水热合成硬硅钙石晶须及其在超轻质硅酸钙材料中应用的研究
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摘要
超轻质硅酸钙材料由于其低导热系数,良好高温热稳定性及较小容重被广泛应用于各行各业。然而,该材料力学性能不易达到使用要求,限制了推广应用。硬硅钙石晶须可作为一种用途广泛的补强增韧材料。本文采用水热合成工艺制备硬硅钙石晶须和球形粒子,分别采用“外掺增强法”和“晶须原位生长增强法”制备技术,最终实现该材料力学性能的提高。
本文率先以硬硅钙石晶体为研究对象,通过水热合成法研究了原料、水热合成工艺对硬硅钙石产物形貌的影响。结果表明,硅质原料前驱体形态决定了水热合成产物的形貌。基于产物不同形貌特征,探讨并对比了硬硅钙石晶须和球形粒子生成机理及水热反应过程。硬硅钙石晶须和球形粒子生成分别按溶解-沉淀反应机理和原位转变机理进行。在CaO-SiO2-H2O反应体系中,CaO:SiO2(mol)=1.0,硬硅钙石晶体反应过程可描述为:非晶态C-S-H凝胶→富钙C-S-H(II)→富硅C-S-H(I)→硬硅钙石。基于硬硅钙石晶体反应过程,建立了相应动力学关系式:硬硅钙石晶须为? dc A /dt = kcA4/5,球形粒子为? dc A /dt = kcA0.9。依此动力学关系式和近藤氏模型计算得到硬硅钙石晶须和球形粒子表观活化能分别为75-77 kJ·mol-1、77-84 kJ·mol-1。动力学分析结果表明了硬硅钙石晶体生长机理及反应过程的正确性。
对各工艺参数条件下制备的硬硅钙石晶须材料微观结构进行了全面分析。结果表明:以CaCl2和100g·L-1KOH溶液混合制得Ca(OH)2悬浮液为钙源,K2SiO3溶液为硅源,体系pH=12.6,反应物浓度为0.05mol·L-1,在225℃保温15 h的条件下水热合成硬硅钙石晶须结晶良好、热稳定性较好、长径比可达50-100。重点分析了杂质及含量对水热合成产物微观结构的影响。以CaCl2为钙源引入Cl-离子,控制Na2O含量小于5%,Al2O3含量小于1%有利于硬硅钙石晶须的制备。
创新性地以电石渣为原料制备硬硅钙石晶体。鉴于不同水热产物形貌对原料提出的特殊要求,以酸洗除杂技术对电石渣进行预处理,并用于制备硬硅钙石晶须,确定了适宜制备工艺参数为酸洗pH=8.0,225℃保温15 h。分别以煅烧和超声技术对电石渣进行预处理,并用于制备硬硅钙石球形粒子,确定了适宜制备工艺参数为:以800℃保温2 h煅烧电石渣,12倍80℃去离子水搅拌30 min制备Ca(OH)2乳液为钙质原料,或以160 W超声3 h预处理电石渣为钙质原料,钙硅摩尔比为1.0,水固比为28:1,升温阶段搅拌速度400 rpm,保温阶段搅拌速度150 rpm,215℃保温10 h。
针对水热合成硬硅钙石及晶体生长特点,采用“外掺增强法”及“晶须原位生长增强法”制备工艺,实现超轻质硅酸钙材料的补强增韧。采用“外掺增强法”时,适宜的制备工艺参数为:长径比50-100硬硅钙石晶须掺量5%,成型压力为0.5 MPa,脱模75℃烘干12 h,制得容重109 Kg·m-3增强体制品抗折、抗压强度分别为0.37 MPa和0.59 MPa。采用“晶须原位生长增强法”时,适宜的制备工艺参数为:以K2SiO3:H2SiO3(mol)=2:1为硅质原料,在225℃保温15 h条件下进行水热合成反应,成型压力为0.5 MPa,脱模75℃烘干12 h,制得容重为118 Kg·m-3的增强体制品抗折、抗压强度分别为0.42 MPa、0.66 MPa。以3%玻璃纤维制得制品的比强度值Specific strengthF和Specific strengthC分别为2.22×103 cm和3.65×103 cm,以5%硬硅钙石晶须制得制品比强度值Specific strengthF和Specific strengthC分别为3.40×103 cm和5.41×103 cm。以硬硅钙石晶须为增强材料制得制品具有更低容重,更高比强度和更好保温隔热性能。
Ultra-light material of calcium silicate has been widely used in industry for its low thermal conductivity, wide applying temperature range and low density. However, it was limited due to the disadvantage of mechanical properties. Xonotlite whiskers, which are required in the development of modern composite materials, have been attracting attention as a kind of strengthening and toughening materials. The xonotlite whiskers and spherical particles were synthesized using the hydrothermal synthesis method, and the ultra-light material of calcium silicate had been strengthened with the methods of“adding reinforcing agent”and“whisker in–situ growth”respectively.
