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WO2019071642A1 - 一种从废铅酸蓄电池铅膏中湿法回收铅的方法 - Google Patents

一种从废铅酸蓄电池铅膏中湿法回收铅的方法 Download PDF

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Publication number
WO2019071642A1
WO2019071642A1 PCT/CN2017/106567 CN2017106567W WO2019071642A1 WO 2019071642 A1 WO2019071642 A1 WO 2019071642A1 CN 2017106567 W CN2017106567 W CN 2017106567W WO 2019071642 A1 WO2019071642 A1 WO 2019071642A1
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lead
zinc
leaching
reducing agent
acid battery
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PCT/CN2017/106567
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English (en)
French (fr)
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王成彦
邢鹏
陈永强
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北京科技大学
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Priority to US16/499,374 priority Critical patent/US11502344B2/en
Publication of WO2019071642A1 publication Critical patent/WO2019071642A1/zh

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/54—Reclaiming serviceable parts of waste accumulators
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00—Obtaining lead
    • C22B13/04—Obtaining lead by wet processes
    • C22B13/045—Recovery from waste materials
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/06—Lead-acid accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/14—Electrodes for lead-acid accumulators
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

Definitions

  • the invention relates to the field of hydrometallurgy technology, in particular to a method for recovering lead from lead-acid battery lead paste.
  • lead consumption of lead-acid batteries accounts for about 85% of the total lead consumption.
  • China's lead battery production accounts for about one-third of the world's output, and the annual discarded batteries amount to more than 1.5 million tons, which has become a huge renewable lead resource.
  • Lead-acid batteries are usually crushed and sorted to produce lead grids, organic waste plastics and lead paste.
  • the recycling of lead grids and organic waste plastics is relatively simple, and the composition of lead paste is complex and the recycling technology is difficult.
  • the pyrometallurgical process for treating lead paste commonly uses a desulfurizing agent to pre-convert PbSO 4 in the lead paste to Pb 2 CO 3 , and the converted Pb 2 CO 3 can be fire-smelted at a lower temperature. Since the conversion is incomplete, about 5% of PbSO 4 is usually left in the converted lead paste, and SO 2 is generated in the smelting.
  • the pyrometallurgical process for treating lead paste not only has high energy consumption, but also consumes a large amount of desulfurizer, and also generates atmospheric pollutants such as SO 2 and volatile lead dust, and the treatment cost of the smelting flue gas is high.
  • the technical problem to be solved by the present invention is to provide a method for recovering lead from a lead-acid battery lead paste, thereby realizing direct extraction of a high content of metal lead from a lead paste.
  • the treatment object of the method is a lead-acid battery lead paste, and the specific steps are as follows:
  • the lead paste processed in the step (1) contains 60 to 75% of Pb; the leaching temperature is 20 to 95 ° C, the leaching time is 0.5 to 4 hours, the concentration of the zinc chloride solution is 100 to 600 g/L, and the lead paste is before leaching.
  • the liquid-solid ratio in the mixed solution composed of the zinc chloride solution and the reducing agent is 20 to 40:1, the equipment used for the leaching is a stirring mill, and the pH of the solution is controlled to be 1.0-4.0 with hydrochloric acid during the leaching process.
  • the metal zinc used in the step (2) is electro-zinc, the replacement temperature is 20 to 90 ° C, the amount of metal zinc is 1 to 1.1 times the theoretical amount, and the replacement time is 0.5 to 2 h.
  • the current density of the zinc electrowinning in the step (3) is 100-500 A/m 2 , the temperature is 10-60 ° C, the anode is graphite or a rhodium-plated titanium plate, and the cathode is a titanium plate.
  • the reaction temperature is 10-60 ° C, and the amount of calcium chloride is 1-1.1 times the theoretical amount.
  • the zinc chloride leaching agent can be recycled, and the metal zinc consumed in the leaching and replacing process enters the solution and is recycled by electrowinning.
  • the lead extraction process consumes only a small amount of calcium chloride, and the reagent consumption is small.
  • the sulfate ions entering the solution after leaching can be crystallized in the form of calcium sulfate, which can be used as building materials and additives.
  • FIG. 1 is a process flow diagram of a method for wetly recovering lead from a lead-acid battery lead paste of the present invention.
  • the invention provides a method for wetly recovering lead from lead-acid battery lead paste. As shown in Figure 1, Process flow chart for the method. The method specifically includes steps of leaching, replacing lead, zinc electrowinning, solution purification, etc., which will be described below in conjunction with specific embodiments.
  • Leaching 100g lead paste (Pb 71.1%), leaching agent is 500g/L zinc chloride solution, reducing agent electric zinc (zinc content 99.5%) dosage is 9g, leaching temperature 80 °C, leaching time 2h, liquid-solid ratio 20: 1, leaching pH 2.0, lead leaching rate of 98.2%.
  • Displacement lead electric zinc (zinc content 99.5%) was used as a displacer, the replacement temperature was 25 ° C, the amount of zinc was 1 times the theoretical amount, and the replacement was 1 h, and a total of 69.9 g of lead mud was obtained, and the lead content was 99.7%.
  • Zinc electrowinning using a ruthenium-plated titanium plate as the anode and a titanium plate as the cathode, accumulating for 2 hours at a current density of 250 A/m 2 and a temperature of 25 ° C, producing zinc (zinc content 99.5%) 31.5 g, current efficiency 93.4 %.
  • Leaching 100g lead paste (Pb 70.5%), leaching agent 500g/L zinc chloride solution, reducing agent lead (pure lead) dosage 26.5g, leaching temperature 65 °C, leaching time 2h, liquid-solid ratio 22:1, Leaching pH 2.5, the lead leaching rate reached 97.8%.
  • Displacement lead electric zinc (zinc content 99.5%) was used as a displacer, the replacement temperature was 30 ° C, the amount of zinc was 1 times the theoretical amount, and the replacement was 1 h, and a total of 69.1 g of lead mud was obtained, and the lead content was 99.5%.
  • Zinc electrowinning using a ruthenium-plated titanium plate as the anode and a titanium plate as the cathode, accumulating for 1.6 h at a current density of 300 A/m 2 and a temperature of 25 ° C, producing zinc (zinc content 99.3%) 30.2 g, current efficiency 93.1%.
  • Leaching 10g lead paste (Pb 68.4%), leaching agent is 400g/L zinc chloride solution, reducing agent hydrogen peroxide dosage is 3mL, leaching temperature 80°C, leaching time 2h, liquid-solid ratio 25:1, leaching pH 3.0, lead The leaching rate is 95.7%.
  • Displacement lead using electro-zinc (zinc content 99.5%) as a displacer, the replacement temperature is 30 ° C, and the amount of zinc is The theoretical amount was doubled and replaced by 1 h, and a total of 6.6 g of lead mud was obtained, and the lead content was 99.4%.
  • Zinc electrowinning graphite as the anode and titanium plate as the cathode.
  • the electric current is 0.5 h at a current density of 150 A/m 2 and a temperature of 30 ° C.
  • the electric zinc (zinc content is 99.6%) is 2.1 g, and the current efficiency is 93.8%.

