(1. 廣東省科學(xué)院資源綜合利用研究所，廣州 510650；
2. 稀有金屬分離與綜合利用國(guó)家重點(diǎn)實(shí)驗(yàn)室，廣州 510650；
3. 廣東省礦產(chǎn)資源開發(fā)和綜合利用重點(diǎn)實(shí)驗(yàn)室，廣州 510650)
摘 要: 針對(duì)國(guó)內(nèi)某石化企業(yè)廢石化催化劑處理過(guò)程中出現(xiàn)的產(chǎn)品純度低、污染大等問(wèn)題，提出了一種微波?超聲波強(qiáng)化處理廢催化劑的工藝采用物質(zhì)流方法對(duì)工藝中稀有金屬釩、鉬元素的行為進(jìn)行研究。結(jié)果表明：采用微波?超聲波強(qiáng)化處理工藝，可制備高純V2O5產(chǎn)品(純度＞99.9%)和普通V2O5產(chǎn)品(純度＞99%)，釩的直收率為91.32%，未有效回收的釩主要分散在浸出渣、凈化沉淀渣、萃釩余液和二段反萃液沉淀母液中，共占原料釩的7.58%。同時(shí)，可以制備合格的鉬酸銨產(chǎn)品，鉬的直收率為91.68%，未有效回收的鉬主要分散在浸出渣、凈化沉淀渣、負(fù)載釩有機(jī)相、萃鉬余液和沉鉬母液中，共占原料鉬的7.99%。本工藝的特色主要體現(xiàn)在微波強(qiáng)化浸出和超聲波強(qiáng)化反萃工序。微波強(qiáng)化浸出工藝中，釩和鉬的浸出效率得到明顯提高，這與反應(yīng)的溫度體系、礦物宏/微觀結(jié)構(gòu)變化以及高價(jià)釩含量的提高有密切關(guān)系。超聲波反萃工藝可明顯縮短反萃時(shí)間，超聲波技術(shù)可降低晶體的團(tuán)聚程度，有效消除氯化銨反萃過(guò)程中團(tuán)聚晶體堵塞管道的現(xiàn)象。
關(guān)鍵字: 廢催化劑；微波；超聲波；釩；鉬
（1. Institute of Resources Comprehensive Utilization, Guangdong Academy of Sciences, Guangzhou 510650, China;
2. State Key Laboratory of Separation and Comprehensive Utilization of Rare Metals, Guangzhou 510650, China;
3. Guangdong Provincial Key Laboratory of Development and Comprehensive Utilization of Mineral Resources, Guangzhou 510650, China）
Abstract:Aiming at the problems of low product purity and high pollution in the treatment process of spent petrochemical catalyst for a petrochemical enterprise in China, a microwave-ultrasonic enhanced process for spent catalyst treatment was proposed, and the behaviors of vanadium and molybdenum in the process were studied by material flow method. The results show that high purity V2O5 product (purity＞99.9%) and common V2O5 product (purity＞99%) can be prepared by microwave-ultrasonic enhanced treatment process. The direct yield of vanadium is 91.32%. The ineffective recovery of vanadium is mainly dispersed in the leached residue, purified precipitation residue, vanadium extraction raffinate and second stage back-extraction solution precipitated solution, which account for 7.58% of vanadium in the raw material. At the same time, qualified ammonium molybdate product can be prepared. The direct yield of molybdenum is 91.68%. The ineffective recovery of molybdenum is mainly dispersed in the leached residue, purified precipitation residue, loaded vanadium organic phase, molybdenum extraction raffinate and molybdenum precipitated solution, which account for 7.99% of molybdenum in the raw material. The characteristics of this process are mainly reflected in microwave enhanced leaching and ultrasonic enhanced back-extraction process. In the microwave enhanced leaching process, the leaching efficiencies of vanadium and molybdenum are obviously improved, which is attributed to the temperature system of the reaction, the macro/microstructure change of the mineral and the increase of the high valence state vanadium content. Ultrasonic back-extraction technology can obviously shorten the back-extraction time. Moreover, ultrasound can reduce the agglomeration degree of crystals and effectively eliminate the phenomenon of the agglomeration crystals blocking the pipes in the ammonium chloride back-extraction process.
Key words: spent catalyst; microwave; ultrasonic; vanadium; molybdenum
