CN105967211A - Method for preparing potassium sulfate from brine - Google Patents
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- CN105967211A CN105967211A CN201610296061.6A CN201610296061A CN105967211A CN 105967211 A CN105967211 A CN 105967211A CN 201610296061 A CN201610296061 A CN 201610296061A CN 105967211 A CN105967211 A CN 105967211A
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- borofluoride
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- quaternary ammonium
- potassium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/063—Tetrafluoboric acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/063—Tetrafluoboric acid; Salts thereof
- C01B35/066—Alkali metal tetrafluoborates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a method for preparing potassium sulfate from brine. The method comprises that a borofluoride is added into brine, the mixture undergoes a reaction at the room temperature, the reaction product is filtered so that potassium borofluoride solids are obtained, the filtrate is collected, the potassium borofluoride solids and concentrated sulfuric acid directly undergo a reaction to produce potassium sulfate solids and fluoroboric acid gas, water-soluble quaternary ammonium sulfate is added into the filtrate so that fluoborate ions in the filtrate are transformed into quaternary ammonium cationic borofluoride, the quaternary ammonium cationic borofluoride further reacts with concentrated sulfuric acid to produce fluoroboric acid gas and a water-soluble quaternary ammonium sulfate solution to be recovered, the fluoroboric acid gas obtained by the two steps are respectively absorbed by an absorbent so that the fluoroboric acid gas is transformed into a borofluoride, the reaction solution is concentrated until saturation and the saturated reaction solution is recovered and then is used in a reaction of a borofluoride and brine. The method mainly comprises two steps, has a fast reaction rate and a high conversion rate, has a potassium ion recovery rate of 92% or more, produces a potassium sulfate product with purity of 97-99% and can be directly applied for crops.
Description
Technical field
The method that the present invention relates to prepare potassium sulfate in field of inorganic chemical engineering, particularly to a kind of with salt as raw material and the method for preparing potassium sulfate.
Background technology
Potassium sulfate is a kind of important potash fertilizer of high-quality without chlorine, has salt-soda soil index relatively low, and applicable crops scope is wide, is provided that the feature of sulfur trace element, can improve crop yield, moreover it is possible to improve crop quality.But China is the country that a potassium resource is relatively deficient, and a large amount of potash fertilizer are dependent on import.Therefore, the method utilizing easily acquisition raw material to prepare potassium sulfate at lower cost becomes the focus of current research.
Salt is from the strongest water of a kind of mineralising, including salt lake bittern, subsurface brine, sea salt salt etc., wherein contain a large amount of magnesium, sodium, chlorine, sulfur, potassium plasma, and other trace element such as bromine, boron, therefore use value is huge, and the salt content distribution of China is extensive: autonomous region of coastal provinces city output substantial amounts of sea salt salt；Xinjiang Lop Nur, a large amount of salt lake bittern of Cha Er Han Salt Lake output；The substantial amounts of subsurface brine of hinterland output.If above-mentioned a few class salt reasonably can be used, ample resources not only can be saved, moreover it is possible to have a tremendous social and economic benefits.
Potassium sulfate is prepared for raw material, it is necessary first to extracting potassium from salt, the existing technology extracting potassium from salt mainly includes following several: chemical precipitation method, ion exchange, evaporative crystallization method, extraction, and inverse flotation method with salt.Wherein chemical precipitation method is due to technical method comparative maturity and easily operated, the most conventional compared to other method.It is to add some chemical agent (precipitant) in salt that chemical precipitation method extracts the core of potassium, makes it and the potassium in salt occur direct chemical reaction to generate and is insoluble in the precipitate of water and separates out, thus reaches to extract the purpose of potassium.The most conventional precipitant has 2,4,6,2',4',6'-hexanitrodiphenylamine., perchlorate, Gypsum Fibrosum, sodium tetraphenylborate, phosphate etc..But, these conventional precipitant or poisonous and harmful own, otherwise higher to the requirement of reaction condition during expensive or precipitation, if 2,4,6,2',4',6'-hexanitrodiphenylamine. is a kind of explosive, poisonous organic solvent, health can be worked the mischief and jeopardize environment；Perchlorate[1]Expensive, precipitation process must be carried out under freezing, causes energy consumption relatively big, and perchlorate can be to environment；Gypsum Fibrosum and phosphate[2]The sedimentation method need to use substantial amounts of precipitant, cause production cost to be higher than value of the product；Sodium tetraphenylborate[3]It it is the common agents of analytical chemistry, for detection by quantitative potassium ion, rubidium ion, cesium ion, silver ion, sub-thallium ion and ammonium ion, white precipitate can be generated with these ions under cryogenic, but price is sufficiently expensive and not can be recycled, also can be to environment.
