贫磷泥中黄磷的提取方法

发布时间：2018-12-14 22:48

【摘要】：黄磷的生产过程中,不可避免的会产生大量磷泥。富磷泥一般用来直接提取黄磷,而贫磷泥由于胶体结构较为复杂难以提取黄磷,大部分作为危险废物堆存或炼制磷酸,少数用于生产肥料,并未得到合理的利用。从贫磷泥中提取黄磷可提高磷资源利用率,获得较好的经济效益和环境效益。本文以磷含量为10%~15%的贫磷泥为研究对象,采用XRF(X射线荧光光谱分析)、XRD(X射线衍射)和显微镜等方法对其成分和结构进行分析,提出了采用“正己烷萃取+紫外分光光度法”测定磷泥中的磷含量;自行设计了一套小型实验室用蒸磷装置,分析探讨了蒸磷温度、蒸磷时间等因素对提取贫磷泥中黄磷的影响,考察了化学药剂法对贫磷泥的预处理效果;对蒸馏残渣进行了初步的浸出试验。研究结果显示:通过XRF测试结果表明,贫磷泥主要由SiO2(34.95%)、P2O5(24.89%)、F(18.20%)、K2O、CaO、Al2O3等成分组成,含有O、F、Si、K、P(10.86%)、Ca、Al等元素;XRD分析结果表明,贫磷泥中主要物相是K2SiF6;在显微镜下观察发现,贫磷泥中的磷主要是以一种被包裹的无定形聚合体形态存在,体积大小不一。采用“正己烷萃取+紫外分光光度法”可测定磷泥中的磷含量,对磷泥中黄磷萃取效率高。取磷泥重2 g,使用正己烷20 mL、振摇10 min,一次萃取即可完全。采用棋盘式全层取样,解决了黄磷在泥饼中二维空间上分布不均匀的问题。本文通过试验发现:蒸磷温度及蒸磷时间是影响贫磷泥中磷回收的主要因素,在温度270℃到300℃,蒸磷时间20 min以上,贫磷泥中磷回收率均能达到80%以上。蒸磷温度越高,蒸出速度越快。采用化学药剂法预处理泥样,可以破坏贫磷泥胶体的稳定性,提高黄磷的回收率。选择硫酸作为预处理剂,最佳预处理条件:硫酸投加量4 mL(1.2 mol/L),预处理温度60℃,预处理时间30 min。在蒸磷温度280℃、蒸磷时间15 min的条件下,未经预处理贫磷泥的磷回收率为53.86%,预处理贫磷泥的磷回收率为82.50%。同时初步的浸出试验发现,提取磷后产生的残渣仍对环境有一定影响,硫酸预处理的贫磷泥蒸磷残渣浸出液中,总磷243.99 mg/L、磷酸盐203.07 mg/L、单质磷8.82 mg/L。应该采取相应措施进行稳定化处理,使其达到一般工业固体废物的要求。本研究为有效的综合处置贫磷泥,提高磷的回收率和经济效益,减轻贫磷泥对环境的污染作出了有益的探索。
[Abstract]:In the production process of yellow phosphorus, a large amount of phosphorus sludge will inevitably be produced. Phosphorus rich mud is generally used to extract yellow phosphorus directly, but poor phosphorus mud is difficult to extract yellow phosphorus because of its complex colloidal structure, most of them are stored as hazardous wastes or refined phosphoric acid, and a few are used in fertilizer production, which are not used reasonably. The extraction of yellow phosphorus from phosphorus-poor mud can improve the utilization rate of phosphorus resources and obtain better economic and environmental benefits. In this paper, the composition and structure of Phosphorus-poor sludge with 10% P content and 15% P content were analyzed by XRF (X ray fluorescence spectroscopy (XRF (X) and), XRD (X ray diffraction (XRD) and microscope. The determination of phosphorus content in phosphorus sludge by "n-hexane extraction ultraviolet spectrophotometry" was put forward. A set of small laboratory phosphorus steaming device was designed. The effects of temperature and time of phosphorus evaporation on the extraction of yellow phosphorus from phosphorus-poor sludge were analyzed and the pretreatment effect of chemical reagent method on phosphorus poor sludge was investigated. A preliminary leaching test of distillation residue was carried out. The results showed that the phosphorus-poor sludge was mainly composed of SiO2 (34.95%), P2O5 (24.89%), F (18.20%), K _ 2O _ 2 + CaOO _ 2O _ 3, etc. Elements such as Ca,Al; The results of XRD analysis showed that K _ 2SiF _ 6 was the main phase in the phosphorus-poor sludge, and it was found that the phosphorus in the phosphorus-poor mud was mainly in the form of a encapsulated amorphous polymer with different volume under microscope. The content of phosphorus in phosphorus sludge can be determined by "n-hexane extraction ultraviolet spectrophotometry", and the extraction efficiency of yellow phosphorus in phosphorus mud is high. The phosphorus sludge was extracted at 2 g by shaking for 10 min, with hexane for 20 mL,. The problem of uneven distribution of yellow phosphorus in two dimensional space in mud cake was solved by chessboard sampling. In this paper, it is found that the temperature and time of steaming phosphorus are the main factors affecting the recovery of phosphorus from poor phosphorus mud. The recovery rate of phosphorus in poor phosphorus mud can reach more than 80% when the temperature is 270 鈩，

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