CN108946795A - A method of utilizing leaded dedusting ash high purity basic lead carbonate - Google Patents
A method of utilizing leaded dedusting ash high purity basic lead carbonate Download PDFInfo
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- CN108946795A CN108946795A CN201811121046.3A CN201811121046A CN108946795A CN 108946795 A CN108946795 A CN 108946795A CN 201811121046 A CN201811121046 A CN 201811121046A CN 108946795 A CN108946795 A CN 108946795A
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- Prior art keywords
- lead
- chloride
- filter residue
- dedusting ash
- drying
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/14—Carbonates
Abstract
The present invention provides a kind of methods using leaded dedusting ash high purity basic lead carbonate to collect filter residue after stirring, filtering in leaded dedusting ash vitriolization solution；Then the filter residue being collected into is leached with sodium chloride and calcium chloride mixed solution, obtains thick lead chloride；Obtained thick lead chloride is refined again, obtains the purification lead chloride of high-purity；Finally obtained purification lead chloride is dissolved in sodium carbonate liquor and is converted to obtain basic lead carbonate, obtains basic lead carbonate finished product after drying.Compared with existing technology, it is that raw material produces high-purity alkali type ceruse product that the present invention, which can use leaded dedusting ash, performance meets chemical industry standard " basic lead carbonate " HG/T 4835-2015, utilizes and offers reference for the leaded solid wastes recycling such as lead skim (ash).Leaded dedusting ash comprehensive utilization of resources approach is expanded, its added value is improved.
Description
Technical field
The invention belongs to Metallurgical resources field of comprehensive utilization, and in particular to a kind of to utilize leaded dedusting ash high purity alkali formula
The method of ceruse.
Background technique
With the continuous rapid growth of China's economy, the consumption figure of lead also increases substantially.According to relevant information, China
It is the country that lead bullion consumption figure is most in the world, lead average consumption speedup is respectively 25.2% between 2006 to 2011 years, is much higher than
Global average level.Chinese lead bullion consumption figure is up to 400.5 ten thousand tons (account for world consumption total amount 41.8%), China's lead within 2011
Application mainly include lead-acid accumulator, lead material, metal and lead oxides etc..As China is stepped to medium-developed country
Into battery will increase lead demand with dry cell industry and other industrial departments, and China's zinc lead will further be stimulated to consume
The growth of demand.
Although China is a lead resource country abundant, reserves occupy second place of the world, and per capita ownership is relatively poor
It is weary.Lead is as resource products, in the future of resource increasingly reduction, in order to alleviate lead resource shortage bring pressure, increasing pair
The exploitation and utilization of lead secondary resource are imperative.
Basic lead carbonate (Pb3(CO3)2(OH)2) as pearlescent pigment be widely used in cosmetics containers, ornament materials,
The essence chemical industrial field such as various films, coating and ink, also serves as lead-acid battery electrode material.Therefore, Pb3(CO3)2
(OH)2Synthesis and application have received widespread attention.
Application No. is 200910241419.5 patents " a kind of technique for producing basic lead carbonate " to have invented one kind with fire
" the superfluous slag " that method refines bismuth is raw material, optimizes " blast furnace-solves lead bismuth alloy-pyro-refining " smelting process for production, so that
Bismuth metallurgical slag is handled and is utilized.Its technique includes: that (1) impregnates neutralization slag acquisition sodium hydroxide solution；(2) lead chloride is leached
Slag, filtering；(3) alkali neutralization, filtration washing；(4) carbonate conversion, crystallization, filtration washing.The basic carbonate produced through the technique
Lead products substitution yellow lead (lead oxide) is directly added into the circular electrolyte of electrolysis lead bismuth alloy, solves the problems, such as " poor lead ".And it produces
Product purity does not clearly state.
Application No. is 201710362048.0 patent " a kind of for purifying the device of ceruse in lead-containing compounds " hairs
Be illustrated it is a kind of in lead-containing compounds purify ceruse device, mainly include reaction kettle, solution circulating device, pedestal, in
Empty three-way pipeline and crystallization strainer etc..It is leached using dust technology, and using the technique of hydrogen peroxide, it is higher ultra-fine to can get purity
Ceruse crystallization.