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  • Manufacturing & Machinery (AREA)
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  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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Abstract

一种从废铅酸蓄电池铅膏中回收铅的方法，属于湿法冶金技术领域。该方法先将还原剂、铅膏加入氯化锌溶液于搅拌磨中进行浸出，使其中的铅进入溶液，浸出液用金属锌置换铅，铅置换后，控制氯化锌溶液少量电积产出电锌，所述还原剂为金属锌或金属铅或双氧水，一部分电锌作为还原剂返回浸出用，用金属铅或双氧水作还原剂时可省略作为还原剂返回的步骤，剩余电锌作为置换剂返回置换铅，电积后液加入少量氯化钙脱除硫酸根后作为浸出剂返回铅膏浸出使用。本工艺具有流程短、工序少、能耗成本低等特点，并满足清洁生产的环保要求。

Description

一种从废铅酸蓄电池铅膏中湿法回收铅的方法 技术领域
本发明涉及湿法冶金技术领域，特别是指一种从废铅酸蓄电池铅膏中回收铅的方法。
背景技术
在铅的消费结构中，铅酸蓄电池的耗铅量占铅总消耗量的85％左右。我国铅蓄电池产量约占世界产量的1/3，每年报废的蓄电池达150万吨以上，已成为一个巨大的可再生铅资源。
废铅酸蓄电池通常先经破碎分选产出的铅板栅、有机废塑料和铅膏。铅板栅、有机废塑料的回收较为简单，而铅膏成分复杂，回收技术难度大。
目前处理铅膏的火法冶金工艺常用脱硫剂将铅膏中的PbSO4预先转化为Pb2CO3，转化后的Pb2CO3可在较低的温度下进行火法熔炼。由于转化不完全，一般会有5％左右的PbSO4残留在转化后的铅膏中，在熔炼中会产生SO2。火法冶金工艺处理铅膏不仅能耗高，脱硫剂消耗量大，而且会产生SO2、挥发性铅尘等大气污染物，熔炼烟气处理成本高。
发明内容
本发明要解决的技术问题是提供一种从废铅酸蓄电池铅膏中回收铅的方法，实现从铅膏中直接提取得到高含量的金属铅。
该方法的处理对象是废铅酸蓄电池铅膏，具体包括步骤如下：
(1)以金属锌或金属铅或双氧水为还原剂，氯化锌溶液为浸出剂浸出铅膏，浸出完成后通过液固分离得到浸出渣和浸出液；
(2)向步骤(1)得到的浸出液中加入金属锌进行置换铅，得到金属铅和置换后液；
(3)将步骤(2)得到的置换后液少量电积，得到电锌和电积后液；
(4)将步骤(3)得到的电锌一部分作为还原剂返回步骤(1)浸出用(用金属铅或双氧水作还原剂时该步骤可省略)，剩余电锌作为置换剂返回步骤(2)置换铅；
(5)向步骤(3)得到的电积后液加入氯化钙脱除溶液中的硫酸根离子，得到硫酸钙和净化后液；
(6)将步骤(5)得到的净化后液重新作为浸出剂返回步骤(1)。
其中，步骤(1)中处理的铅膏含Pb 60～75％；浸出温度为20～95℃，浸出时间为0.5～4h，氯化锌溶液浓度为100～600g/L，浸出前，铅膏、氯化锌溶液和还原剂组成的混合溶液中的液固比为20～40:1，浸出所用设备为搅拌磨；浸出过程用盐酸控制溶液pH为1.0-4.0。
步骤(2)中所用金属锌为电锌，置换温度为20～90℃，金属锌用量为理论量1～1.1倍，置换时间0.5-2h。
