CN102747225A - Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid - Google Patents
Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid Download PDFInfo
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Abstract
一种石煤提钒酸浸液中铜、硒、铀综合回收方法，工艺过程主要包括：石煤硫酸浸出液结晶钾明矾或铵明矾除铝，除铝后液先加入含铜物料及富磷物料调节溶液的铜浓度及铀/磷比，再加碱调pH值，然后加入还原剂，使溶液中的铜、硒和铀还原沉淀析出，再经陈化、过滤，以实现石煤提钒过程铜、硒和铀的高效分离富集，具有工艺简单，铜、硒和铀的回收率高，试剂用量少，回收成本低，环境友好等优点。A method for comprehensive recovery of copper, selenium and uranium in acid leaching solution for extracting vanadium from stone coal. The process mainly includes: removing aluminum by crystallizing potassium alum or ammonium alum in sulfuric acid leaching solution from stone coal, adding copper-containing materials and phosphorus-rich materials to the solution after aluminum removal Adjust the copper concentration and uranium/phosphorus ratio of the solution, add alkali to adjust the pH value, and then add a reducing agent to reduce and precipitate copper, selenium and uranium in the solution, then age and filter to realize the process of extracting vanadium from stone coal The high-efficiency separation and enrichment of copper, selenium and uranium has the advantages of simple process, high recovery rate of copper, selenium and uranium, less reagent consumption, low recovery cost, and environmental friendliness.
Description
技术领域 technical field
本发明涉及一种石煤提钒酸浸液中铜、硒、铀综合回收方法。属于钒矿的选冶技术领域。The invention relates to a comprehensive recovery method for copper, selenium and uranium in an acid leaching solution for extracting vanadium from stone coal. The invention belongs to the technical field of dressing and smelting of vanadium ore.
背景技术 Background technique
石煤是一种含钒多金属矿物资源，石煤中除钒以外，还含有碳、硅、磷、铝、铁、钾、铜、硒、铀等元素。石煤含V2O5大于0.7%可作为钒矿开采，石煤中的钒主要以含钒伊利石(K(Al,V)2(Si,Al)4O10(OH)2)的形式存在。石煤提钒的常用工艺是硫酸浸出，目前从石煤酸浸溶液中提取钒主要采用以下工艺：Stone coal is a vanadium-containing polymetallic mineral resource. In addition to vanadium, stone coal also contains carbon, silicon, phosphorus, aluminum, iron, potassium, copper, selenium, uranium and other elements. Stone coal containing more than 0.7% V 2 O 5 can be exploited as vanadium ore, and the vanadium in stone coal is mainly in the form of vanadium-containing illite (K(Al,V) 2 (Si,Al) 4 O 10 (OH) 2 ) exist. The common process for extracting vanadium from stone coal is sulfuric acid leaching. At present, the following processes are mainly used to extract vanadium from stone coal acid leaching solution:
1)石煤硫酸浸出液→铵盐除铝→还原→萃取→反萃→氧化→铵盐沉钒→煅烧得精钒；1) Stone coal sulfuric acid leaching solution → ammonium salt removal of aluminum → reduction → extraction → stripping → oxidation → ammonium salt precipitation of vanadium → calcination to obtain refined vanadium;
2)石煤硫酸浸出液→铵盐除铝→选择性氧化除铁→钒氧化→离子交换→解吸→铵盐沉钒→煅烧得精钒；2) Stone coal sulfuric acid leaching solution → ammonium salt removal of aluminum → selective oxidation of iron removal → vanadium oxidation → ion exchange → desorption → ammonium salt precipitation of vanadium → calcination to obtain refined vanadium;
3)石煤硫酸浸出液→铵盐除铝→氧化沉钒铁化合物→碱浸→净化除杂→铵盐沉钒→煅烧得精钒。3) Stone coal sulfuric acid leaching solution → ammonium salt removal of aluminum → oxidation precipitation of vanadium iron compound → alkali leaching → purification and removal of impurities → ammonium salt precipitation of vanadium → calcination to obtain refined vanadium.