Application No. is a kind of 201710005041.3 patent " recovery method as resource of the leaded zinc powder dirt of blast furnace " inventions
A kind of recovery method as resource of the leaded zinc powder dirt of blast furnace.Its technical process includes: that (1) mixes the leaded zinc powder dirt of blast furnace with carbon dust
It is placed in the vacuum reactor of condensing unit, the oxide of zinc is subjected to carbon reduction, under vacuum evaporation gasification, by cold
Solidifying device collects recycling；(2) by treated, dust carries out high-temperature calcination, addition nitric acid solution dissolves, addition sodium chloride reacts
Crystallization, addition sodium carbonate liquor are converted into ceruse, and heat resolve obtains lead oxide, and vacuum carbon reduction is recycled to obtain simple substance
Lead.
Through retrieving, at present with leaded dedusting ash, the secondary related patents technology for directly preparing basic lead carbonate containing lead resource
Considerably less, product purity, relevant criterion etc. do not explain.
Summary of the invention
The purpose of the present invention is to provide a kind of methods using leaded dedusting ash high purity basic lead carbonate, with sulfuric acid
Resulting leaded acid sludge is raw material after handling leaded dedusting ash, prepares basic lead carbonate using wet processing, expands leaded dedusting
Grey comprehensive utilization of resources approach, improves its added value.Moreover, present invention process is simple, cleanliness without any pollution, product index meets state
Whole index requests in family chemical industry standard " basic lead carbonate " HG/T 4835-2015.
Specific technical solution of the present invention is as follows:
A method of utilizing leaded dedusting ash high purity basic lead carbonate, comprising the following steps:
1) leaded dedusting ash is mixed, heating stirring reaction, filtering with sulfuric acid solution, collects filter residue, filter residue drying；
2) filter residue after step 1) drying is added into the mixed solution of sodium chloride and calcium chloride, heating stirring reaction, instead
It is filtered while hot after answering, collects filtrate and be cooled to room temperature, filtered after to be precipitated, collect precipitating, precipitating obtains thick after drying
Lead chloride；
3) thick lead chloride prepared by step 2) is placed in sodium chloride solution, heating stirring dissolution filters while hot, collects filter
Liquid and filter residue, filter residue are washed with hot water, must wash filtrate, are merged with the filtrate of collection, crystallisation by cooling, filtering, obtained crystal
After being washed with water, drying obtains purification lead chloride；
4) the purification lead chloride of step 3) preparation is added into sodium carbonate liquor, then heating stirring reaction is filtered, collected
Precipitating is washed, and drying obtains high-purity alkali type ceruse.
The concentration of sulfuric acid solution is 150~230g/L in step 1), and the solid-to-liquid ratio of leaded dedusting ash and sulfuric acid solution is 1:2
~1:8g/mL；
Further, heating stirring reaction temperature described in step 1) is 30~70 DEG C, under the conditions of 200~600r/min
React 30~120min；
After step 1) reaction, filter residue main component is lead sulfate, and filtrate is according to its physicochemical property concrete application.
The additive amount of calcium chloride is 0.6~2.0 times of the filter residue quality after 1) drying, sodium chloride and calcium chloride in step 2)
Mixed solution in calcium chloride concentration be 20~120g/L；Sodium chloride concentration is 160~260g/L.
Further, the mixed solution solid-liquid of the filter residue in step 2) after step 1) used drying and sodium chloride and calcium chloride
Than for 1:4~1:14g/mL；
Under the conditions of the reaction of heating stirring described in step 2) refers to 50~100 DEG C, stirring rate is 100~400r/min,
React 2~6h.In this step, 50~100 DEG C of temperature are to guarantee sodium chloride and calcium chloride mixed solution to institute in step 1
The leaching rate of lead in filter residue, the leaching rate of lead can reach 85% or more within this temperature range.
Step 3) refines thick lead chloride, uses to heat the molten mode of weight and remove impurity in thick lead chloride simultaneously
The recovery rate for guaranteeing lead chloride " is washed " with hot water herein and refers to that the filter residue after filtering is washed with hot water, it is ensured that lead chloride is molten
The recovery rate of liquid.
Concentration of sodium chloride solution described in step 3) is 160~260g/L；The solid-to-liquid ratio of thick lead chloride and sodium chloride solution
Are as follows: 1:10~1:25g/mL.
20~80min of stirring and dissolving under the conditions of the dissolution of heating stirring described in step 3) refers to 50~100 DEG C；
It is washed described in step 3) with hot water and refers to and washed 3 times or more with temperature >=80 DEG C hot water.
Sodium carbonate molar ratio in the purification lead chloride and sodium carbonate liquor of the preparation of step 3) described in step 4) is 1:
1.01~1:1.50.
Further, the purification lead chloride of the preparation of step 3) described in step 4) and the solid-to-liquid ratio of sodium carbonate liquor are 1:5
~1:20g/mL.