步骤(3)中锌电积的电流密度为100-500A/m2，温度10-60℃，阳极为石墨或镀钌钛板，阴极为钛板。
步骤(5)中反应温度10-60℃，氯化钙用量为1-1.1倍理论量。
本发明的上述技术方案的有益效果如下：
与火法冶金方法比，能耗低，满足清洁生产的环保要求。氯化锌浸出剂可循环使用，浸出和置换过程消耗的金属锌进入溶液后又通过电积的方式产出循环使用，提铅过程只消耗少量氯化钙，试剂消耗少。除能直接得到高含量的金属铅外，浸出后进入溶液中的硫酸根离子能以硫酸钙形式结晶，硫酸钙可用作建筑材料和添加剂。
附图说明
图1为本发明的从废铅酸蓄电池铅膏中湿法回收铅的方法工艺流程图。
具体实施方式
为使本发明要解决的技术问题、技术方案和优点更加清楚，下面将结合附图及具体实施例进行详细描述。
本发明提供一种从废铅酸蓄电池铅膏中湿法回收铅的方法。如图1所示， 为该方法的工艺流程图。该方法具体包括浸出、置换铅、锌电积、溶液净化等步骤，下面结合具体实施例予以说明。
实施例1
浸出：100g铅膏(Pb 71.1％)，浸出剂为500g/L氯化锌溶液，还原剂电锌(锌含量99.5％)用量为9g，浸出温度80℃，浸出时间2h，液固比20:1，浸出pH 2.0，铅浸出率达98.2％。
置换铅：采用电锌(锌含量99.5％)作置换剂，置换温度25℃，锌用量为理论量1倍，置换1h，得到铅泥共69.9g，铅含量99.7％。
锌电积：以镀钌钛板为阳极，钛板为阴极，在电流密度为250A/m2、温度25℃条件下电积2h，产电锌(锌含量99.5％)31.5g，电流效率93.4％。
电积后液净化：温度25℃条件下，在循环的铅电积后液中根据硫酸根离子浓度加入1倍理论量的氯化钙，形成硫酸钙沉淀，控制溶液中的硫酸根浓度在20g/L。
实施例2
浸出：100g铅膏(Pb 70.5％)，浸出剂为500g/L氯化锌溶液，还原剂铅(纯铅)用量为26.5g，浸出温度65℃，浸出时间2h，液固比22:1，浸出pH 2.5，铅浸出率达97.8％。
置换铅：采用电锌(锌含量99.5％)作置换剂，置换温度30℃，锌用量为理论量1倍，置换1h，得到铅泥共69.1g，铅含量99.5％。
锌电积：以镀钌钛板为阳极，钛板为阴极，在电流密度为300A/m2、温度25℃条件下电积1.6h，产电锌(锌含量99.3％)30.2g，电流效率93.1％。
电积后液净化：温度25℃条件下，在循环的铅电积后液中根据硫酸根离子浓度加入1倍理论量的氯化钙，形成硫酸钙沉淀，控制溶液中的硫酸根浓度在20g/L。
实施例3
浸出：10g铅膏(Pb 68.4％)，浸出剂为400g/L氯化锌溶液，还原剂双氧水用量为3mL，浸出温度80℃，浸出时间2h，液固比25:1，浸出pH 3.0，铅浸出率达95.7％。
置换铅：采用电锌(锌含量99.5％)作置换剂，置换温度30℃，锌用量为 理论量1倍，置换1h，得到铅泥共6.6g，铅含量99.4％。
锌电积：以石墨为阳极，钛板为阴极，在电流密度为150A/m2、温度30℃条件下电积0.5h，产电锌(锌含量99.6％)2.1g，电流效率93.8％。
电积后液净化：温度20℃条件下，在循环的铅电积后液中根据硫酸根离子浓度加入1倍理论量的氯化钙，形成硫酸钙沉淀，控制溶液中的硫酸根浓度在20g/L。
以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明所述原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (7)

