Si ratio was proposed to be 0.6~0.7,while the water content is 25% in weight,and hydrothermal reaction is performed at 180 ℃ for no more than 24 hours.展开更多
The primary objective of this study was to develop an autoclaved light concrete (ALC) material with ultra-thermal insulation property and to investigate the relationship between its physical characteristics and mech...The primary objective of this study was to develop an autoclaved light concrete (ALC) material with ultra-thermal insulation property and to investigate the relationship between its physical characteristics and mechanical properties. Through tests of dry bulk density and compressive strength, relationship of physical characteristics and mechanical properties of samples were studied, resulting in a material with ultra-thermal insulation property. Scanning electron microscope (SEM) and energy-dispersive X-ray spectroscopy (EDX) were applied to analyze the micro-morphology and elemental composition of samples. To identify the product phases, X-ray diffraction (XRD) was engaged. The test results showed that compressive strength and thermal coefficient were reduced with the increasing of aluminum powder within the mixtures. As a result the optimal thermal coefficient and compressive strength of samples were improved to 0.061 W/(m·k) and 1.2 MPa, respectively. SEM, EDX and XRD analyses showed that calcium silicate hydrate and tobermorite crystal were main resultant phases.展开更多
The influence of polycarboxylic-type admixture on the strength of autoclaved aerated concrete(AAC) was investigated. The flexural strength and compressive strength of AAC with polycarboxylic admixture(PA) were tes...The influence of polycarboxylic-type admixture on the strength of autoclaved aerated concrete(AAC) was investigated. The flexural strength and compressive strength of AAC with polycarboxylic admixture(PA) were tested. The microstructure of AAC reinforced by PA was analyzed using scanning electron microscopic(SEM) methods. The crystal structure analysis of AAC with PA was also carried out using X-ray diffraction(XRD). The results showed that the compressive strength and flexural strength of AAC were increased by 43.9% and 42.8%, respectively, when 1.5wt% of PA was mixed. In addition, the dosage of admixture influenced the reinforcing effect. Admixture affected pore structure and surface characteristic of the products in autoclaved curing process and improved the formation of high crystallite tobermorite which led to the enhancement of the compressive and flexural strength of AAC.展开更多
基金Projects(51234008,51174230)supported by the National Natural Science Foundation of ChinaProject(NCET-11-0515)supported by the Program for New Century Excellent Talents in University,ChinaProject supported by Co-Innovation Center for Clean and Efficient Utilization of Strategic Metal Mineral Resources,China
文摘A large amount of coal gangue from coal mining and processing is regarded as waste and usually stockpiled directly. In order to recycle the valuable elements from the coal gangue, an integrated process is proposed. The process consists of three steps: 1concentrating alumina from the coal gangue via activation roasting followed by alkali leaching of Si O2 which produces alumina concentrate for alumina extraction by the Bayer process; 2) synthesizing tobermorite whiskers from the filtrated alkali liquo containing silicate via a hydrothermal method and reusing excess caustic liquor; and 3) enriching titanium component from the Baye process residue by sulfuric acid leaching. Alumina concentrate with 69.5% Al_2O_3 and mass ratio of alumina to silica(A/S) of 5.9pure 1.1 nm tobermorite whisker and TiO_2-rich material containing 33% TiO_2 are produced, respectively, with the optimal parameters Besides, the actual alumina digestion ratio of alumina concentrate reaches 80.4% at 270 oC for 40 min in the Bayer process.
基金Funded by the National Natural Science Foundation of China(No.11134004)the National Science and Technology Major Project(No.2012ZX04010032)+2 种基金the natural science foundation of Ningxia(No.NZ12157)the Project of Jiangsu Constructive Department(No.201007100002)the Graduate Innovation and Creativity Foundation of Jiangsu Province(No.CXZZ11-0243)
文摘The high-temperature phase transition of tobermofite was investigated by TGA/DSC, X-ray diffraction and Infrared spectroscopy (IR), respectively. The experimental results showed that Si-OH bonds were cleaved at 724℃ and dehydroxylation occured at the same time, implying that the crystal structure of tobermorite was broken. As a result, the dehydroxylatiun tobermorite was metastable state, exhibiting obviously hydrolysis activity. The suspension was alkaline and Ca^2+ ions content reached a maximum value 4.76% after heat treatment at 724℃. The dehydroxylation tobermorite had potential reactive activity due to the strong hydrolysis activity. The disordered structure recombined to wollastonite, and the crystal structure became ordering and stable at 861℃. Finally, 2M-wollastonite structure can be found in the sample as the temperature reached up to 1 000℃.
