KMnO_4、KClO_3等无机固体的热分解
摘要
固体的热分解反应是固体化学的重要研究领域,具有十分广阔的应用背景。很多无机盐产品的生产过程都包含碳酸盐、碱式碳酸盐和硫酸盐等原料或中间产物的煅烧分解工序。探明固体热分解机理,取得高效、适用的催化剂,对于相关产品的生产工艺改革、节能降耗、增加效益等有重要实际意义。CaCO_3是硅酸盐水泥生产中重要的工业原料,它的分解温度对水泥的能耗与质量具有重要的影响。另外,CaCO_3分解反应为一种典型的气固反应,对其反应动力学的研究有助于揭示并建立这一类反应的完整物理化学图景。可以通过对CaCO_3热分解机理尤其是催化热分解机理的研究来加深对固体热分解规律的认识,寻求CaCO_3热分解的高效催化剂并尽快投入应用;同时有助于增加对BaSO_4的热分解规律的认识,推进各种钡盐生产工艺的改革。
鉴于CaCO_3、BaSO_4等热分解研究的较大难度和对实验条件较高的要求,我们经过长时间认真思考后,决定从一些较常见的、有相似性的、易分解的无机固体开始(实为进入科研启动阶段),熟悉有关的基础理论和研究手段,提高研究能力,积累研究经验,明确并创造研究条件,最终很好地展开、完成这一艰难、巨大的研究开发课题。对于无机固体的热分解,KMnO_4和KClO_3的热分解是人们再也熟悉不过的实例。但我们通过大量认真细致的调研,竟然发现有关的反应机理完全不清楚。为此我们选择从研究KMnO_4、KClO_3的热分解入手,在深厚、宽广的理论基础上,设计、完成了一系列巧妙、新颖的实验,取得一些重要发现。主要工作如下:
1总结了国内外KClO_3、CaCO_3热分解研究的进展及热分析动力学方法,指出了不足之处,提出了有待解决的问题。
2采用马弗炉把KMnO_4在一定温度下长时间加热,测定KMnO_4热分解失重率,根据是否失重确定其分解温度,发现KMnO_4热分解温度与其结晶状况有关,分解温度为190℃,不是文献中所载的240℃。首次提出了KMnO_4热分解机理。
3配制ClO_3~-和微量ClO_2~-混合存在的溶液,ρ(ClO_3~-) = 34.1g/L,ρ(ClO2-) = 208mg/L,尝试以碘量法直接测定其中亚氯酸根离子的含量。考察测定条件及向待测溶液中添加ClO_4~-对分析结果的影响,确定了方法的测定程序、精密度、准确度和该方法可以较方便检测的最低ClO_2~-浓度。测定过程的关键之处是使用约0.5mol/L的盐酸来调节待测溶液的pH值。
4认真研究了KClO_3热分解行为,发现学者们对KClO_3热分解温度和机理模型有不同看法。我们课题组在各个温度下对KClO_3长时间加热,认为其分解温度为330℃。并发现反应气氛、光辐射都影响KClO_3热分解,其中光辐射可以催化KClO_3热分解。同时提出了一个新的机理模型,该机理模型能够较好地解释一些实验现象。
5通过对KClO_3和MnO_2混合体系的热分解研究,认为其分解温度与分析纯KClO_3热分解温度相同,为330℃;MnO_2对KClO_3的催化作用属于液-固催化,即MnO_2催化的是熔融态KClO_3的分解,混合体系在固态时MnO_2不起催化作用。同时发现KClO_3颗粒大小、升温速率都影响混合体系的热分解,并指出催化剂MnO_2最合适用量为10%-25%.
6通过对KClO_3和KMnO_4混合体系的热分解研究,发现原位产生的MnO_2对KClO_3热分解有较强的催化作用。
The thermal decomposition of solid is an important research area of solid chemistry, it has a wide application background. The production process of many inorganic salts includes the decomposition process of the raw materials such as carbonate, basic carbonate, sulfate or inter- mediate products. It is of great important practical significance to the technology reform, saving energy, reducing consumption and increasing efficiency for us to proved thermal decomposition mechanism of the solid, made highly efficient and appropriate catalyst. CaCO_3 is an important industrial raw materials in the production of portland cement, its decomposition temperature has an important effect on the quality and energy consumption in portland cement production. In addition, CaCO_3 decomposition as a simple and typical gas-solid reaction, Studying its reaction dynamics is helpful to reveal this type of reaction and the establishment of a complete principle of physical chemistry. It can make us deepen the understanding on the laws of thermal decomposition by the studying on the thermal decomposition mechanism, especially on catalytic thermal decomposi- tion. This is helpful to seek the efficient catalyst of CaCO_3 thermal decomposition, as soon as possible play its industrial value. Of course, this also contribute to the understanding on the laws of BaSO_4 thermal decomposition, then reform all kinds of barium-salt production process.