In this paper, xonotlite crystal was firstly prepared by the hydrothermal synthesis method, and the effect of raw materials and hydrothermal synthetic technologies on the morphology of xonotlite was also studied. The results indicated that the morphologies of hydrothermal synthesis products were determined by the precursor states of kiesel materials. Base on the different morphology characteristics of the products, the growth mechanism and reaction mechanism of xonotlite whiskers and spherical particles were explored, and the growth of xonotlite whiskers and spherical particles were accorded with the dissolution-precipitation mechanism and in situ transformation mechanism. In the CaO-SiO2-H2O system, the reaction mechanism of xonotlite crystal was described as follows while having CaO:SiO2(mol)=1.0: amorphous C-S-H gel→calcium-rich C-S-H(II)→silicon-rich C-S-H(I)→xonotlite. The kinetics formulas of xonotlite whiskers and spherical particles were found based on the reaction mechanism of xonotlite crystal: ? dc A /dt = kcA4/5 is for xonotlite whiskers and ? dc A /dt = kcA0.9 is for xonotlite spherical particles. At last, the apparent activation energy of xonotlite whiskers and spherical particles are 75-77 kJ·mol-1 and 77-84 kJ·mol-1 respectively through those kinetics formulas and Kondo model. The anlysis results of kinetics indicated that the growth and reaction mechanisms of xonotlite crystal are correct.
The microstructures of xonotlite whiskers prepared at different process parameters were analyzed comprehensively. The results showed that the xonotlite whiskers, which are of well crystallized, excellent thermal stability and aspect ratio of 50-100, were synthesized by hydrothermal processing with Ca(OH)2 suspension which was prepared by using CaCl2 and 100g·L-1KOH solution as calcareous material and K2SiO3 solution as kiesel materials, controlling the system of pH=12.6 and reactant concentration of 0.05mol·L-1 at 225℃for 15 h. The effect of impurities and its content on the morphologies of hydrothermal synthesis products was studied mainly in this paper, and adding Cl- ions when using CaCl2 as calcareous material, controlling the Na2O content less than 5% and Al2O3 content less than 1% are beneficial to the preparation of xonotlite whiskers.
The xonotlite crystal was prepared for the first time using the carbide slag as raw material. The requirements of raw materials are different attributed to the different morphologies of hydrothermal synthesis products, and then the xonotlite whiskers were synthesized from the carbide slag which was pretreated by the way of pickling under the conditions of pH=8.0 when pickling, at 225℃for 15 h, which are the best process parameters in this paper. The xonotlite spherical particles were prepared from the carbide slag which was pretreated by the methods of calcination and ultrasonic technologies respectively, under the conditions of using Ca(OH)2 suspension which was prepared from the carbide slag calcined at 800℃for 2 h and digested by the deionized water of 12 times and 80℃for 30 min as calcareous material, or using the carbide slag slurry at 160 W ultrasonic for 3 h as calcareous material, CaO/SiO2 mol ratio 1.0, water/solid weight ratio of 28:1, stirring speed of 400 rpm and 150 rpm when heating and reaction stage respectively, at 215℃for 10 h.
Base on the growth characteristics of xonotlite crystal, the ultra-light material of calcium silicate was strengthened with the methods of“adding reinforcing agent”and“whisker in–situ growth”respectively. The product of 109 Kg·m-3 was prepared under the conditions of aspect ratio of 50-100, whiskers mixing amount of 5%, forming pressure of 0.5 MPa, demould and drying at 75℃for 12 h, and its flexural and compressive strength are 0.37 MPa and 0.59 MPa respectively when having the method of“adding reinforcing agent”. The product of 118 Kg·m-3 was prepared under the conditions of K2SiO3/H2SiO3 mol ratio 2.0, hydrothermal treatment proceeded at 225℃for 15 h, forming pressure of 0.5 MPa, demould and drying at 75℃for 12 h, and its flexural and compressive strength are 0.42 MPa and 0.66 MPa respectively when having the method of“whisker in–situ growth”. The specific strengthF and specific strengthC of the products prepared by adding glass fibers of 3% are 2.22×103 cm and 3.65×103 cm respectively, and the specific strengthF and specific strengthC of the products prepared by adding xonotlite whiskers of 5% are 3.40×103 cm and 5.41×103 cm respectively. The results indicated that the product prepared by adding xonotlite whiskers is of lower density, higher specific strength and well thermal insulation performance.
