CN100560758C - Method for recycling indium from waste mercury-free alkaline zinc-manganese dioxide battery - Google Patents
Method for recycling indium from waste mercury-free alkaline zinc-manganese dioxide battery Download PDFInfo
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- CN100560758C CN100560758C CNB2007100285218A CN200710028521A CN100560758C CN 100560758 C CN100560758 C CN 100560758C CN B2007100285218 A CNB2007100285218 A CN B2007100285218A CN 200710028521 A CN200710028521 A CN 200710028521A CN 100560758 C CN100560758 C CN 100560758C
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Abstract
The invention discloses a method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries, which comprises the following steps: separating and extracting negative electrode substances of the waste mercury-free alkaline zinc-manganese dioxide battery, dissolving the negative electrode substances with acid, adding a reducing agent to replace sponge indium, smelting the sponge indium to obtain indium ingots, and using filtrate for preparing zinc by electrolysis; or the pH value of the solution is adjusted to 5 by using the alkaline solution after the solution is dissolved by using the acid, and the indium becomes In (OH) 3 Precipitating, filtering, using filtrate for electrolyzing to prepare zinc, dissolving the precipitate with acid as electrolyte, and electrolyzing to obtain pure indium. The method provided by the invention has the advantages that the indium is recovered according to the existing state of the indium in the waste alkaline zinc-manganese dioxide battery and the actual recovery process of the waste mercury-free alkaline zinc-manganese dioxide battery, the operation process is simple, and the implementation is easy; the recovery rate of indium is high and stable, and the chemical substances added in the recovery process are few, so that secondary pollution is hardly generated; the purity of the extracted metal indium is high, so that the recycling of the anode material of the waste alkali-manganese battery is realized; therefore, the method has better economic benefit and environmental protection value.
Description
Technical Field
The invention relates to a waste battery recovery technology, in particular to a method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries.
Background
China is a large country for producing and consuming zinc-manganese batteries. From 1/2005, the domestic alkaline zinc-manganese battery has reached complete amalgamation, and the production and consumption of the alkaline zinc-manganese battery occupy the dominant position of primary batteries. The main measure of the alkali zinc-manganese battery without mercury is to use a suitable mercury substitute additive. The mercury substitute additive usually comprises inorganic type (such as indium, gallium, thallium, aluminum and other metal elements or compounds) and organic type (such as biphenyl, alcamines, amides and other compounds) for achieving the effect of mercury in the battery. There are many combinations of mercury-substituting additives used in literature and production practice, however, regardless of which combination, indium is an essential component. The indium added to the cathode of the alkaline zinc-manganese battery generally comprises In and In 2 O 3 And In (OH) 3 Three forms. Since indium has a larger electrode potential than zinc, indium added to zinc powder is mostly present In the form of In. Because the utilization rate of the zinc of the cathode is not 100 percent, the indium is in the waste alkaline zinc-manganese batteryThe presence In the cell is largely still In the form of In. Although the content of indium in the waste alkaline zinc-manganese dioxide battery is small, the indium is less abundant in the earth crust and is a rare and precious metal. Therefore, the indium in the waste alkaline zinc-manganese dioxide battery is extracted and utilized, so that the harm to environmental water and soil can be reduced, better economic benefit can be obtained, and the method has great significance for the sustainable development of the society.
The recycling of the waste alkaline zinc-manganese dioxide battery has been widely researched. The patent application number of 200510036193.7 of a recycling method of waste alkaline zinc-manganese batteries discloses a recycling method of waste alkaline zinc-manganese batteries, which comprises the following steps: separating and extracting anode and cathode substances of the waste alkaline zinc-manganese dioxide battery, leaching with alkaline liquor at room temperature, separating zincate, electrolyzing to prepare zinc, preparing potassium manganate, electrolyzing to prepare potassium permanganate and the like, but the method mainly recovers zinc and manganese, and does not mention extraction of metal indium and graphite. The patent application No. 200510120906.8 'method for extracting metal indium and graphite from waste alkaline zinc-manganese dioxide batteries' discloses a method for extracting metal indium and graphite from waste alkaline zinc-manganese dioxide batteries, which is characterized In that indium is insoluble In alkaline solution, and In is insoluble In alkaline solution 2 O 3 Insoluble In alkaline solution, in (OH) 3 The indium is extracted by the property of difficult dissolution in an alkaline solution with certain alkalinity. However, the method is relatively high in treatment processOxidant (unused anode material MnO) 2 ) Indium may be converted into In (OH) 3 Due to In (OH) 3 The complexity of dissolution in alkaline solutions is such that loss of indium is easily caused, and therefore, this method has the disadvantages of poor and unstable recovery.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for recovering indium from the waste mercury-free alkaline zinc-manganese dioxide battery, which has the advantages of simple process, low cost, high recovery rate and stability.