石煤中一般含Cu0.01~0.08%、Se0.001～0.005%、U0.001～0.02%。铜是一种有价金属，铜在石煤提钒过程主要进入提钒后液的净化渣中，提钒后液净化渣由于含有铜等有害的重金属元素，成为石煤提钒的有害固废；硒是一种稀散元素，广泛用于半导体、生物、医药等行业，石煤提钒过程硒分散在废水和废渣中，造成宝贵的硒资源浪费；铀是一种放射性元素，同时也是一种重要的战略元素，铀在石煤提钒过程分散在废水和废渣中，放射性废水废渣的产生对石煤提钒周边环境构成严重的威胁。硫酸浸出过程，石煤中的铝、铁、钾、铜、硒、铀等元素随钒一起进入溶液。石煤酸浸液中的铁、铝、钾已有方法综合利用，但其中的铜、硒、铀却还没有找到合适的方法予以回收，给石煤提钒带来很大的环保压力。Stone coal generally contains Cu0.01~0.08%, Se0.001~0.005%, U0.001~0.02%. Copper is a valuable metal. During the process of vanadium extraction from stone coal, copper mainly enters the purification slag of the liquid after vanadium extraction. The liquid purification slag after vanadium extraction contains harmful heavy metal elements such as copper, and becomes a harmful solid waste for vanadium extraction from stone coal. Selenium is a kind of scattered element, which is widely used in industries such as semiconductor, biology, and medicine. Selenium is dispersed in waste water and waste residue in the process of extracting vanadium from stone coal, resulting in a waste of valuable selenium resources; Uranium is a radioactive element, and it is also a An important strategic element, uranium is dispersed in waste water and waste residue during the vanadium extraction process from stone coal, and the generation of radioactive waste water and waste residue poses a serious threat to the surrounding environment of vanadium extraction from stone coal. During the sulfuric acid leaching process, elements such as aluminum, iron, potassium, copper, selenium, and uranium in stone coal enter the solution together with vanadium. The iron, aluminum, and potassium in the stone coal acid leaching solution have been comprehensively utilized, but the copper, selenium, and uranium in it have not yet found a suitable method to recover, which brings great environmental pressure to the extraction of vanadium from stone coal.
发明内容 Contents of the invention
本发明的目的在于提供一种可有效回收石煤提钒酸浸液中铜、硒和铀，提高资源综合利用率，避免含铜的放射性废渣废水产生，环境友好的石煤提钒酸浸液中铜、硒、铀综合回收方法。The object of the present invention is to provide a kind of acid leaching solution for extracting vanadium from stone coal that can effectively recover copper, selenium and uranium, improve the comprehensive utilization rate of resources, avoid the production of copper-containing radioactive waste slag wastewater, and be environmentally friendly. A comprehensive recovery method for copper, selenium and uranium.
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，是采用下述方案实现的：A method for comprehensively recovering copper, selenium and uranium in the acid leaching solution for extracting vanadium from stone coal of the present invention is realized by adopting the following scheme:
按石煤硫酸浸出液中的铝形成钾明矾或铵明矾理论量的1~3倍加入钾盐或铵盐，使溶液中的铝以钾明矾或铵明矾的形式结晶析出，过滤得到明矾和除铝后液；控制除铝后液中铜的浓度为0.1~10g/L，然后加入富磷物料调节溶液中的铀/磷摩尔比为1:100~5000，再加碱调节溶液的pH值至0.2~2.5，然后按除铝后液中铁和钒还原成二价铁和四价钒化学反应计量数的1.1~4.5倍加入标准电极电位小于等于0.1伏的还原剂，搅拌，使溶液中的铜、硒和铀还原沉淀析出；还原后液经陈化、过滤得到还原后液和还原渣；还原后液萃取提钒，还原渣分离回收铜、硒和铀。Add potassium salt or ammonium salt according to 1~3 times of the theoretical amount of potassium alum or ammonium alum in the sulfuric acid leaching solution of stone coal, so that the aluminum in the solution crystallizes and precipitates in the form of potassium alum or ammonium alum, and filters to obtain alum and aluminum removal After liquid: control the concentration of copper in the liquid after removing aluminum to 0.1~10g/L, then add phosphorus-rich materials to adjust the molar ratio of uranium/phosphorus in the solution to 1:100~5000, and then add alkali to adjust the pH value of the solution to 0.2 ~2.5, then add a reducing agent with a standard electrode potential of less than or equal to 0.1 volts by reducing iron and vanadium in the solution to 1.1 to 4.5 times the stoichiometric number of ferrous iron and tetravalent vanadium after removing aluminum, and stir to make the copper, vanadium in the solution Selenium and uranium are reduced and precipitated; the reduced liquid is aged and filtered to obtain the reduced liquid and reduced slag; the reduced liquid is extracted to extract vanadium, and the reduced slag is separated and recovered to recover copper, selenium and uranium.