  1. 一种从废铅酸蓄电池铅膏中湿法回收铅的方法，其特征在于：包括以下步骤：
    (1)以金属锌或金属铅或双氧水为还原剂，氯化锌溶液为浸出剂浸出铅膏，浸出完成后通过液固分离得到浸出渣和浸出液；
    (2)向步骤(1)得到的浸出液中加入金属锌进行置换铅，得到金属铅和置换后液；
    (3)将步骤(2)得到的置换后液少量电积，得到电锌和电积后液；
    (4)将步骤(3)得到的电锌一部分作为还原剂返回步骤(1)浸出用(用金属铅或双氧水作还原剂时该步骤可省略)，剩余电锌作为置换剂返回步骤(2)置换铅；
    (5)向步骤(3)得到的电积后液加入氯化钙脱除溶液中的硫酸根离子，得到硫酸钙和净化后液；
    (6)将步骤(5)得到的净化后液重新作为浸出剂返回步骤(1)使用。
  2. 根据权利要求1所述的从废铅酸蓄电池铅膏中回收铅的方法，其特征在于：所述步骤(1)中处理的铅膏含Pb 60～75％。
  3. 根据权利要求1所述的从废铅酸蓄电池铅膏中回收铅的方法，其特征在于：所述步骤(1)中浸出温度为20～95℃，浸出时间为0.5～4h，氯化锌溶液浓度为100～600g/L，浸出前，铅膏、氯化锌溶液和还原剂组成的混合溶液中的液固比为20～40:1，浸出所用设备为搅拌磨。
  4. 根据权利要求1所述的从废铅酸蓄电池铅膏中回收铅的方法，其特征在于：所述步骤(1)中浸出过程用盐酸控制溶液pH为1.0-4.0。
  5. 根据权利要求1所述的从废铅酸蓄电池铅膏中回收铅的方法，其特征在于：所述步骤(2)中所用金属锌为电锌，置换温度为20～90℃，金属锌用量为理论量1～1.1倍，置换时间0.5-2h。
  6. 根据权利要求1所述的从废铅酸蓄电池铅膏中回收铅的方法，其特征在于：所述步骤(3)中锌电积的电流密度为100-500A/m2，温度10-60℃，阳极为石墨或镀钌钛板，阴极为钛板。
  7. 根据权利要求1所述的从废铅酸蓄电池铅膏中回收铅的方法，其特征在于：所述步骤(5)中反应温度10-60℃，氯化钙用量为1-1.1倍理论量，硫酸根浓度控制在20g/L。
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