新型无机功能材料的制备与表征
摘要
纳米材料晶粒在磁、光、电、热、力及化学等方面具有独特的性能,新型功能纳米材料在工业发展的各个领域都有着广泛的应用和前景。层状化合物是一类新的纳米结构材料,由于其结构的特殊性,本身可以认为是一种特殊的纳米结构,同时可作为制备无机-无机、无机-有机纳米复合材料的母体材料。
近年来,随着工农业的发展,环境水污染日益严重,环境科学家致力于研究和开发各种新型环境材料。作为变价金属氧化物之一的锰氧化物,近年来在降解水环境中的污染物方面已显示出巨大的潜能。
本文第一篇的主要研究内容是采用不同的分析测试手段对新方法制备的新型混凝剂的结构进行表征和分析,从结构改变的本质上研究其混凝机理。同时通过混凝效能的对比实验证实使用新型混凝剂可以大大提高混凝效果。论文采用硫酸亚铁和高锰酸钾反应制备新型混凝剂,在同样的投加量的情况下,新型混凝剂对水中的污染物具有更好的去除效果。利用XRD、BET、FTIR、XPS、SEM等分析方法对制得的产物进行了表征。结果表明,新型混凝剂是铁锰氧的复合金属氧化物,表面含有大量的羟基,利用N_2吸附法测得其BET比表面积为153.03g/m~2,结构上具有更多的化学活性位点。结合XRD晶相鉴定,新型混凝剂主体为δ-MnO_2依然具备其层状结构而铁的氧化物为无定形态。通过XPS定量分析和金属含量的分析进一步确定了新型混凝剂表面以δ-MnO_2为主体内层主要为氢氧化铁的结构。该结构使得新型混凝剂表面带有更多的正电荷,更容易与带电粒子发生强烈的吸附,使更多的带电的胶体粒子在相对更大的范围内聚结形成以新型混凝剂粒子为絮凝中心的较大的凝聚体而混凝沉降。结合混凝效能的对比实验研究,进一步验证了新型混凝剂具有优异的混凝效能。
高岭土主要用于造纸、橡胶、陶瓷、颜料、水泥、建材、耐火材料等行业。高岭土一些特征参数包括比表面积、亮度、晶粒的大小和形状直接决定其在技术上的应用性。若能在较短时间内,成功使高岭石剥片达到纳米级别,将会带来工业上的革新,产生良好的效益。
论文第二篇采用微波剥离水合肼插层高岭土的方法,在短时间内可将高岭土的的晶粒厚度从原土的30 nm减小到剥离后的8.6 nm,剥离效果显著提高。经XRD,SEM等表征手段,证实了高岭土剥片变薄,颗粒变小,片层的径厚比明显。经FTIR和TG-DTA分析表明,高岭土剥离后出现了两个失重台阶(100-400℃和>400℃),初始的脱羟基温度也从原土的530℃降低为510℃。同时,高岭土总的失重率也从原土的11.3%增大为13.4%。论文还系统考察了不同因素对新方法剥离效果的影响,结果表明高岭土剥片的晶粒厚度随着高岭土-水合肼插层复合物插层率的增大而减小。
Nanomaterials have the unique performance in different properties such as the aspects of magnetic,light,electricity,heat,power and chemicals.New functional nanomaterials have a wide range of applications and prospects in all fields of industrial development.Layered compounds is a new type of nano-structured materials,as a result of the specificity of its structure,it can be regarded as a special kind of nano-structure material.At the same it can also be the matrix of the preparation of inorganic-inorganic, inorganic-organic nanocomposite.
Recently,with the development of industrial and agricultural,the environmental pollution especially the contamination of water becomes more and more serious.Environmental scientists committed to research and develop a variety of new environmental materials.As one of the most important metals oxide,manganese oxides have shown great potential in degradation of the water pollutants in recent years.
In this paper,different means were used to test the novel coagulant in order to make clear of the flocculent mechanism from the quite basic structure,the effectiveness of the novel coagulant was confirmed through coagulation experiments which indicate that the coagulation effect has been greatly enhanced.