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，所述钾盐选自K2SO4、KHSO4、KCl、KNO3、KH2PO4、K2HPO4、K3PO4、K2CO3、KHCO3中的一种，使溶液中的铝以钾明矾(KAl(SO4)2·12H2O)的形式结晶析出。The present invention relates to a comprehensive recovery method for copper, selenium and uranium in acid leaching solution for extracting vanadium from stone coal. The potassium salt is selected from K 2 SO 4 , KHSO 4 , KCl, KNO 3 , KH 2 PO 4 , K 2 HPO 4 , One of K 3 PO 4 , K 2 CO 3 , and KHCO 3 causes the aluminum in the solution to crystallize in the form of potassium alum (KAl(SO 4 ) 2 ·12H 2 O).
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，所述铵盐选自(NH4)2SO4、NH4HSO4、NH4Cl、NH4NO3、NH4H2PO4、(NH4)2HPO4、(NH4)3PO4、(NH4)2CO3、NH4HCO3中的一种，使溶液中的铝以铵明矾(NH4Al(SO4)2·12H2O)的形式结晶析出。The present invention relates to a comprehensive recovery method for copper, selenium and uranium in acid leaching solution for extracting vanadium from stone coal, wherein the ammonium salt is selected from (NH 4 ) 2 SO 4 , NH 4 HSO 4 , NH 4 Cl, NH 4 NO 3 , NH One of 4 H 2 PO 4 , (NH 4 ) 2 HPO 4 , (NH 4 ) 3 PO 4 , (NH 4 ) 2 CO 3 , NH 4 HCO 3 , so that the aluminum in the solution is converted to ammonium alum (NH 4 Al(SO 4 ) 2 ·12H 2 O) crystallized out.
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，所述控制除铝后液中铜的浓度，是指除铝后液中铜的浓度小于0.1g/L时，向除铝后液中添加含铜物料补铜；所述含铜物料选自氧化铜、氢氧化铜、硫酸铜、硝酸铜、氯化铜、碱式碳酸铜中的一种。The present invention is a method for comprehensive recovery of copper, selenium and uranium in acid leaching solution for extracting vanadium from stone coal. The described control of the concentration of copper in the solution after aluminum removal refers to when the concentration of copper in the solution after aluminum removal is less than 0.1g/L. Add copper-containing material to the liquid after aluminum removal; the copper-containing material is selected from one of copper oxide, copper hydroxide, copper sulfate, copper nitrate, copper chloride, and basic copper carbonate.
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，所述富磷物料选自磷酸、磷酸钾、磷酸一氢钾、磷酸二氢钾、磷酸钠、磷酸一氢钠、磷酸二氢钠、磷酸铵、磷酸一氢铵、磷酸二氢铵中的一种。The present invention relates to a comprehensive recovery method for copper, selenium and uranium in vanadium acid leaching solution for extracting vanadium from stone coal. The phosphorus-rich material is selected from phosphoric acid, potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate, sodium phosphate, and sodium monohydrogen phosphate , one of sodium dihydrogen phosphate, ammonium phosphate, ammonium monohydrogen phosphate, and ammonium dihydrogen phosphate.
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，所述的加碱调节溶液pH值是指在除铝后液中加入KOH、K2CO3、KHCO3、氨水、(NH4)2CO3、NH4HCO3中的一种作为pH值调节剂，调节溶液的pH值至0.2~2.5。The present invention relates to a method for comprehensive recovery of copper, selenium and uranium in acid leaching solution for extracting vanadium from stone coal. The pH adjustment of the solution by adding alkali refers to adding KOH, K 2 CO 3 , KHCO 3 , and ammonia water to the solution after aluminum removal , (NH 4 ) 2 CO 3 , and NH 4 HCO 3 as a pH regulator to adjust the pH of the solution to 0.2-2.5.
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，所述还原剂选自铁粉、锌粉、铝粉、硫代硫酸钠、亚硫酸钠、二氧化硫中的至少一种。The invention discloses a method for comprehensively recovering copper, selenium and uranium in an acid leaching solution for extracting vanadium from stone coal, wherein the reducing agent is selected from at least one of iron powder, zinc powder, aluminum powder, sodium thiosulfate, sodium sulfite and sulfur dioxide.
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，所述还原沉淀工艺参数为：温度0~60℃，搅拌时间0.1~5h。The invention discloses a method for comprehensively recovering copper, selenium and uranium in an acid leaching solution for extracting vanadium from stone coal. The reduction precipitation process parameters are as follows: temperature 0-60°C, stirring time 0.1-5 hours.
本发明一种石煤提钒酸浸液中铜、硒、铀综合回收方法，所述陈化的时间为1~10h，使铜、硒、铀的沉淀物颗粒长大，便于液固分离。The invention discloses a method for comprehensively recovering copper, selenium and uranium in an acid leaching solution for extracting vanadium from stone coal. The aging time is 1 to 10 hours, so that the precipitate particles of copper, selenium and uranium grow up to facilitate liquid-solid separation.