文摘This article presents the thermal transitions of a tobermorite-bearing sample when heated from 30℃ up to 1200℃,both in vacuum and in static air,including tobermorite transforming to wollastonite,aragonite to calcite and calcite to lime.Characteristics obtained by in situ high temperature X-ray diffraction,field emission scanning electron microscopy and scanning transmission electron microscopy analyses jointly indicate that the investigated tobermorite is anomalous.The variations along the a,b,c axes and the volume changes of tobermorite with increasing temperature are described,and its thermal shrinkage coefficients therefore determined.The comparison between the refined structures at 30℃ and 800℃ demonstrates that the shrinkage degree(Δa/a0)along the a axis is higher than those(Δb/b0,Δc/c0)along the b and c axes.The wollastonite is formed in two ways:Tobermorite converting to wollastonite and lime reacting with quartz to form wollastonite.
文摘The difference between the systems of CaO-SiO2,-H2O and CaO-SiO2-Al(OH)3,-H2O, was studied, especially the effect of Al3+on the crystallinity of tobermorite was focussed. As a result, in the system of CaO-SiO2-H2O, tobermorite formed early, however, withreaction time forward, tobermorite was replaced by xonotlite. So far as CaO-SiO2-Al(OH)3,-H2O was concemed, hydrothermal reactionwas cdried out under the same condition as CaO-SiO2-H2O to study the morphological changes of tobermorite crystals. It was found thatAl3+ accelefated the crystal growth of tobermorite to some extent and was in faVor ofplaty crystals. Moreovef, with the Al3+ content in-creasing in the starting material, the morphology of tobermorite did not change magnificently, but platy crystals became more and moreeminent. As soon as the Al2O3 content was over 15.6%, synthetic mineral greatly changed in smicthe and haled into hibschite differentfrom 1 .1 nm tobermorite. Obviously, xonotlite was not apt to form in the presence of Al3+.
文摘The objective of the present work was to investigate the transition reaction of the calcium silicate hydrate tobermorite into xonotlite under influence of additives. Tobermorite is the main binding agent in steam hardened building materials and the appearance of xonotlite indicates the progress of hardening and an overcuring of the material. Hydrothermal experiments under addition of sucrose, calcium formate and calcium chloride dihydrate to the main components quartz and lime were done using temperatures of 220°C and a reaction time of 40.5 h. All experiments were performed with powders as well as with pressed educts. The products of all syntheses were analyzed with XRD, SEM/EDX and FTIR. The references as well as the syntheses with calcium chloride dihydrate led to the formation of 11 Å tobermorite and xonotlite. The former showed the best results and even synthesis with pressed educts and calcium chloride dihydrate revealed an accelerating effect of the additive. In contrast syntheses with sucrose had the worst reactivity and led to the formation of calcite beside the CSH-phase scawtite. The additive calcium formate was only slightly oppressing the crystallization of tobermorite and favouring the formation of xonotlite. Syntheses with pressed pellets and sucrose or calcium formate showed generally worse results.
文摘Calcium-Silicate-Hydrate-phases (CSH-phases) are important binding agents of building materials. The synthesis of CSH phases and their structural characterization was done to investigate the crystallization in dependence of an increasing CaO/SiO2 ratio (C/S ratios) from 0.41 up to 1.66 at temperatures in the crossover region of tobermorite to xonotlite (180℃ and 230℃). Parallel runs with the same C/S ratio but on the one hand with constant mass of quartz and variation of lime and on the other hand under reverse conditions (constant mass of lime but variable amounts of quartz) were performed at both temperatures. The aim was to clarify the connections of crystallization mechanism and kinetics of phase formation with structure, crystallinity and morphology of the CSH’s in the mentioned C/S ratio for both temperatures in the tobermorite-xonotlite crossover region. The parallel experiments with different mass ratios of the educts are important to study the influence of time evaluation of supersaturation within the solution under the peculiarities of the retrograde solubility of lime but accelerated solubility of quartz. The products were characterized by XRD, SEM/EDX, FTIR and 29Si MAS NMR spectroscopy (using the Q-site nomenclature [1]). The experiments could clarify some important connections of crystallization process and the reaction pathway.
