利用含铬废渣制备重铬酸钠的研究
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摘要
重铬酸钠是生产铬盐过程的中间产品,在国民经济各部门中用途广泛,利用铬铁矿制备重铬酸钠等含铬系列产品造成的严重污染问题一直制约着铬盐工业的可持续发展。我国是一个铬矿资源短缺的国家,而铬渣污染事故日益严重。因此,利用含铬废渣制备重铬酸钠,实现清洁化生产是当前铬盐工业面临的重要课题。本文以不锈钢冶炼与加工行业产生的含铬废渣为原料,研究了焙烧-硫酸酸化法制备重铬酸钠的工艺,明确了原料化学组分、颗粒大小以及物料配比等诸因素对炉料氧化焙烧阶段的影响,探究了制备高纯度重铬酸钠的必要条件,在工业实施过程中,成功制备了产品重铬酸钠,提出了经济高效利用含铬废渣的方法。
试验的主要研究结果与进展如下：
1)在氧化焙烧工艺中,含铬废渣的粒度以-60目为宜,铬渣焙烧工艺的最佳条件为：焙烧温度1000℃,m(碳酸钠)：m(铬渣)=0.18,氧化添加剂用量为6g,焙烧时间为8h。
2)铬酸钠熟料浸滤过程中,浸泡时间以及浸泡液固比对铬回收率有一定的影响,浸出时间以2h为宜,浸泡液固比为1：1,铬回收率可达99.3%。
3)在铬酸钠溶液的中和去杂过程中,中和液pH值为6.5,中和液浓度为120g.L-1,中和反应温度为60℃,杂质离子去除率在97.6%以上。
4)在重铬酸钠溶液的蒸发及硫酸钠的分离工艺中,酸化液pH值为3.5,Na2Cr2O7·2H20料液浓度为1800g·L-1,Na2Cr207·2H2O-Na2S04体系共饱和点温度为128℃,Na2SO4基本分离。
5)影响重铬酸钠纯度的因素主要是结晶时间与质量浓度,结晶时间以12h为宜,质量浓度以74%为宜,此时产品纯净度高达99.5%。
6)工业制备重铬酸钠,一次结晶率可达48%,纯度为99.2%,产品质量符合GB1611-92《工业重铬酸钠》中一等品的质量标准。
7)尾渣含铁量为46.6%,符合乙种铁矿石对铁含量的要求,可进行冶炼,处理1吨含铬废渣可制备重铬酸钠175kg,现制备工业重铬酸钠1吨可产生经济效益3570元。
Sodium dichromate is the intermediate product of the production process of chromium salt, which is widely used in various sectors of the national economy. The serious pollution caused by the chromite preparation of sodium dichromate-containing chromium series products has been constraining the sustainable development of the chromium salt industry. China is in the shortage of chrome ores, but the chromium slag pollution is more and more serious. Therefore, the preparation of sodium dichromate from chromium waste to realize clean production in chromium salt industry is significant task. We used Chromium-containing wastes from stainless steel smelting and processing industry as raw materials in our research, studied the process of sodium dichromate by roasting-sulfuric acid, cleared raw material chemical composition, particle size and the ratio of raw materials such as oxidizing roasting of charge stage, explored the necessary conditions for preparation of high purity sodium dichromate, prepared the sodium dichromate in the industrial process of implementation, and proposed a cost-effective and efficient way to use chromium residue.
The main findings of the trial and progress are as follows:
1) The chromium-containing residue particle size to60meshes is appropriate in the oxidation roasting process. The best conditions for the calcination process of chromium slag are as follows:the calcination temperature is1000℃, m (sodium carbonate):m (chromium slag)=0.18, the amount of oxide fillers is6g, the calcination time lasts8h.
2)Soaking time and soaking solid ratio have a certain impact on chromium recovery in the sodium chromate clinker leaching process.When the leaching time is2h and the soaking solid ratio is1:1, chromium recovery rate will be up to99.3%.
3) In the process of sodium chromate solution neutralization and cleaning, some parameters are as follows:the pH value is6.5, the neutraliaing solution concentration is120g·L-1, the neutralization reaction tempreture is60℃. the removal rate of impurity ions will be up to97.6%or more.
4) In the separation process of evaporation of the sodium dichromate solution and sodium sulfate, when the acidification of pH value is3.5, the feed concentration of Na2Cr2O7·2H20is1800g·L-1, the system saturation point temperature of Na2Cr2O7·2H2O-Na2SO4is128℃, Na2SO4will be separated basically.
5) Influence on the purity of sodium dichromate is the main factor of the crystallization time and mass concentration. Crystallization time to12h is advisable. Mass concentration in74%is as well. The product of high purity will reach99.5%.