The purpose of the invention is realized by the following technical scheme: a method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries comprises the following steps: separating and extracting negative substances of the waste mercury-free alkaline zinc-manganese dioxide battery, dissolving the negative substances with acid (the pH value of the solution is less than 1), adding a reducing agent to replace sponge indium, filtering, smelting the sponge indium to obtain indium ingots, and using filtrate for preparing zinc by electrolysis; or adjusting the pH value of the solution to 4.5-5.0 with alkali solution after dissolving with acid, wherein the indium is changed into In (OH) 3 Precipitating, filtering, using the filtrate for preparing zinc by electrolysis, dissolving the precipitate with acid, adjusting the dissolved precipitate into electrolyte, and electrolyzing to obtain pure indium.
The negative electrode material, the acid and the water are prepared according to the following weight percentage:
8 to 20 percent of negative electrode material
10 to 25 percent of acid
55 to 82 percent of water.
The acid may be an inorganic acid such as sulfuric acid, hydrochloric acid, fluoroboric acid, etc. The pH value of the solution is controlled to be less than 1.
The proportion of the reducing agent to the anode material before dissolution is as follows in percentage by weight:
40 to 60 percent of negative electrode material
40 to 60 percent of reducing agent
The reducing agent can adopt active metal, such as zinc, aluminum, magnesium and the like.
The sponge indium smelting conditions are as follows:
the sponge indium and alkali proportion is as follows by weight percent:
40 to 50 percent of sponge indium
50 to 60 percent of alkali
The alkali can be sodium hydroxide, potassium hydroxide, etc.
The smelting temperature is 400-500 ℃.
The alkali liquor for adjusting the pH value is prepared from the following substances in percentage by weight:
5 to 10 percent of alkali
90 to 95 percent of water.
The alkali can be sodium hydroxide, potassium hydroxide, etc.
The precipitate is dissolved by acid, and the acid and the water are prepared according to the following weight percentage:
5 to 30 percent of acid
70 to 95 percent of water.
The acid may be an inorganic acid such as sulfuric acid, hydrochloric acid, fluoroboric acid, etc.
The electrolyte comprises the following substances in percentage by weight:
0.1 to 10 percent of indium ions
1 to 15 percent of sodium salt or potassium salt
84.9 to 89 percent of water
The conditions of the electrolysis are as follows: the pH value of the electrolyte is 1-3; the temperature is 20-30 ℃, and the cathode current density is 10-500A/m 2 The anode is an insoluble anode and can be graphite, metallic titanium and the like; the cathode is a metal indium sheet, a pure aluminum sheet, a titanium sheet and the like.
The electrolyzed solution can be returned to the previous step for recycling.
Compared with the prior art, the invention has the following advantages and effects: the method has the advantages that the indium is recovered according to the existing state of the indium in the waste alkaline zinc-manganese dioxide battery and the actual recovery process of the waste mercury-free alkaline zinc-manganese dioxide battery, the operation process is simple, and the implementation is easy; the recovery rate of indium is high and stable, and few chemical substances are added in the recovery process, so that secondary pollution is hardly generated; the indium content of the metal indium extracted by the reducing agent is 95-99 percent, the purity of the metal indium extracted by the electrolysis method is high, and the indium content is more than 99.9 percent, so that the recycling of the cathode material of the waste alkaline manganese battery is realized; the value created by the extract is far higher than the recovery and production cost, so that the extract has better economic benefit and environmental protection value.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Examples
The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries comprises the following steps: the method is characterized in that the negative electrode material of the waste mercury-free alkaline zinc-manganese dioxide battery is separated and extracted, and can be prepared by adopting the existing method, such as: the method comprises the steps of adopting a 'recovery processing device of waste alkaline zinc-manganese dioxide batteries' with the patent application number of 200620059353.X to cut the waste mercury-free alkaline manganese dioxide batteries apart, separating a positive electrode and a negative electrode by screening, taking out the negative electrode, and removing a brass nail, a plastic cover and a diaphragm to obtain a negative electrode substance.
