铬盐清洁工艺中铬酸钾—氯化钾的多元相平衡与相分离研究
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摘要
传统的由铬铁矿生产铬盐是重要的化工与冶金基础原料工业。目前我国采用的高温氧化-钠化焙烧法传统工艺,要排放出大量高毒性铬渣及含铬粉尘废气,严重污染环境。而本文所研究的液相氧化铬盐清洁生产新工艺,以取代传统的铬盐生产方法。新工艺可大幅降低反应温度,提高转化率,实现资源有价组分全利用及铬渣的零排放。
铬盐清洁生产工艺的核心部分为铬铁矿在碱系熔盐流动介质中与空气进行氧化反应的液相氧化过程。在液相氧化过程以及铬碱分离之后,多余的氢氧化钾溶液将返回到液相氧化过程进行循环使用。但是,随着氢氧化钾的循环以及生产的放大,氢氧化钾所含的杂质氯化钾在整个系统中不断积累,极大地影响了铬酸钾产品的质量。本文测定了产业链中氢还原生产铬绿清洁工艺中铬酸钾多元水盐体系相平衡,并构筑了体系相图,建立了铬酸钾-氯化钾-水体系的结晶分离方法,为铬酸钾粗晶中除氯工艺路线的设计及优化提供理论依据,论文的主要内容包括如下几个方面:
1.分别研究了K_2CrO_4-KCl-H_2O三元体系在30℃,60℃和90℃时以及KOH-K_2CrO_4-KCl-H_2O四元体系在20℃,40℃,60℃和80℃时的相平衡数据,并且分别绘制了各自相应的相图。通过相图的研究,为实际的含氯铬酸钾粗晶的结晶分离提供了理论上的依据。
2.分别以实验测的K_2CrO_4-KCl-H_2O三元体系和KOH-K_2CrO_4-KCl-H_2O四元体系相图为依据,对清洁工艺中铬盐除氯设计了两种不同的分离工艺,并且进行了实验验证。
3.就耗能量及晶体的纯度,结晶率,耗水量等进行综合对比,找出最优的工艺方式,并且在现场得到很好的应用。
Chromate produced from chromite is one of the important basic raw materials in the chemical and metallurgical industries.The high-temperature roasting technology presently used in China discharges a large amount of chromium - containing residue,chromite dust and waste gas,which severely pollute the environment.The clean production technology of chromate measured in the paper replaced the traditional production technology of chromate.In this new technology the reaction temperature can be significantly decreased,the conversion of chrome can be greatly improved,all valuable components in chromite can be fully utilized,and the zero discharge of residue can be realized.
The key of the new technology is the heterogeneous reaction of chromite with air in the molten alkaline medium.After the liquid phase oxidation process of chromite and the separation process of chromate and alkali, excessive potassium hydroxide solution will go back to the process of the liquid phase oxidation.However,with the reuse of KOH and enlargement of production,KCl can accumulate to a certain amount in the KOH as an impurity and influence the quality of potassium chromate.The present paper mainly focused on the phase equilibria and crystallization separation of the potassium chromate and potassium chloride multi-component aqueous salt system in the cleaner production of chromate.And these diagrams of the above systems were studied for the first time.These results are important for designing technological flow sheet and optimizing parameters.The main points in this work are as follows:
1.The phase equilibria for the system K_2CrO_4 - KCl - H_2O from 30℃to 90℃and the system KOH - K_2CrO_4 - KCl - H_2O from 20℃to 80℃were studied by employing the method of isothermal solution saturation.The phase diagrams were plotted as well.The study will be used as a basis for the separation of K_2CrO_4 and KCl for cleaner production of chromate.
2.Based on the phase diagrams for the system K_2CrO_4 - KCl - H_2O and KOH - K_2CrO_4 - KCl - H_2O,two different crystallization seperation processes between the K_2CrO_4 and KCl for cleaner production of chromate were studied and testified by experiments.
3.General comparisons were carried on energy consumption,crystal purity,crystal rate and water consumption,etc.in order to optimize the process.It has been applied in the scene.
铬盐清洁生产工艺的核心部分为铬铁矿在碱系熔盐流动介质中与空气进行氧化反应的液相氧化过程。在液相氧化过程以及铬碱分离之后,多余的氢氧化钾溶液将返回到液相氧化过程进行循环使用。但是,随着氢氧化钾的循环以及生产的放大,氢氧化钾所含的杂质氯化钾在整个系统中不断积累,极大地影响了铬酸钾产品的质量。本文测定了产业链中氢还原生产铬绿清洁工艺中铬酸钾多元水盐体系相平衡,并构筑了体系相图,建立了铬酸钾-氯化钾-水体系的结晶分离方法,为铬酸钾粗晶中除氯工艺路线的设计及优化提供理论依据,论文的主要内容包括如下几个方面:
1.分别研究了K_2CrO_4-KCl-H_2O三元体系在30℃,60℃和90℃时以及KOH-K_2CrO_4-KCl-H_2O四元体系在20℃,40℃,60℃和80℃时的相平衡数据,并且分别绘制了各自相应的相图。通过相图的研究,为实际的含氯铬酸钾粗晶的结晶分离提供了理论上的依据。
2.分别以实验测的K_2CrO_4-KCl-H_2O三元体系和KOH-K_2CrO_4-KCl-H_2O四元体系相图为依据,对清洁工艺中铬盐除氯设计了两种不同的分离工艺,并且进行了实验验证。
3.就耗能量及晶体的纯度,结晶率,耗水量等进行综合对比,找出最优的工艺方式,并且在现场得到很好的应用。
Chromate produced from chromite is one of the important basic raw materials in the chemical and metallurgical industries.The high-temperature roasting technology presently used in China discharges a large amount of chromium - containing residue,chromite dust and waste gas,which severely pollute the environment.The clean production technology of chromate measured in the paper replaced the traditional production technology of chromate.In this new technology the reaction temperature can be significantly decreased,the conversion of chrome can be greatly improved,all valuable components in chromite can be fully utilized,and the zero discharge of residue can be realized.
The key of the new technology is the heterogeneous reaction of chromite with air in the molten alkaline medium.After the liquid phase oxidation process of chromite and the separation process of chromate and alkali, excessive potassium hydroxide solution will go back to the process of the liquid phase oxidation.However,with the reuse of KOH and enlargement of production,KCl can accumulate to a certain amount in the KOH as an impurity and influence the quality of potassium chromate.The present paper mainly focused on the phase equilibria and crystallization separation of the potassium chromate and potassium chloride multi-component aqueous salt system in the cleaner production of chromate.And these diagrams of the above systems were studied for the first time.These results are important for designing technological flow sheet and optimizing parameters.The main points in this work are as follows:
1.The phase equilibria for the system K_2CrO_4 - KCl - H_2O from 30℃to 90℃and the system KOH - K_2CrO_4 - KCl - H_2O from 20℃to 80℃were studied by employing the method of isothermal solution saturation.The phase diagrams were plotted as well.The study will be used as a basis for the separation of K_2CrO_4 and KCl for cleaner production of chromate.
2.Based on the phase diagrams for the system K_2CrO_4 - KCl - H_2O and KOH - K_2CrO_4 - KCl - H_2O,two different crystallization seperation processes between the K_2CrO_4 and KCl for cleaner production of chromate were studied and testified by experiments.
3.General comparisons were carried on energy consumption,crystal purity,crystal rate and water consumption,etc.in order to optimize the process.It has been applied in the scene.
引文
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