Considering the difficulty and the higher demands of experiment conditions in studying the decomposition of CaCO_3, BaSO_4, we decide to do some works begin from those inorganic solids which are familiar, similar, easy decomposition. Those are helpful to master the basic theories, research means and improve our research capability, accumulate some research experience and complete the hard task. So that we decide to do the research begin from the thermal decomposi- tion of KMnO_4, KClO_3. At present, the mechanism of potassium chlorate thermal decomposition is still very imperfect. Many scholars conducted extensive research on the mechanism of potassium chlorate thermal decomposition. because of the differenent experimental methods, experimental conditions, the researchers come to different mechanism model. None of these mechanism models can give a reasonable explanation completely accepted by us. Therefore, making a further study on the decomposition mechanism of KClO_3 has significant theoretical value. The main achievements of this dissertation are as follows:
1 Introduce the progress of CaCO_3, KClO_3 thermal decomposition and the main research methods about thermal analysis kinetics at present in China and abroad. Meanwhile,the deficiency and the improvement approach were put forward in this dissertation.
2 KMnO_4 was heated under a given temperature for long time in Muffle furnace, then we calculated the weight loss rate of KMnO_4. we determine the decomposition temperature of KMnO_4 according to the weight loss rate and found that thermal decomposition temperature of KMnO_4 is 190℃which is related to the crystalled status, not 240℃said in some literature. The mechanism models of KMnO_4 thermal decomposition were also firstly proposed by us.
3 The mixture solution of ClO_3- and trifle amount ClO_2-, in whichρ(ClO_3- ) = 34.1 g/L,ρ(ClO_2~-) =208 mg/L, was prepared, and the ClO_2- concentration in the solution was tried to be determined directly by iodometricmethod. The influences of varying the detecting conditions and adding ClO_4~- to the solution on the results were investigated. The procedure,precision, accuracy, and the least detectable ClO_2~- concentration of the method,were obtained. In the analysis process, the pH value of the solution to be detected should be adjusted by 0.5 mol/L HCl.
4 The researchers have different views on mechanism model and the thermal decomposi- tion temperature of KClO_3. We found that KClO_3 can decomposed at 330℃if it is heated for a long time under a given temperature. And found that reaction atmosphere, light radiation has effect on the thermal decomposition of KClO_3, light radiation can catalyze the thermal decomposition of KClO_3. We also proposed a new mechanism which can explain some experiments very well.
5 By studying on the thermal decomposition for the mixture system of KClO_3 and MnO_2, we think that the decomposition temperature of KClO_3 is 330℃which is the same as analytical reagent.we found it belongs to liquid-solid phase catalysis for MnO_2 catalyzing the thermal decomposition of KClO_3. That is to say that MnO_2 can’t catalyze the KClO_3 decomposition when KClO_3 is still in solide states. We also found that particle size of KClO_3, heating rate can effect the thermal decomposition of the mixture system, and pointed out that the most suitable amount of MnO_2 in the mixture system is about 10% -25%.
6 By studying on the thermal decomposition of the mixture system of KClO_3 and KMnO_4, we found that the situ MnO_2 has a high catalytic activity obtained from the decomposition products of KMnO_4.
鉴于CaCO_3、BaSO_4等热分解研究的较大难度和对实验条件较高的要求,我们经过长时间认真思考后,决定从一些较常见的、有相似性的、易分解的无机固体开始(实为进入科研启动阶段),熟悉有关的基础理论和研究手段,提高研究能力,积累研究经验,明确并创造研究条件,最终很好地展开、完成这一艰难、巨大的研究开发课题。对于无机固体的热分解,KMnO_4和KClO_3的热分解是人们再也熟悉不过的实例。但我们通过大量认真细致的调研,竟然发现有关的反应机理完全不清楚。为此我们选择从研究KMnO_4、KClO_3的热分解入手,在深厚、宽广的理论基础上,设计、完成了一系列巧妙、新颖的实验,取得一些重要发现。主要工作如下:
1总结了国内外KClO_3、CaCO_3热分解研究的进展及热分析动力学方法,指出了不足之处,提出了有待解决的问题。
2采用马弗炉把KMnO_4在一定温度下长时间加热,测定KMnO_4热分解失重率,根据是否失重确定其分解温度,发现KMnO_4热分解温度与其结晶状况有关,分解温度为190℃,不是文献中所载的240℃。首次提出了KMnO_4热分解机理。
3配制ClO_3~-和微量ClO_2~-混合存在的溶液,ρ(ClO_3~-) = 34.1g/L,ρ(ClO2-) = 208mg/L,尝试以碘量法直接测定其中亚氯酸根离子的含量。考察测定条件及向待测溶液中添加ClO_4~-对分析结果的影响,确定了方法的测定程序、精密度、准确度和该方法可以较方便检测的最低ClO_2~-浓度。测定过程的关键之处是使用约0.5mol/L的盐酸来调节待测溶液的pH值。
4认真研究了KClO_3热分解行为,发现学者们对KClO_3热分解温度和机理模型有不同看法。我们课题组在各个温度下对KClO_3长时间加热,认为其分解温度为330℃。并发现反应气氛、光辐射都影响KClO_3热分解,其中光辐射可以催化KClO_3热分解。同时提出了一个新的机理模型,该机理模型能够较好地解释一些实验现象。
5通过对KClO_3和MnO_2混合体系的热分解研究,认为其分解温度与分析纯KClO_3热分解温度相同,为330℃;MnO_2对KClO_3的催化作用属于液-固催化,即MnO_2催化的是熔融态KClO_3的分解,混合体系在固态时MnO_2不起催化作用。同时发现KClO_3颗粒大小、升温速率都影响混合体系的热分解,并指出催化剂MnO_2最合适用量为10%-25%.