List of references:
[1] D.R.George,J.M.Ri1eyandJ.R.Ross[J].Chem.Eng.Progr.,
64(6), 96-99(1968).
[2] Maia G. Dunseth,
Arlington, Va., and Murrell L. Salutsky, etc. Mehtod of recovering potassium values from brines[P].
US3195978A, 1965-07-20.
[3] Buraian Ruisu, Sutefuan Eichi Angaa, Kaaru Jii
Anchi, Preparation of thiazole
derivative[p]. JPS5312858, 1978-02-04。
Summary of the invention
The problem existed for prior art, the present invention provides a kind of method preparing potassium sulfate for raw material with salt, with the water-soluble fluorine borate that is readily available as precipitant, use chemical precipitation method extract potassium from salt and prepare potassium sulfate, and the most repeatable recovery of water-soluble fluorine borate is in technical process.The inventive method technique is simple, and feed stock conversion is high, and precipitant toxicity is low, and due to raw-material accessibility, the boratory repeatable usability of water-soluble fluorine and the simplicity of processing step thus there is bigger economic worth.The technical scheme is that
A kind of method preparing potassium sulfate for raw material with salt, is included in salt addition borofluoride and at room temperature reacts, reacted and filtered out Potassium borofluoride solid, and retained filtrate；Potassium borofluoride solid and strong sulfuric acid response are directly obtained potassium sulfate solid and fluoboric acid gas.
In said method, potassium content >=10g/L in described salt.
In said method, described borofluoride is water-soluble fluorine borate, including Sodium fluoroborate, fluoboric acid calcium, ammonium fluoroborate or fluoboric acid magnesium；And the addition of borofluoride is in terms of 0.9 ~ 1.3:1 by the mol ratio of potassium ion in fluoro boron acid ion and salt.
In said method, described Potassium borofluoride solid with the condition of strong sulfuric acid response is: Potassium borofluoride is 1:0.5 ~ 0.6 with the mol ratio of concentrated sulphuric acid, and reaction temperature is 500 ~ 700 ° of C, and the response time is 30 ~ 120min.
In said method, it is additionally included in described filtrate addition water solublity quaternary ammonium sulfate, makes the fluoro boron acid ion in filtrate change into quaternary ammonium cation borofluoride；Quaternary ammonium cation borofluoride obtains the liquid to be recycled of fluoboric acid gas and water solublity quaternary ammonium sulfate further with strong sulfuric acid response；The fluoboric acid gas obtained by secondary in course of reaction again absorbs with absorbent respectively and is allowed to be converted into borofluoride, and reactant liquor is concentrated into saturated rear recovery to the course of reaction of borofluoride Yu salt.
Described water solublity quaternary ammonium sulfate includes sulphuric acid cetyl pyridinium, dodecyl trimethyl ammonium sulfate, cetyl trimethyl ammonium sulfate or octadecyl trimethyl ammonium sulfate, and the addition of quaternary ammonium salt is counted for 1:1 with quaternary ammonium salt ion with the mol ratio of fluoro boron acid ion in filtrate.