本发明与已有的技术相比具有以下优点及效果：Compared with the existing technology, the present invention has the following advantages and effects:
本发明的优势在于巧妙地利用还原沉淀技术，以磷为铀的沉淀剂，以铜为硒和铀的沉淀诱导剂，使铀在特定的pH条件下，还原形成难溶的磷酸盐沉淀析出，硒则以硒化铜的形式析出。补铜的目的是为了还原过程在溶液中形成足量的铜粉，以捕集硒和铀的沉淀物；加磷调节铀/磷摩尔比的目的则是促使溶液中的铀沉淀更完全；陈化的作用是使铜、硒和铀沉淀物颗粒长大，便于液固分离，以实现石煤提钒过程铜、硒、铀的高效分离富集。通过本发明工艺的整体重新设计，各个步骤间的相互配合，因而可有效回收石煤酸浸提钒液中的铜、硒和铀，避免了含铜的放射性废水废渣的产生，减少石煤提钒对环境造成的污染，也符合我国节能减排技术改造的发展趋势。The advantage of the present invention is that the reduction precipitation technology is cleverly used, phosphorus is used as the precipitating agent for uranium, and copper is used as the precipitation inducer for selenium and uranium, so that uranium is reduced to form insoluble phosphate precipitation under specific pH conditions, Selenium is precipitated in the form of copper selenide. The purpose of supplementing copper is to form a sufficient amount of copper powder in the solution during the reduction process to capture the precipitates of selenium and uranium; the purpose of adding phosphorus to adjust the molar ratio of uranium/phosphorus is to promote more complete precipitation of uranium in the solution; The function of chemicalization is to make the precipitate particles of copper, selenium and uranium grow up, which is convenient for liquid-solid separation, so as to realize the efficient separation and enrichment of copper, selenium and uranium in the process of vanadium extraction from stone coal. Through the overall redesign of the process of the present invention and the mutual cooperation between the various steps, copper, selenium and uranium in the vanadium leaching solution of stone coal acid leaching can be effectively recovered, the generation of radioactive waste water containing copper is avoided, and the reduction of waste water from stone coal extraction is reduced. The pollution caused by vanadium to the environment is also in line with the development trend of my country's energy-saving and emission-reduction technological transformation.
具体实施方式 Detailed ways
下面结合实施例，对本发明作进一步描述，以下实施例旨在说明本发明而不是对本发明的进一步限定。The present invention will be further described below in conjunction with the examples, and the following examples are intended to illustrate the present invention rather than further limit the present invention.
实施例1Example 1
取含V2O5 4.86g/L、Cu 0.09g/L、U 5mg/L、P 1.1g/L的石煤酸浸溶液6000ml，加入150g硫酸钾和50g氯化钾使溶液中的铝以钾明矾的形式结晶析出，过滤得钾明矾和除铝后液；除铝后液先加入硫酸铜，使溶液中铜的浓度升至0.6g/L Cu，再加入磷酸使溶液中的铀/磷摩尔比增至1:600，然后加入碳酸钾调pH至0.2，最后按除铝后液中铁和钒还原成Fe(II)和V(IV)化学反应计量数的1.5倍加入还原铁粉，室温还原2h，陈化1h，过滤得到含Cu 5mg/L、U﹤1mg/L的还原后液和含Cu 43.2%、P 1.1%、Se 1.3%、U 0.33%的还原渣。还原后液萃取提钒，还原渣收集作为分离回收铜、硒、铀的原料。Get 6000ml of stone coal acid leaching solution containing V 2 O 5 4.86g/L, Cu 0.09g/L, U 5mg/L, P 1.1g/L, add 150g of potassium sulfate and 50g of potassium chloride to make the aluminum in the solution The form of potassium alum is crystallized and separated out, and the potassium alum and the solution after removing aluminum are obtained by filtering; the solution after removing aluminum is firstly added with copper sulfate to make the concentration of copper in the solution rise to 0.6g/L Cu, and then add phosphoric acid to make the uranium/phosphorus in the solution Increase the molar ratio to 1:600, then add potassium carbonate to adjust the pH to 0.2, and finally add reduced iron powder according to 1.5 times the stoichiometric number of iron and vanadium in the solution after aluminum removal to Fe(II) and V(IV), at room temperature Reduction for 2 hours, aging for 1 hour, and filtration to obtain the reduced solution containing Cu 5mg/L, U<1mg/L and the reduced residue containing Cu 43.2%, P 1.1%, Se 1.3%, and U 0.33%. After reduction, vanadium is extracted by liquid extraction, and the reduction slag is collected as raw materials for the separation and recovery of copper, selenium and uranium.