6通过对KClO_3和KMnO_4混合体系的热分解研究,发现原位产生的MnO_2对KClO_3热分解有较强的催化作用。
The thermal decomposition of solid is an important research area of solid chemistry, it has a wide application background. The production process of many inorganic salts includes the decomposition process of the raw materials such as carbonate, basic carbonate, sulfate or inter- mediate products. It is of great important practical significance to the technology reform, saving energy, reducing consumption and increasing efficiency for us to proved thermal decomposition mechanism of the solid, made highly efficient and appropriate catalyst. CaCO_3 is an important industrial raw materials in the production of portland cement, its decomposition temperature has an important effect on the quality and energy consumption in portland cement production. In addition, CaCO_3 decomposition as a simple and typical gas-solid reaction, Studying its reaction dynamics is helpful to reveal this type of reaction and the establishment of a complete principle of physical chemistry. It can make us deepen the understanding on the laws of thermal decomposition by the studying on the thermal decomposition mechanism, especially on catalytic thermal decomposi- tion. This is helpful to seek the efficient catalyst of CaCO_3 thermal decomposition, as soon as possible play its industrial value. Of course, this also contribute to the understanding on the laws of BaSO_4 thermal decomposition, then reform all kinds of barium-salt production process.
Considering the difficulty and the higher demands of experiment conditions in studying the decomposition of CaCO_3, BaSO_4, we decide to do some works begin from those inorganic solids which are familiar, similar, easy decomposition. Those are helpful to master the basic theories, research means and improve our research capability, accumulate some research experience and complete the hard task. So that we decide to do the research begin from the thermal decomposi- tion of KMnO_4, KClO_3. At present, the mechanism of potassium chlorate thermal decomposition is still very imperfect. Many scholars conducted extensive research on the mechanism of potassium chlorate thermal decomposition. because of the differenent experimental methods, experimental conditions, the researchers come to different mechanism model. None of these mechanism models can give a reasonable explanation completely accepted by us. Therefore, making a further study on the decomposition mechanism of KClO_3 has significant theoretical value. The main achievements of this dissertation are as follows:
1 Introduce the progress of CaCO_3, KClO_3 thermal decomposition and the main research methods about thermal analysis kinetics at present in China and abroad. Meanwhile,the deficiency and the improvement approach were put forward in this dissertation.
2 KMnO_4 was heated under a given temperature for long time in Muffle furnace, then we calculated the weight loss rate of KMnO_4. we determine the decomposition temperature of KMnO_4 according to the weight loss rate and found that thermal decomposition temperature of KMnO_4 is 190℃which is related to the crystalled status, not 240℃said in some literature. The mechanism models of KMnO_4 thermal decomposition were also firstly proposed by us.
3 The mixture solution of ClO_3- and trifle amount ClO_2-, in whichρ(ClO_3- ) = 34.1 g/L,ρ(ClO_2~-) =208 mg/L, was prepared, and the ClO_2- concentration in the solution was tried to be determined directly by iodometricmethod. The influences of varying the detecting conditions and adding ClO_4~- to the solution on the results were investigated. The procedure,precision, accuracy, and the least detectable ClO_2~- concentration of the method,were obtained. In the analysis process, the pH value of the solution to be detected should be adjusted by 0.5 mol/L HCl.
4 The researchers have different views on mechanism model and the thermal decomposi- tion temperature of KClO_3. We found that KClO_3 can decomposed at 330℃if it is heated for a long time under a given temperature. And found that reaction atmosphere, light radiation has effect on the thermal decomposition of KClO_3, light radiation can catalyze the thermal decomposition of KClO_3. We also proposed a new mechanism which can explain some experiments very well.
5 By studying on the thermal decomposition for the mixture system of KClO_3 and MnO_2, we think that the decomposition temperature of KClO_3 is 330℃which is the same as analytical reagent.we found it belongs to liquid-solid phase catalysis for MnO_2 catalyzing the thermal decomposition of KClO_3. That is to say that MnO_2 can’t catalyze the KClO_3 decomposition when KClO_3 is still in solide states. We also found that particle size of KClO_3, heating rate can effect the thermal decomposition of the mixture system, and pointed out that the most suitable amount of MnO_2 in the mixture system is about 10% -25%.
6 By studying on the thermal decomposition of the mixture system of KClO_3 and KMnO_4, we found that the situ MnO_2 has a high catalytic activity obtained from the decomposition products of KMnO_4.
引文
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