6) Industrial preparation of sodium dichromate, a crystallization rate is up to48%, the purity is99.2%, and the quality reach the first-class quality standard in GB1611-92of "industrial sodium dichromate".
7) Slag iron content46.6%, consistent with an iron ore of iron content, can be used for smelting. Sodium dichromate of175KG can be produced from one ton waste residue. Preparation1tons industrial sodium dichromate can produce economic benefits3570yuan.
试验的主要研究结果与进展如下：
1)在氧化焙烧工艺中,含铬废渣的粒度以-60目为宜,铬渣焙烧工艺的最佳条件为：焙烧温度1000℃,m(碳酸钠)：m(铬渣)=0.18,氧化添加剂用量为6g,焙烧时间为8h。
2)铬酸钠熟料浸滤过程中,浸泡时间以及浸泡液固比对铬回收率有一定的影响,浸出时间以2h为宜,浸泡液固比为1：1,铬回收率可达99.3%。
3)在铬酸钠溶液的中和去杂过程中,中和液pH值为6.5,中和液浓度为120g.L-1,中和反应温度为60℃,杂质离子去除率在97.6%以上。
4)在重铬酸钠溶液的蒸发及硫酸钠的分离工艺中,酸化液pH值为3.5,Na2Cr2O7·2H20料液浓度为1800g·L-1,Na2Cr207·2H2O-Na2S04体系共饱和点温度为128℃,Na2SO4基本分离。
5)影响重铬酸钠纯度的因素主要是结晶时间与质量浓度,结晶时间以12h为宜,质量浓度以74%为宜,此时产品纯净度高达99.5%。
6)工业制备重铬酸钠,一次结晶率可达48%,纯度为99.2%,产品质量符合GB1611-92《工业重铬酸钠》中一等品的质量标准。
7)尾渣含铁量为46.6%,符合乙种铁矿石对铁含量的要求,可进行冶炼,处理1吨含铬废渣可制备重铬酸钠175kg,现制备工业重铬酸钠1吨可产生经济效益3570元。
Sodium dichromate is the intermediate product of the production process of chromium salt, which is widely used in various sectors of the national economy. The serious pollution caused by the chromite preparation of sodium dichromate-containing chromium series products has been constraining the sustainable development of the chromium salt industry. China is in the shortage of chrome ores, but the chromium slag pollution is more and more serious. Therefore, the preparation of sodium dichromate from chromium waste to realize clean production in chromium salt industry is significant task. We used Chromium-containing wastes from stainless steel smelting and processing industry as raw materials in our research, studied the process of sodium dichromate by roasting-sulfuric acid, cleared raw material chemical composition, particle size and the ratio of raw materials such as oxidizing roasting of charge stage, explored the necessary conditions for preparation of high purity sodium dichromate, prepared the sodium dichromate in the industrial process of implementation, and proposed a cost-effective and efficient way to use chromium residue.
The main findings of the trial and progress are as follows:
1) The chromium-containing residue particle size to60meshes is appropriate in the oxidation roasting process. The best conditions for the calcination process of chromium slag are as follows:the calcination temperature is1000℃, m (sodium carbonate):m (chromium slag)=0.18, the amount of oxide fillers is6g, the calcination time lasts8h.
2)Soaking time and soaking solid ratio have a certain impact on chromium recovery in the sodium chromate clinker leaching process.When the leaching time is2h and the soaking solid ratio is1:1, chromium recovery rate will be up to99.3%.
3) In the process of sodium chromate solution neutralization and cleaning, some parameters are as follows:the pH value is6.5, the neutraliaing solution concentration is120g·L-1, the neutralization reaction tempreture is60℃. the removal rate of impurity ions will be up to97.6%or more.
4) In the separation process of evaporation of the sodium dichromate solution and sodium sulfate, when the acidification of pH value is3.5, the feed concentration of Na2Cr2O7·2H20is1800g·L-1, the system saturation point temperature of Na2Cr2O7·2H2O-Na2SO4is128℃, Na2SO4will be separated basically.
5) Influence on the purity of sodium dichromate is the main factor of the crystallization time and mass concentration. Crystallization time to12h is advisable. Mass concentration in74%is as well. The product of high purity will reach99.5%.
6) Industrial preparation of sodium dichromate, a crystallization rate is up to48%, the purity is99.2%, and the quality reach the first-class quality standard in GB1611-92of "industrial sodium dichromate".
7) Slag iron content46.6%, consistent with an iron ore of iron content, can be used for smelting. Sodium dichromate of175KG can be produced from one ton waste residue. Preparation1tons industrial sodium dichromate can produce economic benefits3570yuan.
引文
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