纳米TiO_2及其纳米复合粉体的制备与改性水性塑胶涂料的研究
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摘要
本文主要包括三方面的内容：
1.以工业级硫酸氧钛为原料采用溶胶凝胶水热法复合新工艺制备纳米TiO_2粉体，通过利用IR、XRD、TEM、SEM等手段对样品进行测试分析，研究了各种工艺条件对纳米TiO_2结构及分散性能的影响并初步探讨有关机理。实验结果表明：最佳工艺条件为：溶胶阶段：H+/TiO_2为0.8，TiO_2浓度0.5mol/l，胶溶温度90oC，胶溶时间为90min。水热的最佳条件为：水热温度170oC，水热时间5h，反应釜填充度80%；煅烧的最佳工艺条件为：采用NH4NO3为盐处理剂，煅烧温度350oC，煅烧时间1.5h，钛盐比为1:5；纳米TiO_2为球状；煅烧前晶型以锐钛型为主，粒径在2030nm；煅烧后纳米TiO_2的晶型逐渐为金红石型，粒径在7090nm；纳米TiO_2粉体在水溶液中具有较好的分散性。
2.以自制的自分散型纳米TiO_2，γ AlOOH和纳米SiO_2为复合原料，采用物理复合和原位复合工艺成功地制备了纳米TiO_2AlOOH、TiO_2SiO_2、TiO_2AlOOH SiO_2纳米复合粉体，通过IR、TEM、SEM等手段对样品进行测试分析，研究了纳米复合粉体的复合形式、外观形状、结构尺寸以及在水溶液中的分散情况。结果表明：制得的纳米复合粉体，不只是简单的物理混合，有一定程度的化学复合；复合粉体在水中的分散稳定性比未复合的纳米TiO_2较好；部分粒子聚合形成胶束，但粒子之间只是简单的聚合，并没有形成完成的化学结构，属于软团聚。
3.用HS6100005水性塑胶漆为原料，采用液相准均相溶胶共混复合法，成功制备了纳米TiO_2/水性塑胶复合涂料、纳米TiO_2AlOOH/水性塑胶复合涂料、纳米TiO_2SiO_2/水性塑胶复合涂料、TiO_2AlOOH SiO_2/水性塑胶复合涂料。通过利用IR、XRD、TEM、SEM等手段对样品进行测试分析，研究了纳米粒子在涂料中的分布以及纳米粒子和涂料的复合形式。结果表明：纳米粉体以球状形式，较为均匀地分散在涂料当中，分散粒径在6090nm；纳米粒子和涂料之间的复合，存在着部分化学键的结合。纳米复合涂料的性能测试结果表明：纳米复合涂料各方面的性能都符合水性塑胶涂料的技术要求，并在硬度和耐磨性方面有了一定的提高。
This article consists of three aspects:
1. nano TiO_2powder has been synthesized using sol gel hydrothermalmethod. The variety of process conditions on the impact of nano TiO_2structureand dispersion properties and the mechanism have benn studied by the analysisof the samples by IR, XRD, TEM, SEM. The experimental results show that theoptimum conditions are: sol stage, H+/TiO_2is0.8, the TiO_2concentration is0.5mol/l, the temperature is90℃， the peptization time is90min. Hydrothermaloptimal conditions: the hydrothermal temperature170℃, the hydrothermal time is5h, the reactor filling degree is80%; calcined optimum process conditions: usingNH4NO3as the salt processing agent, the calcination temperature is350℃, thecalcination time is1.5h, the titanium salt rate is1:5; nano TiO_2powder in aqueoussolutiona have a certain degree of dispersion.
2. The nano TiO_2AlOOH, TiO_2SiO_2, TiO_2AlOOH SiO_2nano compositepowders have been Successfully prepared, using self dispersed nanoTiO_2，nano γ AlOOH and nano SiO_2as the composite materials, by the method ofpHysical composite and in situ composite technology. The compound in the formof nano composite powders, the appearance of the shape, structure, size anddispersed in aqueous solution of samples were tested and analyzed through the useof the means of the IR, TEM, SEM. The results showed that: the obtainednanocomposite powder, not simply pHysical mixing, there is a certain degree ofchemical compound; the dispersion stability of the composite powder in the waterbetter than the non composite TiO_2nanoparticles; composite powders arespHerical structure, some particles aggregate to form micelles, but simpleaggregation between the particles, and did not form the completion of the chemicalstructure of a soft reunion.
3. Nano TiO_2/waterborne composite coatings for plastic, nano TiO_2AlOOH/waterborne composite coatings for plastic, nano TiO_2SiO_2/wa terbornecomposite coatings for plastic, TiO_2AlOOH SiO_2/waterborne composite coatings for plastic have been synthesised using HS6100005plastic water based paint asraw material, and liquid pHase quasi homogeneous sol blends complex methold.The distribution of nanoparticles in paint and coating nanoparticles and compositeform of sample were studied by using IR, XRD, TEM, SEM etc. The results showthat: the nanometer powder in the globular form is uniformly dispersed in thecoating, dispersed particle size in the6090nm; the composition betweennanoparticles and coating exist some chemical bonding. Nanocomposite coatingperformance results show that: the performance of all aspects of thenano composite coatings meet the technical requirements of the water basedplastic coatings, and have a certain improvement in the hardness and wearresistance.