A-novel coagulant which has an outstanding coagulation effect and a better ability to remove contamination from water was prepared by FeSO_4 and KMnO_4.XRD,BET,FTIR,XPS,SEM and other analytical methods were used to characterize the product.The result indicated that,the novel coagulant is an oxygen-rich ferromanganese metal oxide,containing a large number of surface hydroxyl groups and the Obtained specific surface area is 153.03g/m~2 which proves abundant active sites on the surface.Combined with the XRD identification,the crystal form for the novel coagulant wasδ-MnO_2 with the layered structure and the state of the ferric hydroxide was amorphous.XPS quantitative analysis and the metal content analysis further identified that the basic surface structure of the coagulant was that theδ-MnO_2 stated as the main body which coated with a relatively small amount of ferric hydroxide.This structure can make more positive charge on the surface of the novel coagulant and it is easy to form a strong adsorption with the particles in the water thus formed a new particle Center for the flocculation and made it easy to shape the particles into network structure in the water.The experimental studies may further validate that the new coagulant has excellent coagulation performance.
Kaolinite[Al_2Si_2O_5(OH)_4]is a kind of layered silicate material.The thickness,specific surface area,brightness and structure of kaolinite particles significantly affect their dispersibility,agglomeration and rheological properties,whenever kaolinite is used as a coating,pigment paper,ceramics,rubber,refractory materials or polymers etc.Therefore,the rapid delamination of kaolinite is very important,which will result in the industrial innovation and produce good economic benefits.
This work presents a novel method of microwave to delaminate kaolinite rapidly.It is found that the treatment with microwave can delaminate kaolinite more effectively in a short time.And the thickness decreases to 8.6 nm from 30 nm for raw kaolinite.Study on the changes of functional groups and thermal decomposition behavior were investigated. The microwave caused the loss of some OH groups due to the prototropy. The TG curve shows a two-step weight loss(100～400℃and＞400℃).The initial dehydroxylation temperature also decreases to 510℃from 530℃and the total mass loss also increases to 13.4%from 11.3%.The research of factors affecting the delamination also had been carried out.The thickness of kaolinite decreases with the increase of intercalation ratio.
近年来,随着工农业的发展,环境水污染日益严重,环境科学家致力于研究和开发各种新型环境材料。作为变价金属氧化物之一的锰氧化物,近年来在降解水环境中的污染物方面已显示出巨大的潜能。
本文第一篇的主要研究内容是采用不同的分析测试手段对新方法制备的新型混凝剂的结构进行表征和分析,从结构改变的本质上研究其混凝机理。同时通过混凝效能的对比实验证实使用新型混凝剂可以大大提高混凝效果。论文采用硫酸亚铁和高锰酸钾反应制备新型混凝剂,在同样的投加量的情况下,新型混凝剂对水中的污染物具有更好的去除效果。利用XRD、BET、FTIR、XPS、SEM等分析方法对制得的产物进行了表征。结果表明,新型混凝剂是铁锰氧的复合金属氧化物,表面含有大量的羟基,利用N_2吸附法测得其BET比表面积为153.03g/m~2,结构上具有更多的化学活性位点。结合XRD晶相鉴定,新型混凝剂主体为δ-MnO_2依然具备其层状结构而铁的氧化物为无定形态。通过XPS定量分析和金属含量的分析进一步确定了新型混凝剂表面以δ-MnO_2为主体内层主要为氢氧化铁的结构。该结构使得新型混凝剂表面带有更多的正电荷,更容易与带电粒子发生强烈的吸附,使更多的带电的胶体粒子在相对更大的范围内聚结形成以新型混凝剂粒子为絮凝中心的较大的凝聚体而混凝沉降。结合混凝效能的对比实验研究,进一步验证了新型混凝剂具有优异的混凝效能。
高岭土主要用于造纸、橡胶、陶瓷、颜料、水泥、建材、耐火材料等行业。高岭土一些特征参数包括比表面积、亮度、晶粒的大小和形状直接决定其在技术上的应用性。若能在较短时间内,成功使高岭石剥片达到纳米级别,将会带来工业上的革新,产生良好的效益。
论文第二篇采用微波剥离水合肼插层高岭土的方法,在短时间内可将高岭土的的晶粒厚度从原土的30 nm减小到剥离后的8.6 nm,剥离效果显著提高。经XRD,SEM等表征手段,证实了高岭土剥片变薄,颗粒变小,片层的径厚比明显。经FTIR和TG-DTA分析表明,高岭土剥离后出现了两个失重台阶(100-400℃和>400℃),初始的脱羟基温度也从原土的530℃降低为510℃。同时,高岭土总的失重率也从原土的11.3%增大为13.4%。论文还系统考察了不同因素对新方法剥离效果的影响,结果表明高岭土剥片的晶粒厚度随着高岭土-水合肼插层复合物插层率的增大而减小。