文摘The measures of steam curing and early-strengthening agents to promote the precast components to reach the target strength quickly can bring different degrees of damage to the concrete.Based on this,the new nanomaterial CSH-the hydration product of cement effectively solves these measures’disadvantages,such as excessive energy consumption,thermal stress damage,and the introduction of external ions.In this paper,the effect of CSH on the early strength of precast fly ash concrete components was investigated in terms of setting time,workability,and mechanical properties and analyzed at the microscopic level using hydration temperature,XRD,and SEM.The results showed that under the same workability,CSH could significantly reduce the amount of admixture,shorten the final setting time,almost not affect the initial setting time,and accelerate the hydration of cement.At the optimum dose of 5%,the mechanical properties of the specimens were improved by more than 98%within 12 h of hydration,resulting in an earlier release time of 12 h and no risk of strength inversion later.The results of this paper give theoretical support to the behavior of precast components under steam-free curing.
基金Funded by the National Natural Science Foundation of China(Nos.51272180,51072138)
文摘Synthesis of autoclaved aerated concrete (AAC) has been carried out with carbide slag addition, and the carbide slag could be used as a main material to produce the AAC with the compressive strength about 2 MPa and the density below 0.6 g.cm-3. In this study, quartz sand acted as frame structure phase in the matrix, and quartz addition also influenced the Si/Ca of starting material. Tobermorite and CSH gel were formed readily at 62%, which seemed to enhance the compressive strength of samples. Curing time seemed to affect the morphology of phase produced, and specimen with the plate-like tobermorite formed at 10 h appeared to have a better compressive strength development than the fiber-like one at 18 h. The higher curing temperature seemed to favor the tobermorite and CSH gel formation, which also exerted a significant effect on the strength development of the samples. On the micro-scale, the formed CSH gel was filled in the interface of the matrix, and the tobermorite appeared to grow in internal-surface of the pores and interstices. The tobermorite or/and CSH formation seemed to densify the matrix, and therefore enhanced the strength of the samples.
文摘To meet the commercial requirements of inorganic heat insulators,the mixture of diatomite and Ca(OH)2 are evenly dispersed,mold-compacted,and then hydrothermally solidified due to the formation of tobermorite under an autoclaved process.Systematic investigations of the preparation conditions(including mix ratio,autoclaved factors,mold pressure,etc)were carried out to optimize the serving properties of such tobermorite-based products.As a result,a compressive strength of more than 30 MPa was realized for the specimen in high density(about 1.30(g·cm-3)).On the contrary,the specimen in light weight for example 0.63(g·cm-3)typically showed a thermal conductivity of around 0.12(W·m-1·K-1).The present work developed a feasible way to produce and to control the serving properties of diatomite-based heat insulators by a process of hydrothermal solidification,in which the optimized value of Ca/Si ratio was proposed to be 0.6~0.7,while the water content is 25% in weight,and hydrothermal reaction is performed at 180 ℃ for no more than 24 hours.
基金Funded by the National Science & Technology Program During theEleventh Five-Year Plan Period (No.2008BAJ12B04)
文摘The primary objective of this study was to develop an autoclaved light concrete (ALC) material with ultra-thermal insulation property and to investigate the relationship between its physical characteristics and mechanical properties. Through tests of dry bulk density and compressive strength, relationship of physical characteristics and mechanical properties of samples were studied, resulting in a material with ultra-thermal insulation property. Scanning electron microscope (SEM) and energy-dispersive X-ray spectroscopy (EDX) were applied to analyze the micro-morphology and elemental composition of samples. To identify the product phases, X-ray diffraction (XRD) was engaged. The test results showed that compressive strength and thermal coefficient were reduced with the increasing of aluminum powder within the mixtures. As a result the optimal thermal coefficient and compressive strength of samples were improved to 0.061 W/(m·k) and 1.2 MPa, respectively. SEM, EDX and XRD analyses showed that calcium silicate hydrate and tobermorite crystal were main resultant phases.
基金Funded by the Fundamental Research Funds for the Central Universities(No.2242016K41003)
文摘The influence of polycarboxylic-type admixture on the strength of autoclaved aerated concrete(AAC) was investigated. The flexural strength and compressive strength of AAC with polycarboxylic admixture(PA) were tested. The microstructure of AAC reinforced by PA was analyzed using scanning electron microscopic(SEM) methods. The crystal structure analysis of AAC with PA was also carried out using X-ray diffraction(XRD). The results showed that the compressive strength and flexural strength of AAC were increased by 43.9% and 42.8%, respectively, when 1.5wt% of PA was mixed. In addition, the dosage of admixture influenced the reinforcing effect. Admixture affected pore structure and surface characteristic of the products in autoclaved curing process and improved the formation of high crystallite tobermorite which led to the enhancement of the compressive and flexural strength of AAC.