After obtaining the above negative electrode material, the following steps were then carried out:
| step (ii) of | Example 1 | Example 2 | Example 3 |
| (1) Acid soluble | The negative electrode material is mixed at room temperature Soaking in sulfuric acid, and stirring to dissolve And (5) solving. Negative electrode material, sulfuric acid, and water Is prepared from the following components in percentage by weight And the following steps: 8 percent of negative electrode material Sulfuric acid content is 10% 82 percent of water Controlling the pH value of the solutionSmall food At 1. | Negative electrode material at room temperature Soaking in fluoboric acid, and stirring And (4) dissolving. A negative electrode material, fluoroboric acid, The water is prepared according to the following weight percentage The preparation method comprises the following steps: negative electrode material 14% 18 percent of fluoboric acid 68 percent of water The pH value of the solution needs to be controlled to be small 1, the reaction is carried out. | The negative electrode material is mixed at room temperature Soaking in hydrochloric acid, and stirring And (4) dissolving. A negative electrode material, hydrochloric acid, The water is prepared according to the following weight percentage The preparation method comprises the following steps: 20 percent of negative electrode material Hydrochloric acid 25% 55 percent of water The pH value of the solution is controlled Less than 1. |
| (2) Replacement of | Containing indium in step 1 Adding zinc powder into the solution to replace And (4) sponge indium. Zinc powder and dissolved precursor The ratio of polar substances is defined by The weight percentages of the substances are as follows: 40 percent of negative electrode material 60 percent of zinc powder | Indium-containing solution in step 1 Adding aluminium powder into the liquid to displace the sea And (5) cotton indium. Aluminum powder and anode before dissolution The ratio of the substances is composed of The weight percentages are as follows: 50% of negative electrode material 50 percent of aluminum powder | Containing indium in step 1 Adding magnesium powder into the solution to displace And (4) sponge indium. Magnesium powder and before dissolution The ratio of the negative electrode material is as follows The substances are calculated by weight percent as The following: the negative electrode material is 60% 40 percent of magnesium powder |
| (3) Smelting of | The sponge in the step 2 Mixing and melting the indium and the sodium hydroxide, an indium ingot can be obtained. Sponge indium and sodium hydroxide Is prepared from the following materials in percentage by weight The weight percentage is as follows: sponge indium 40% 60 percent of sodium hydroxide Melting temperature: at 400 deg.c. | The sponge indium in the step 2 is treated Mixing with sodium hydroxide, and melting Indium ingots can be obtained. Sponge indium and sodium hydroxide The ratio of (A) to (B) is calculated by weight The weight percentage is as follows: sponge indium 60% Sodium hydroxide 40% Melting temperature: at 500 deg.c. | The sponge in the step 2 Mixed melting of indium and potassium hydroxide And melting to obtain indium ingots. Sponge indium and potassium hydroxide The ratio of (A) to (B) is calculated by weight The weight percentage is as follows: 50 percent of sponge indium 50 percent of potassium hydroxide Melting temperature: at 450 deg.c. |
| Step (ii) of | Example 4 | Example 5 | Example 6 |
| (1) Acid soluble | The negative electrode material is mixed at room temperature Soaking in sulfuric acid, and stirring to dissolve And (5) solving. Negative electrode material, sulfuric acid, and water Is prepared from the following components in percentage by weight And the following steps: negative electrode material 8% Sulfuric acid 10% 82 percent of water The pH value of the solution needs to be controlled to be small At 1. | The negative electrode material is mixed at room temperature Soaking in fluoroboric acid, and stirring And (4) dissolving. A negative electrode material, fluoroboric acid, The water is prepared according to the following weight percentage The preparation method comprises the following steps: negative electrode material 14% 18 percent of fluoboric acid 68 percent of water The pH value of the solution needs to be controlled to be small At 1. | The negative electrode material is mixed at room temperature Soaking in hydrochloric acid, and stirring to dissolve And (5) solving. Negative electrode material, hydrochloric acid, and water Is prepared from the following components in percentage by weight And the following steps: 20 percent of negative electrode material Hydrochloric acid 25% 55 percent of water The pH value of the solution needs to be controlled to be small At 1. |