Nanomaterials have the unique performance in different properties such as the aspects of magnetic,light,electricity,heat,power and chemicals.New functional nanomaterials have a wide range of applications and prospects in all fields of industrial development.Layered compounds is a new type of nano-structured materials,as a result of the specificity of its structure,it can be regarded as a special kind of nano-structure material.At the same it can also be the matrix of the preparation of inorganic-inorganic, inorganic-organic nanocomposite.
Recently,with the development of industrial and agricultural,the environmental pollution especially the contamination of water becomes more and more serious.Environmental scientists committed to research and develop a variety of new environmental materials.As one of the most important metals oxide,manganese oxides have shown great potential in degradation of the water pollutants in recent years.
In this paper,different means were used to test the novel coagulant in order to make clear of the flocculent mechanism from the quite basic structure,the effectiveness of the novel coagulant was confirmed through coagulation experiments which indicate that the coagulation effect has been greatly enhanced.
A-novel coagulant which has an outstanding coagulation effect and a better ability to remove contamination from water was prepared by FeSO_4 and KMnO_4.XRD,BET,FTIR,XPS,SEM and other analytical methods were used to characterize the product.The result indicated that,the novel coagulant is an oxygen-rich ferromanganese metal oxide,containing a large number of surface hydroxyl groups and the Obtained specific surface area is 153.03g/m~2 which proves abundant active sites on the surface.Combined with the XRD identification,the crystal form for the novel coagulant wasδ-MnO_2 with the layered structure and the state of the ferric hydroxide was amorphous.XPS quantitative analysis and the metal content analysis further identified that the basic surface structure of the coagulant was that theδ-MnO_2 stated as the main body which coated with a relatively small amount of ferric hydroxide.This structure can make more positive charge on the surface of the novel coagulant and it is easy to form a strong adsorption with the particles in the water thus formed a new particle Center for the flocculation and made it easy to shape the particles into network structure in the water.The experimental studies may further validate that the new coagulant has excellent coagulation performance.
Kaolinite[Al_2Si_2O_5(OH)_4]is a kind of layered silicate material.The thickness,specific surface area,brightness and structure of kaolinite particles significantly affect their dispersibility,agglomeration and rheological properties,whenever kaolinite is used as a coating,pigment paper,ceramics,rubber,refractory materials or polymers etc.Therefore,the rapid delamination of kaolinite is very important,which will result in the industrial innovation and produce good economic benefits.
This work presents a novel method of microwave to delaminate kaolinite rapidly.It is found that the treatment with microwave can delaminate kaolinite more effectively in a short time.And the thickness decreases to 8.6 nm from 30 nm for raw kaolinite.Study on the changes of functional groups and thermal decomposition behavior were investigated. The microwave caused the loss of some OH groups due to the prototropy. The TG curve shows a two-step weight loss(100～400℃and＞400℃).The initial dehydroxylation temperature also decreases to 510℃from 530℃and the total mass loss also increases to 13.4%from 11.3%.The research of factors affecting the delamination also had been carried out.The thickness of kaolinite decreases with the increase of intercalation ratio.
引文
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