红外反射氧化铬绿颜料产品制备工艺研究
文献类型：学位论文
| 作者 | 周祯 |
| 学位类别 | 硕士 |
| 答辩日期 | 2012-05-24 |
| 授予单位 | 中国科学院研究生院 |
| 导师 | 徐红彬 ; 李平 ; 张红玲 |
| 关键词 | 红外反射颜料 氧化铬绿 亚熔盐 铬酸酐 铬酸钾 掺杂 |
| 其他题名 | Technical Research On Preparation Process For Infrared Reflection Chromic Oxide Pigment Product |
| 学位专业 | 化学工程 |
| 中文摘要 | 红外反射氧化铬绿颜料，因其优异的红外反射性能，具有隔热降温、环保节能的效果，可有效削减城市热岛效应，成为新型特种涂料，在建筑行业得到广泛应用；同时，因其在可见光区显示绿色，具有仿叶绿素功能，在国防军事等领域也具有较好的应用前景。本文以制备高性能红外反射氧化铬绿颜料为目标，在对现有工业铬酸酐热分解工艺进行优化的基础上，研究红外反射氧化铬绿颜料的制备工艺条件和相关机理，并应用于亚熔盐法铬盐清洁工艺与集成技术铬酸钾低温氢还原法氧化铬绿制备新工艺过程，对提高氧化铬绿产品的红外反射性能的方法进行了系统研究。本文主要取得了以下创新性进展：（1）优化了铬酸酐热分解工艺，拓展了氧化铬绿产品的色度范围，有效提高了产品的红外反射性能。以铬酸酐为原料，通过优化热分解温度、热分解时间、投料方式等煅烧工艺条件获得了不同颜色性能的氧化铬绿颜料，使氧化铬绿产品颜色由蓝相到黄相。研究发现，不同的热分解温度导致粒径变化，从而影响红外反射率，在最优制备工艺条件（热分解温度1250 ℃、热分解时间0.5 h）下，氧化铬绿产品的红外反射率超过90%；（2）在最优热分解工艺条件下，研究了掺杂不同添加剂烧结后对氧化铬绿产品红外反射性能的影响规律和机理，通过掺杂V2O5烧结，氧化铬绿产品的最高反射率可达98%。研究发现，随着V2O5或TiO2添加量的增加，红外反射率先增加后减少；随着CuO添加量的增加，红外反射率逐渐减少；红外反射率，电导率和介电常数三者具有一致变化规律。机理分析结果表明，氧化铬本征导电类型为空穴导电，掺杂V2O5或TiO2以后导电类型会发生改变；反之，掺杂CuO会加强空穴导电的能力。伴随着电阻率的变化，氧化铬吸收和反射光子的能力改变，从而导致红外反射率的变化。（3）在铬酸酐热分解法红外反射氧化铬绿颜料制备工艺研究基础上，对铬酸钾低温氢还原法红外反射氧化铬绿颜料制备工艺进行了深入研究。以K2CrO4氢还原产物经水解并洗涤回收KOH后得到的中间产物为原料，通过组分调控、掺杂煅烧等手段制备出了红外反射氧化铬绿颜料。在煅烧温度1150 ℃，煅烧时间30 min条件下，通过添加0.7 g P2O5和0.7 gTiO2，形成KCrPO7相和(Cr,Ti)2O3相，制备出的氧化铬绿产品最高反射率可达70%，满足商业产品红外反射性能指标；同时，该产品色度值为L*=40.43，a*=12.56，b*=12.16，C*=17.48，颜色性能优异。 |
| 英文摘要 | Infrared reflection chrome oxide green pigment, due to its high infrared reflection, excellent heat insulation, and environmentally friendly energy-saving effect, is capable of effectively reducing the urban heat island effect and finds its wide application in construction industry. Morever, the unique chlorophyll imitation function enables its application in the national defense and military fields. With the objective of preparing infrared reflection chrome oxide green pigments, the process optimization of the industrially employed thermal decomposition process of chromic anhydride was firstly investigated. On its basis, the preparation process of infrared reflection chromic oxide green pigments via the hydrogen reduction method of chromate potassium was systematically developed, and the product engineering of the integrated technology and clean process for manufacturing chromium compounds with SMS media was further extended. The following innovative progresses were achieved in this work: (1)The thermal decomposition process of chromic anhydride was optimized, the color performance of chromic oxide green pigments was improved, and the infrared reflection of the products was raised as well. Through the optimization of the thermal decomposition temperature, decomposition time, and feeding mode, chromic oxide green pigments with different color properties were prepred and the color range was extended from the original blue phase to the yellow phase. It was found that, the particle sizes, as well as the reflectance, of the chromic oxide green pigment are dependent on the decomposition temperature. Under the optimized conditions, 1250 ℃ and 0.5 h of the decomposition temperature and time, respectively, the infrared reflectivity of the obtained products can be achieved as high as 90%. (2) The influence and mechanism of sinstering with impurity doping with different impurities was investigated under the optimized conditions of the thermal decomposition of chromium anhydride. The maximum infrared reflectivity of the chromium oxide green pigment obtained by sinstering of chromic oxide green with doping of the V2O5 impurity, was achieved even 98% approximately. It was found that, as the contents of the V2O5 or TiO2 impurity increases, the reflectance firstly increases and then decreases; while as the content of the CuO impurity increases, the reflectance decreases. The reflectance, conductivity and the dielectric constant have the same tendency. In principle, the intrinsic conductive type of chromium oxide is hole conductive. The conductive type was changed when V2O5 or TiO2 was doped. Conversely, CuO will strengthen the ability of hole conduction. According to the band theory, due to the change of resistivity, the capability of absorptive or reflective photon of chromic oxide was also changed, therefore leading to the change of the reflectance. (3)On the above basis, the preparation process of infrared reflection chromic oxide green pigment via the hydrogen reduction method of K2CrO4 was investigated in detail. Through the component control of the intermediate product, which is obtained by the hydrolysis of the hydrogen reduction products with the produced KOH washed off, impurity doping during the calcination process, infrared reflection chromic oxide green pigment was prepared. When the intermediate product was calcinated for 0.5 h at 1150 ℃ with droping 0.7 g of P2O5 and 0.7 g of TiO2, the maximum reflectivity of the chromic oxide green pigement was raised up to 70%, probably resulting from the fact that the formed KCrPO7 phase and (Cr, Ti)2O3 phase improved the infrared reflectance of chrome oxide green pigments. Furthermore, the chromatic value of L*= 40.43, a*= 12.56, b*=12.16, C*=17.48 implies its excellent color perfoemance. |
| 语种 | 中文 |
| 公开日期 | 2013-09-25 |
| 源URL | [http://ir.ipe.ac.cn/handle/122111/1834]  |
| 专题 | 过程工程研究所_研究所（批量导入） |
| 推荐引用方式 GB/T 7714 | 周祯. 红外反射氧化铬绿颜料产品制备工艺研究[D]. 中国科学院研究生院. 2012. |
入库方式： OAI收割
来源：过程工程研究所
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