本文率先以硬硅钙石晶体为研究对象,通过水热合成法研究了原料、水热合成工艺对硬硅钙石产物形貌的影响。结果表明,硅质原料前驱体形态决定了水热合成产物的形貌。基于产物不同形貌特征,探讨并对比了硬硅钙石晶须和球形粒子生成机理及水热反应过程。硬硅钙石晶须和球形粒子生成分别按溶解-沉淀反应机理和原位转变机理进行。在CaO-SiO2-H2O反应体系中,CaO:SiO2(mol)=1.0,硬硅钙石晶体反应过程可描述为:非晶态C-S-H凝胶→富钙C-S-H(II)→富硅C-S-H(I)→硬硅钙石。基于硬硅钙石晶体反应过程,建立了相应动力学关系式:硬硅钙石晶须为? dc A /dt = kcA4/5,球形粒子为? dc A /dt = kcA0.9。依此动力学关系式和近藤氏模型计算得到硬硅钙石晶须和球形粒子表观活化能分别为75-77 kJ·mol-1、77-84 kJ·mol-1。动力学分析结果表明了硬硅钙石晶体生长机理及反应过程的正确性。
对各工艺参数条件下制备的硬硅钙石晶须材料微观结构进行了全面分析。结果表明:以CaCl2和100g·L-1KOH溶液混合制得Ca(OH)2悬浮液为钙源,K2SiO3溶液为硅源,体系pH=12.6,反应物浓度为0.05mol·L-1,在225℃保温15 h的条件下水热合成硬硅钙石晶须结晶良好、热稳定性较好、长径比可达50-100。重点分析了杂质及含量对水热合成产物微观结构的影响。以CaCl2为钙源引入Cl-离子,控制Na2O含量小于5%,Al2O3含量小于1%有利于硬硅钙石晶须的制备。
创新性地以电石渣为原料制备硬硅钙石晶体。鉴于不同水热产物形貌对原料提出的特殊要求,以酸洗除杂技术对电石渣进行预处理,并用于制备硬硅钙石晶须,确定了适宜制备工艺参数为酸洗pH=8.0,225℃保温15 h。分别以煅烧和超声技术对电石渣进行预处理,并用于制备硬硅钙石球形粒子,确定了适宜制备工艺参数为:以800℃保温2 h煅烧电石渣,12倍80℃去离子水搅拌30 min制备Ca(OH)2乳液为钙质原料,或以160 W超声3 h预处理电石渣为钙质原料,钙硅摩尔比为1.0,水固比为28:1,升温阶段搅拌速度400 rpm,保温阶段搅拌速度150 rpm,215℃保温10 h。
针对水热合成硬硅钙石及晶体生长特点,采用“外掺增强法”及“晶须原位生长增强法”制备工艺,实现超轻质硅酸钙材料的补强增韧。采用“外掺增强法”时,适宜的制备工艺参数为:长径比50-100硬硅钙石晶须掺量5%,成型压力为0.5 MPa,脱模75℃烘干12 h,制得容重109 Kg·m-3增强体制品抗折、抗压强度分别为0.37 MPa和0.59 MPa。采用“晶须原位生长增强法”时,适宜的制备工艺参数为:以K2SiO3:H2SiO3(mol)=2:1为硅质原料,在225℃保温15 h条件下进行水热合成反应,成型压力为0.5 MPa,脱模75℃烘干12 h,制得容重为118 Kg·m-3的增强体制品抗折、抗压强度分别为0.42 MPa、0.66 MPa。以3%玻璃纤维制得制品的比强度值Specific strengthF和Specific strengthC分别为2.22×103 cm和3.65×103 cm,以5%硬硅钙石晶须制得制品比强度值Specific strengthF和Specific strengthC分别为3.40×103 cm和5.41×103 cm。以硬硅钙石晶须为增强材料制得制品具有更低容重,更高比强度和更好保温隔热性能。
Ultra-light material of calcium silicate has been widely used in industry for its low thermal conductivity, wide applying temperature range and low density. However, it was limited due to the disadvantage of mechanical properties. Xonotlite whiskers, which are required in the development of modern composite materials, have been attracting attention as a kind of strengthening and toughening materials. The xonotlite whiskers and spherical particles were synthesized using the hydrothermal synthesis method, and the ultra-light material of calcium silicate had been strengthened with the methods of“adding reinforcing agent”and“whisker in–situ growth”respectively.