| (2) Precipitation of | The solution obtained in the step 1 is mixed Adjusting the pH with sodium hydroxide solution A value of 4.5, the dissolved indium is In (OH) 3 And (4) precipitating. By using In a pH-adjusted sodium hydroxide solution The liquid is prepared from the following substances in percentage by weight The ratio of ingredients is as follows: sodium hydroxide 5% And (4) 95 percent of water. | The solution obtained in the step 1 is mixed Adjusting the pH with sodium hydroxide solution A value of 5.0, such that the dissolved indium is In (OH) 3 And (4) precipitating. By using In a pH-adjusted sodium hydroxide solution The liquid is prepared from the following substances in percentage by weight The ratio of ingredients is as follows: 10 percent of sodium hydroxide And (5) 90% of water. | The solution obtained in the step 1 is mixed Adjusting the pH of the solution with potassium hydroxide solution A value of 4.8, the dissolved indium is In (OH) 3 And (4) precipitating. By using In a pH-adjusted potassium hydroxide solution The liquid is prepared from the following substances in percentage by weight The ratio is calculated as follows: 7.5 percent of potassium hydroxide 92.5 percent of water. |
| (3) Precipitation solution Solution (II) | Precipitating the precipitate obtained in the step 2 Taken out and dissolved by sulfuric acid. Sulfuric acid, The water is prepared according to the following weight percentage The preparation method comprises the following steps: sulfuric acid 5% 95 percent of water | Precipitating the precipitate obtained in the step 2 Taken out and dissolved by fluoroboric acid. Fluorine Boric acid and water in the following weight percentage Is prepared by the following steps: 18 percent of fluoboric acid 82 percent of water | Precipitating the precipitate obtained in the step 2 Taking out and dissolving with hydrochloric acid. Hydrochloric acid, The water is prepared according to the following weight percentage The preparation method comprises the following steps: hydrochloric acid 30% 70 percent of water |
| (4) Electrolytic extraction Taking out metal | The indium in the step 3 is added The solution is adjusted to be electrolyte and is in the negative And preparing the metal indium. | The indium in the step 3 is added The solution is adjusted to be electrolyte and is in the negative And preparing the metal indium. | The indium in the step 1 is added The solution is adjusted to be electrolyte and is in the negative And preparing the metal indium. |
| Indium (In) | The electrolysis conditions were as follows: electrolyte composition (by weight) Percent): 0.1 percent of indium ions Sodium sulfate 15% Water 84.9% Cathode current density: 500A/m 2 The electrolysis temperature is as follows: 30 deg.C pH value of the electrolyte: 3 Anode: metallic titanium Cathode: metallic indium sheet The electrolyzed solution was returned to (3) The waste water is recycled. | The electrolysis conditions were as follows: electrolyte composition (by weight) Percent): indium ion 5% Sodium fluoborate 8% 87 percent of water Cathode current density: 250A/m 2 The electrolysis temperature is as follows: 25 deg.C pH value of the electrolyte: 2 Anode: metallic titanium Cathode: pure aluminum sheet The electrolyzed solution was returned to (3) And can be recycled. | The electrolysis conditions were as follows: electrolyte composition (by weight) Percent): 10 percent of indium ions 1 percent of potassium chloride 89 percent of water Cathode current density: 10A/m 2 The electrolysis temperature is as follows: 20 deg.C pH value of the electrolyte: 1 Anode: graphite (II) Cathode: metallic titanium sheet The electrolyzed solution was returned to (3) And can be recycled. |
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries is characterized by comprising the following steps: separating and extracting negative electrode substances of the waste mercury-free alkaline zinc-manganese dioxide battery, dissolving the negative electrode substances with acid, adding a reducing agent to replace sponge indium, smelting the sponge indium to obtain indium ingots, and using filtrate for preparing zinc by electrolysis; or adjusting the pH value of the solution to 4.5-5.0 with alkali solution after dissolving with acid, wherein the indium is changed into In (OH) 3 Precipitating, filtering, using filtrate for preparing zinc by electrolysis, dissolving the precipitate with acid, adjusting the dissolved precipitate into electrolyte, and electrolyzing to obtain pure indium.
2. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 1, characterized in that: when the acid is used for dissolving the negative electrode material, the acid and the water are prepared according to the following weight percentage:
8 to 20 percent of negative electrode material
10 to 25 percent of acid
55 to 82 percent of water.
3. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 2, characterized in that: the acid is an inorganic acid.
4. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 1, characterized in that: the proportion of the reducing agent to the anode material before dissolution is as follows in percentage by weight:
40 to 60 percent of negative electrode material
40 to 60 percent of reducing agent
The reducing agent is zinc, aluminum or magnesium.
5. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 1, characterized in that: the sponge indium smelting conditions are as follows:
the sponge indium and alkali proportion is as follows by weight percent:
40 to 50 percent of sponge indium
50 to 60 percent of alkali
The alkali is sodium hydroxide or potassium hydroxide.
6. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 1, characterized in that: the smelting temperature is 400-500 ℃.
7. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 1, characterized in that: the alkali liquor for adjusting the pH value is prepared from the following substances in percentage by weight:
5 to 10 percent of alkali
90 to 95 percent of water
The alkali is sodium hydroxide or potassium hydroxide.
8. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 1, characterized in that: the precipitate is dissolved by acid, and the acid and the water are prepared according to the following weight percentage:
5 to 30 percent of acid
70 to 95 percent of water
The acid is an inorganic acid.
9. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 1, characterized in that: the electrolyte comprises the following substances in percentage by weight:
0.1 to 10 percent of indium ions
1 to 15 percent of sodium salt or sylvite
84.9 to 89 percent of water.
10. The method for recovering indium from waste mercury-free alkaline zinc-manganese dioxide batteries according to claim 1, characterized in that: the conditions of the electrolysis are as follows: the pH value of the electrolyte is 1-3; the temperature is 20-30 ℃, and the cathode current density is 10-500A/m 2 The anode is an insoluble anode; the cathode is a metal indium sheet, a pure aluminum sheet or a titanium sheet.
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| KR101155355B1 (en) * | 2008-02-12 | 2012-06-19 | 제이엑스 닛코 닛세키 킨조쿠 가부시키가이샤 | Method of recovering valuable metals from izo scrap |
| WO2013015032A1 (en) * | 2011-07-26 | 2013-01-31 | Jx日鉱日石金属株式会社 | Method for producing indium hydroxide or compound containing indium hydroxide |
| CN102951618B (en) * | 2011-08-31 | 2014-07-30 | 深圳市格林美高新技术股份有限公司 | Method for recycling germanium, gallium, indium and selenium in waste diode |
| CN103160855A (en) * | 2011-12-15 | 2013-06-19 | 广东先导稀材股份有限公司 | Preparation method of high-purity indium |
| US9555386B2 (en) | 2014-06-20 | 2017-01-31 | Johnson Controls Technology Company | Systems and methods for closed-loop recycling of a liquid component of a leaching mixture when recycling lead from spent lead-acid batteries |
| US9670565B2 (en) | 2014-06-20 | 2017-06-06 | Johnson Controls Technology Company | Systems and methods for the hydrometallurgical recovery of lead from spent lead-acid batteries and the preparation of lead oxide for use in new lead-acid batteries |
| US10062933B2 (en) | 2015-12-14 | 2018-08-28 | Johnson Controls Technology Company | Hydrometallurgical electrowinning of lead from spent lead-acid batteries |
| CN106086410A (en) * | 2016-08-10 | 2016-11-09 | 王凯 | A kind of indium extracts indium, zinc separation and recovery method in displaced liquid |
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