The reaction of heating stirring described in step 4) refers to that under the conditions of 50~100 DEG C, revolving speed is 100~400r/min stirring
Under the conditions of 30~180min of isothermal reaction.
The high-purity ceruse performance indicator prepared in step 4) reaches chemical industry " basic lead carbonate " (HG/T4835-
2015) standard requirements.
The present invention is by leaded dedusting ash vitriolization solution, and (main component is sulphur to collection filter residue after stirring, filtering
Lead plumbate)；Then the filter residue being collected into is leached with sodium chloride and calcium chloride mixed solution, obtains thick lead chloride；Again to
To thick lead chloride refined, obtain the purification lead chloride of high-purity；Obtained purification lead chloride is finally dissolved in sodium carbonate
It is converted to obtain basic lead carbonate in solution, obtains basic lead carbonate finished product after drying.
The present invention leaches the leaded dedusting ash filter residue of sulfuric acid-treated mistake with sodium chloride and calcium chloride mixed solution, not only lead
Leaching rate it is high, and leachate can also reuse, save the cost.Compared with existing " rich lead method " handles lead skim, this hair
Bright to can use leaded dedusting ash as raw material production high-purity alkali type ceruse product, performance meets chemical industry standard " alkali formula carbon
Lead plumbate " HG/T 4835-2015, it utilizes and offers reference for the leaded solid wastes recycling such as lead skim (ash).Expand leaded dedusting ash resource
Comprehensive Utilization Ways improve its added value.
Detailed description of the invention
Fig. 1 is the method for the present invention flow diagram.
Specific embodiment
The present invention is further illustrated below by embodiment:
Embodiment 1
A method of utilizing leaded dedusting ash high purity basic lead carbonate, comprising the following steps:
1), used its main component of leaded dedusting ash and particle diameter distribution take the leaded dedusting of 200g as shown in table 1, table 2
Ash is added in the sulfuric acid solution of 700mL concentration 150g/L, is heated to 65 DEG C of heat preservations, and under the conditions of stirring switchs to 300r/min
It is stirred to react 30min, after complete reaction, is filtered, collects filtrate and filter residue respectively, 110 DEG C of filter residue are dried, is changed
Constituent analysis is learned, testing result is as shown in table 3；
2), compound concentration is the sodium chloride solution 200mL of 180g/L, and 12g work is added into prepared sodium chloride solution
Industry calcium chloride is configured to sodium chloride and calcium chloride mixed solution, and prepared mixed solution is placed in 60 DEG C of waters bath with thermostatic control,
Filter residue after taking 20g step 1) to dry is slowly added in above-mentioned sodium chloride and calcium chloride mixed solution, using magnetic agitation
Then device is filtered while hot until the reaction is complete with 300r/min speed stirring 4h, collect filtrate and be cooled to room temperature, after to be precipitated
Filtering collects precipitating and obtains thick lead chloride after drying；
3), the thick lead chloride of the resulting 20g of step 2) is added in the sodium chloride solution that 200mL concentration is 180g/L, is placed in
It after being heated to 60 DEG C of constant temperature stirring and dissolving 30min in thermostat water bath, is filtered while hot with Buchner funnel, collects filtrate, filter
Slag is washed 4 times with 90 DEG C of hot water, must wash filtrate, the filtrate of aforementioned collection and 4 washing filtrates is merged, crystallisation by cooling, mistake
Filter after obtained crystal is washed with water 3 times, is dried in 110 DEG C, obtains purification lead chloride.
4) the sodium carbonate liquor 200mL for, taking prepared 50g/L, after placing it in 60 DEG C of water bath with thermostatic control constant temperature 10min,
It is slowly added to the purification lead chloride 18g of step 3) preparation, isothermal reaction under the conditions of revolving speed is 200r/min magnetic agitation
60min, filtering, is precipitated, and washs precipitating with clear water until the chloride ion in precipitating completely removes, then 110 DEG C dry, and obtain
Basic lead carbonate product, performance indicator is as shown in table 4, reaches chemical industry " basic lead carbonate " (HG/T 4835-2015) mark
Alignment request.