In this paper, xonotlite crystal was firstly prepared by the hydrothermal synthesis method, and the effect of raw materials and hydrothermal synthetic technologies on the morphology of xonotlite was also studied. The results indicated that the morphologies of hydrothermal synthesis products were determined by the precursor states of kiesel materials. Base on the different morphology characteristics of the products, the growth mechanism and reaction mechanism of xonotlite whiskers and spherical particles were explored, and the growth of xonotlite whiskers and spherical particles were accorded with the dissolution-precipitation mechanism and in situ transformation mechanism. In the CaO-SiO2-H2O system, the reaction mechanism of xonotlite crystal was described as follows while having CaO:SiO2(mol)=1.0: amorphous C-S-H gel→calcium-rich C-S-H(II)→silicon-rich C-S-H(I)→xonotlite. The kinetics formulas of xonotlite whiskers and spherical particles were found based on the reaction mechanism of xonotlite crystal: ? dc A /dt = kcA4/5 is for xonotlite whiskers and ? dc A /dt = kcA0.9 is for xonotlite spherical particles. At last, the apparent activation energy of xonotlite whiskers and spherical particles are 75-77 kJ·mol-1 and 77-84 kJ·mol-1 respectively through those kinetics formulas and Kondo model. The anlysis results of kinetics indicated that the growth and reaction mechanisms of xonotlite crystal are correct.
The microstructures of xonotlite whiskers prepared at different process parameters were analyzed comprehensively. The results showed that the xonotlite whiskers, which are of well crystallized, excellent thermal stability and aspect ratio of 50-100, were synthesized by hydrothermal processing with Ca(OH)2 suspension which was prepared by using CaCl2 and 100g·L-1KOH solution as calcareous material and K2SiO3 solution as kiesel materials, controlling the system of pH=12.6 and reactant concentration of 0.05mol·L-1 at 225℃for 15 h. The effect of impurities and its content on the morphologies of hydrothermal synthesis products was studied mainly in this paper, and adding Cl- ions when using CaCl2 as calcareous material, controlling the Na2O content less than 5% and Al2O3 content less than 1% are beneficial to the preparation of xonotlite whiskers.
The xonotlite crystal was prepared for the first time using the carbide slag as raw material. The requirements of raw materials are different attributed to the different morphologies of hydrothermal synthesis products, and then the xonotlite whiskers were synthesized from the carbide slag which was pretreated by the way of pickling under the conditions of pH=8.0 when pickling, at 225℃for 15 h, which are the best process parameters in this paper. The xonotlite spherical particles were prepared from the carbide slag which was pretreated by the methods of calcination and ultrasonic technologies respectively, under the conditions of using Ca(OH)2 suspension which was prepared from the carbide slag calcined at 800℃for 2 h and digested by the deionized water of 12 times and 80℃for 30 min as calcareous material, or using the carbide slag slurry at 160 W ultrasonic for 3 h as calcareous material, CaO/SiO2 mol ratio 1.0, water/solid weight ratio of 28:1, stirring speed of 400 rpm and 150 rpm when heating and reaction stage respectively, at 215℃for 10 h.
Base on the growth characteristics of xonotlite crystal, the ultra-light material of calcium silicate was strengthened with the methods of“adding reinforcing agent”and“whisker in–situ growth”respectively. The product of 109 Kg·m-3 was prepared under the conditions of aspect ratio of 50-100, whiskers mixing amount of 5%, forming pressure of 0.5 MPa, demould and drying at 75℃for 12 h, and its flexural and compressive strength are 0.37 MPa and 0.59 MPa respectively when having the method of“adding reinforcing agent”. The product of 118 Kg·m-3 was prepared under the conditions of K2SiO3/H2SiO3 mol ratio 2.0, hydrothermal treatment proceeded at 225℃for 15 h, forming pressure of 0.5 MPa, demould and drying at 75℃for 12 h, and its flexural and compressive strength are 0.42 MPa and 0.66 MPa respectively when having the method of“whisker in–situ growth”. The specific strengthF and specific strengthC of the products prepared by adding glass fibers of 3% are 2.22×103 cm and 3.65×103 cm respectively, and the specific strengthF and specific strengthC of the products prepared by adding xonotlite whiskers of 5% are 3.40×103 cm and 5.41×103 cm respectively. The results indicated that the product prepared by adding xonotlite whiskers is of lower density, higher specific strength and well thermal insulation performance.
引文
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