1.以工业级硫酸氧钛为原料采用溶胶凝胶水热法复合新工艺制备纳米TiO_2粉体，通过利用IR、XRD、TEM、SEM等手段对样品进行测试分析，研究了各种工艺条件对纳米TiO_2结构及分散性能的影响并初步探讨有关机理。实验结果表明：最佳工艺条件为：溶胶阶段：H+/TiO_2为0.8，TiO_2浓度0.5mol/l，胶溶温度90oC，胶溶时间为90min。水热的最佳条件为：水热温度170oC，水热时间5h，反应釜填充度80%；煅烧的最佳工艺条件为：采用NH4NO3为盐处理剂，煅烧温度350oC，煅烧时间1.5h，钛盐比为1:5；纳米TiO_2为球状；煅烧前晶型以锐钛型为主，粒径在2030nm；煅烧后纳米TiO_2的晶型逐渐为金红石型，粒径在7090nm；纳米TiO_2粉体在水溶液中具有较好的分散性。
2.以自制的自分散型纳米TiO_2，γ AlOOH和纳米SiO_2为复合原料，采用物理复合和原位复合工艺成功地制备了纳米TiO_2AlOOH、TiO_2SiO_2、TiO_2AlOOH SiO_2纳米复合粉体，通过IR、TEM、SEM等手段对样品进行测试分析，研究了纳米复合粉体的复合形式、外观形状、结构尺寸以及在水溶液中的分散情况。结果表明：制得的纳米复合粉体，不只是简单的物理混合，有一定程度的化学复合；复合粉体在水中的分散稳定性比未复合的纳米TiO_2较好；部分粒子聚合形成胶束，但粒子之间只是简单的聚合，并没有形成完成的化学结构，属于软团聚。
3.用HS6100005水性塑胶漆为原料，采用液相准均相溶胶共混复合法，成功制备了纳米TiO_2/水性塑胶复合涂料、纳米TiO_2AlOOH/水性塑胶复合涂料、纳米TiO_2SiO_2/水性塑胶复合涂料、TiO_2AlOOH SiO_2/水性塑胶复合涂料。通过利用IR、XRD、TEM、SEM等手段对样品进行测试分析，研究了纳米粒子在涂料中的分布以及纳米粒子和涂料的复合形式。结果表明：纳米粉体以球状形式，较为均匀地分散在涂料当中，分散粒径在6090nm；纳米粒子和涂料之间的复合，存在着部分化学键的结合。纳米复合涂料的性能测试结果表明：纳米复合涂料各方面的性能都符合水性塑胶涂料的技术要求，并在硬度和耐磨性方面有了一定的提高。
This article consists of three aspects:
1. nano TiO_2powder has been synthesized using sol gel hydrothermalmethod. The variety of process conditions on the impact of nano TiO_2structureand dispersion properties and the mechanism have benn studied by the analysisof the samples by IR, XRD, TEM, SEM. The experimental results show that theoptimum conditions are: sol stage, H+/TiO_2is0.8, the TiO_2concentration is0.5mol/l, the temperature is90℃， the peptization time is90min. Hydrothermaloptimal conditions: the hydrothermal temperature170℃, the hydrothermal time is5h, the reactor filling degree is80%; calcined optimum process conditions: usingNH4NO3as the salt processing agent, the calcination temperature is350℃, thecalcination time is1.5h, the titanium salt rate is1:5; nano TiO_2powder in aqueoussolutiona have a certain degree of dispersion.
2. The nano TiO_2AlOOH, TiO_2SiO_2, TiO_2AlOOH SiO_2nano compositepowders have been Successfully prepared, using self dispersed nanoTiO_2，nano γ AlOOH and nano SiO_2as the composite materials, by the method ofpHysical composite and in situ composite technology. The compound in the formof nano composite powders, the appearance of the shape, structure, size anddispersed in aqueous solution of samples were tested and analyzed through the useof the means of the IR, TEM, SEM. The results showed that: the obtainednanocomposite powder, not simply pHysical mixing, there is a certain degree ofchemical compound; the dispersion stability of the composite powder in the waterbetter than the non composite TiO_2nanoparticles; composite powders arespHerical structure, some particles aggregate to form micelles, but simpleaggregation between the particles, and did not form the completion of the chemicalstructure of a soft reunion.
3. Nano TiO_2/waterborne composite coatings for plastic, nano TiO_2AlOOH/waterborne composite coatings for plastic, nano TiO_2SiO_2/wa terbornecomposite coatings for plastic, TiO_2AlOOH SiO_2/waterborne composite coatings for plastic have been synthesised using HS6100005plastic water based paint asraw material, and liquid pHase quasi homogeneous sol blends complex methold.The distribution of nanoparticles in paint and coating nanoparticles and compositeform of sample were studied by using IR, XRD, TEM, SEM etc. The results showthat: the nanometer powder in the globular form is uniformly dispersed in thecoating, dispersed particle size in the6090nm; the composition betweennanoparticles and coating exist some chemical bonding. Nanocomposite coatingperformance results show that: the performance of all aspects of thenano composite coatings meet the technical requirements of the water basedplastic coatings, and have a certain improvement in the hardness and wearresistance.
引文
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