The leaded dedusting ash main chemical compositions of table 1, wt%
| ZnO | Zn | Cu | Fe | Pb | S | Ag | SiO2 |
| 38.03 | 30.52 | <0.005 | 12.68 | 7.92 | 2.06 | <0.005 | 1.29 |
The leaded dedusting ash granularmetric analysis of table 2
| Granule size/mesh | > 80 | 80~120 | 120~150 | 150~200 | < 200 |
| Particle size content/% | 3.31 | 3.20 | 3.81 | 12.11 | 77.57 |
3 filter residue main chemical compositions of table, wt%
| Project | Pb | Fe | Zn | Cu | As |
| Filter residue | 42.23 | 19.41 | 1.48 | - | - |
4 basic lead carbonate product performance index detection data of table
The high-purity alkali type ceruse product of the method for the present invention production, performance meet chemical industry standard " basic lead carbonate "
HG/T 4835-2015。
Claims (10)
1. a kind of method using leaded dedusting ash high purity basic lead carbonate, which is characterized in that the method includes following
Step:
1) leaded dedusting ash is mixed, heating stirring reaction, filtering with sulfuric acid solution, collects filter residue, filter residue drying；
2) filter residue after step 1) drying is added into the mixed solution of sodium chloride and calcium chloride, heating stirring reaction, reaction knot
It is filtered while hot after beam, collects filtrate and be cooled to room temperature, filtered after to be precipitated, collect precipitating, precipitating obtains thick chlorination after drying
Lead；
3) by step 2) prepare thick lead chloride be placed in sodium chloride solution, heating stirring dissolution, filter while hot, collect filtrate and
Filter residue, filter residue are washed with hot water, must wash filtrate, are merged with the filtrate of collection, crystallisation by cooling, filtering, obtained crystal water
After washing, drying obtains purification lead chloride；
4) the purification lead chloride of step 3) preparation is added into sodium carbonate liquor, then heating stirring reaction is filtered, it is heavy to collect
It forms sediment, washs, drying obtains high-purity alkali type ceruse.
2. the method according to claim 1, wherein in step 1) sulfuric acid solution concentration be 150~230g/L,
Leaded dedusting ash and the solid-to-liquid ratio of sulfuric acid solution are 1:2~1:8g/mL.
3. method according to claim 1 or 2, which is characterized in that heating stirring reaction temperature described in step 1) is 30
~70 DEG C, 30~120min is reacted under the conditions of 200~600r/min.
4. the method according to claim 1, wherein the additive amount of calcium chloride is the filter after 1) drying in step 2)
Calcium chloride concentration is 20~120g/L in the mixed solution of 0.6~2.0 times of slag amount, sodium chloride and calcium chloride；Sodium chloride is dense
Degree is 160~260g/L.
5. method according to claim 1 or 4, which is characterized in that filter residue in step 2) after step 1) used drying and
The mixed solution solid-to-liquid ratio of sodium chloride and calcium chloride is 1:4~1:14g/mL.
6. method according to claim 1 or 4, which is characterized in that the reaction of heating stirring described in step 2) refers to 50~
Under the conditions of 100 DEG C, stirring rate is 100~400r/min, reacts 2~6h.
7. the method according to claim 1, wherein the dissolution of heating stirring described in step 3) refers to 50~100
20~80min of stirring and dissolving under the conditions of DEG C.
8. the method according to claim 1, wherein step 3) described in step 4) preparation purification lead chloride with
Sodium carbonate molar ratio in sodium carbonate liquor is 1:1.01~1:1.50.
9. method according to claim 1 or 8, which is characterized in that the purification chlorination of the preparation of step 3) described in step 4)
The solid-to-liquid ratio of lead and sodium carbonate liquor is 1:5~1:20g/mL.
10. method according to claim 1 or 8, which is characterized in that the reaction of heating stirring described in step 4) refers to 50
Under the conditions of~100 DEG C, revolving speed is 30~180min of isothermal reaction under 100~400r/min stirring condition.
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Cited By (2)
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| CN110923468A (en) * | 2019-12-02 | 2020-03-27 | 赵坤 | Method for recovering metallic lead from lead-containing materials such as lead sulfate slag |
| CN111939954A (en) * | 2019-05-16 | 2020-11-17 | 天津大学 | Basic lead carbonate nanosheet, preparation method thereof and application of nanosheet in electrocatalysis of carbon dioxide hydrogenation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111939954A (en) * | 2019-05-16 | 2020-11-17 | 天津大学 | Basic lead carbonate nanosheet, preparation method thereof and application of nanosheet in electrocatalysis of carbon dioxide hydrogenation |
| CN111939954B (en) * | 2019-05-16 | 2022-09-13 | 天津大学 | Basic lead carbonate nanosheet, preparation method thereof and application of nanosheet in electrocatalysis of carbon dioxide hydrogenation |
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