实施例2Example 2
取含V2O5 5.61g/L、Cu 0.17g/L、U 41mg/L、P 3.2g/L的石煤酸浸溶液10000ml，加入220g硫酸铵和50g碳酸铵，使溶液中的铝以铵明矾的形式结晶析出，过滤得铵明矾和除铝后液；除铝后液先加入氯化铜，使溶液中铜的浓度升至1.1g/L Cu；加磷酸一氢钠使溶液中的铀/磷摩尔比增至1:120，再后加入碳酸氢钠调pH至1.5，然后按除铝后液中铁和钒还原成Fe(II)和V(IV)化学反应计量数的1.2倍加入硫代硫酸钠，60℃还原0.1h，陈化3h，过滤得含Cu 3mg/L、U﹤1mg/L的还原后液和含Cu 49.1%、Se 2.7%、P 2.2%、U 1.8%的还原渣。还原后液萃取提钒；还原渣加入稀硫酸和适量双氧水搅拌后过滤，得到含铀溶液和铜硒渣；含铀溶液加氢氧化钠中和结晶析出黄色的重铀酸钠；铜硒渣加硫酸焙烧，焙烧烟气水吸收得粗硒，焙砂加稀硫酸溶解、过滤，滤液蒸发结晶得硫酸铜。Take 10000ml of stone coal acid leaching solution containing V 2 O 5 5.61g/L, Cu 0.17g/L, U 41mg/L, P 3.2g/L, add 220g ammonium sulfate and 50g ammonium carbonate to make the aluminum in the solution The form crystallization of ammonium alum separates out, filters and obtains ammonium alum and the liquid after removing aluminum; Add copper chloride earlier to the liquid after removing aluminum, make the concentration of copper in the solution rise to 1.1g/L Cu; Add sodium monohydrogen phosphate to make the solution in the solution Increase the uranium/phosphorus molar ratio to 1:120, then add sodium bicarbonate to adjust the pH to 1.5, and then add 1.2 times the stoichiometric number of Fe(II) and V(IV) in the liquid after the removal of aluminum Sodium thiosulfate, reduced at 60°C for 0.1h, aged for 3h, filtered to obtain the reduced liquid containing Cu 3mg/L, U<1mg/L and the liquid containing Cu 49.1%, Se 2.7%, P 2.2%, U 1.8%. Reduction slag. After reduction, vanadium is extracted by liquid extraction; the reduction residue is added with dilute sulfuric acid and appropriate amount of hydrogen peroxide, stirred and filtered to obtain uranium-containing solution and copper-selenium slag; Sulfuric acid roasting, roasting flue gas water absorption to obtain crude selenium, calcined sand added dilute sulfuric acid to dissolve, filter, the filtrate evaporates and crystallizes to obtain copper sulfate.
实施例3Example 3
取含V2O5 6.38g/L、Cu 0.81g/L、U 1.0mg/L、P 4.1g/L的石煤酸浸溶液3000ml，先氨水调pH值至2.5，使溶液中的铝以铵明矾的形式结晶析出，过滤得铵明矾和除铝后液；由于溶液中已有足量的铜，且铀/磷摩尔比已达1:4100，所以还原前无需补铜和加磷。除铝后液按其中铁和钒还原成Fe(II)和V(IV)化学反应计量数的2倍加入锌粉，15℃还原5h，陈化10h，过滤得含Cu 1.5mg/L、U﹤1mg/L的还原后液和含Cu 44.2%、Se 1.8%、P 1.1%、U 0.06%的还原渣。还原后液萃取提钒，还原渣收集作为分离回收铜、硒、铀的原料。Take 3000ml of stone coal acid leaching solution containing V 2 O 5 6.38g/L, Cu 0.81g/L, U 1.0mg/L, P 4.1g/L, adjust the pH value to 2.5 with ammonia water first, so that the aluminum in the solution is The form of ammonium alum crystallizes out, and the ammonium alum and the solution after aluminum removal are obtained by filtration; since there is sufficient copper in the solution, and the uranium/phosphorus molar ratio has reached 1:4100, there is no need to supplement copper and phosphorus before reduction. Add zinc powder to the solution after removing aluminum according to twice the stoichiometric number of iron and vanadium reduced to Fe(II) and V(IV), reduce at 15°C for 5 hours, age for 10 hours, and filter to obtain Cu 1.5mg/L, U <1mg/L reduced liquid and reduced slag containing Cu 44.2%, Se 1.8%, P 1.1%, U 0.06%. After reduction, vanadium is extracted by liquid extraction, and the reduction slag is collected as raw materials for the separation and recovery of copper, selenium and uranium.
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