【摘要】：黃磷的生產(chǎn)過程中,不可避免的會產(chǎn)生大量磷泥。富磷泥一般用來直接提取黃磷,而貧磷泥由于膠體結(jié)構(gòu)較為復(fù)雜難以提取黃磷,大部分作為危險廢物堆存或煉制磷酸,少數(shù)用于生產(chǎn)肥料,并未得到合理的利用。從貧磷泥中提取黃磷可提高磷資源利用率,獲得較好的經(jīng)濟(jì)效益和環(huán)境效益。本文以磷含量為10%~15%的貧磷泥為研究對象,采用XRF(X射線熒光光譜分析)、XRD(X射線衍射)和顯微鏡等方法對其成分和結(jié)構(gòu)進(jìn)行分析,提出了采用“正己烷萃取+紫外分光光度法”測定磷泥中的磷含量;自行設(shè)計了一套小型實驗室用蒸磷裝置,分析探討了蒸磷溫度、蒸磷時間等因素對提取貧磷泥中黃磷的影響,考察了化學(xué)藥劑法對貧磷泥的預(yù)處理效果;對蒸餾殘渣進(jìn)行了初步的浸出試驗。研究結(jié)果顯示:通過XRF測試結(jié)果表明,貧磷泥主要由SiO2(34.95%)、P2O5(24.89%)、F(18.20%)、K2O、CaO、Al2O3等成分組成,含有O、F、Si、K、P(10.86%)、Ca、Al等元素;XRD分析結(jié)果表明,貧磷泥中主要物相是K2SiF6;在顯微鏡下觀察發(fā)現(xiàn),貧磷泥中的磷主要是以一種被包裹的無定形聚合體形態(tài)存在,體積大小不一。采用“正己烷萃取+紫外分光光度法”可測定磷泥中的磷含量,對磷泥中黃磷萃取效率高。取磷泥重2 g,使用正己烷20 mL、振搖10 min,一次萃取即可完全。采用棋盤式全層取樣,解決了黃磷在泥餅中二維空間上分布不均勻的問題。本文通過試驗發(fā)現(xiàn):蒸磷溫度及蒸磷時間是影響貧磷泥中磷回收的主要因素,在溫度270℃到300℃,蒸磷時間20 min以上,貧磷泥中磷回收率均能達(dá)到80%以上。蒸磷溫度越高,蒸出速度越快。采用化學(xué)藥劑法預(yù)處理泥樣,可以破壞貧磷泥膠體的穩(wěn)定性,提高黃磷的回收率。選擇硫酸作為預(yù)處理劑,最佳預(yù)處理條件:硫酸投加量4 mL(1.2 mol/L),預(yù)處理溫度60℃,預(yù)處理時間30 min。在蒸磷溫度280℃、蒸磷時間15 min的條件下,未經(jīng)預(yù)處理貧磷泥的磷回收率為53.86%,預(yù)處理貧磷泥的磷回收率為82.50%。同時初步的浸出試驗發(fā)現(xiàn),提取磷后產(chǎn)生的殘渣仍對環(huán)境有一定影響,硫酸預(yù)處理的貧磷泥蒸磷殘渣浸出液中,總磷243.99 mg/L、磷酸鹽203.07 mg/L、單質(zhì)磷8.82 mg/L。應(yīng)該采取相應(yīng)措施進(jìn)行穩(wěn)定化處理,使其達(dá)到一般工業(yè)固體廢物的要求。本研究為有效的綜合處置貧磷泥,提高磷的回收率和經(jīng)濟(jì)效益,減輕貧磷泥對環(huán)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，

本文編號：2379450