Described quaternary ammonium cation borofluoride with the condition of strong sulfuric acid response is: quaternary ammonium cation borofluoride is 2.4 ~ 1.5:1 with the mol ratio of concentrated sulphuric acid, reaction temperature is 50 ~ 90 ° of C, preferably 60 ~ 75 ° C, vacuum is-0.098 ~-0.08MP, and the response time is 0.5 ~ 2h.
The liquid to be recycled of described water solublity quaternary ammonium sulfate is concentrated into saturated rear recovery to water solublity quaternary ammonium sulfate and filtrate and reacts the course of reaction converting fluoro boron acid ion.
Described absorbent includes sodium carbonate, sodium bicarbonate, magnesium carbonate, magnesium oxide, calcium hydroxide, calcium carbonate, ammonia, ammonium bicarbonate soln, and the addition of absorbent is in terms of 0.9 ~ 1.1:1 by the mol ratio of absorbent cation Yu fluoro boron acid ion.
During the recycled of borofluoride or water solublity quaternary ammonium sulfate, if the amount of the borofluoride reclaimed or water solublity quaternary ammonium sulfate can not meet experiment demand, in the way of new borofluoride or water solublity quaternary ammonium sulfate can being added in the borofluoride using recovery or water solublity quaternary ammonium sulfate.
The present invention compared with prior art, has the beneficial effect that
The present invention is with containing potassium salt and easily the obtaining of potassium content >=10g/L, hypotoxic water-soluble fluorine borate as initial feed, Potassium borofluoride solid is obtained by chemical precipitation method, Potassium borofluoride solid obtains potassium sulfate solid again with strong sulfuric acid response, dominant response process is two steps, being swift in response and conversion ratio is high, the potassium ion response rate can reach more than 92%；Extract the filtrate after potassium element and pass sequentially through quaternary ammonium salt and absorbent to extract fluoboric acid and then to generate water-soluble fluorine borate, repeatable recycled is to technical process, and the potassium ion response rate still can reach about 80%, and the most repeatable recycled of water solublity quaternary ammonium sulfate generated during reclaiming borofluoride is to borofluoride removal process, the present invention reduces the pollution to environment while reducing cost savings resource as far as possible, has bigger industrial value.Additionally, the purity of potassium product prepared by the present invention is 97 ~ 99%, it is not necessary to being further purified, applicable crops are directly used.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
The salt containing potassium that the present invention implements to use takes from saltern, Shandong, and concentration is 30 Baume degrees, and density is 1.26g/ml, and its main component is as shown in table 1.
Table 1 extracts potassium salt leading ion component list
| Ionic species | Mg2+ | Na+ | K+ | Cl- | SO4 2- |
| Content g/L | 56.2 | 42.2 | 13.7 | 187.7 | 63.4 |
Embodiment 1
The method preparing potassium sulfate for raw material with salt, process chart, as it is shown in figure 1, take salt 1.5L described in table 1, adds saturated Sodium fluoroborate solution, and the mole of Sodium fluoroborate is 0.476mol, after being stirred at room temperature reaction 20min, filters out precipitation, retains filtrate；105 ° of C will be deposited in dry, and weigh, 52.73gKBF can be obtained4Solid, by KBF4Solid mixes with the concentrated sulphuric acid that 21.25g mass fraction is 98.3%, it is heated to 700 ° of C, and collect fluoboric acid gas with the suspension containing 27.0g sodium bicarbonate, after 50min, stopped reaction, it is 37.16g that 105 ° of C weigh potassium sulfate solid masses after drying, and purity is 98.2%, and the potassium ion response rate is 79.5%.
To extracting, the filtrate of gained adds after potassium the sulphuric acid cetyl pyridinium solution containing 0.0286mol, it is immediately generated cetyl pyridinium borofluoride precipitation, filter out precipitation, 60 ° of C are dried, cetyl pyridinium borofluoride precipitation is reacted under conditions of 60 ° of C and vacuum are-0.096MP with concentrated sulphuric acid, and absorb fluoboric acid gas with the suspension of above-mentioned sodium bicarbonate, filter out sulphuric acid cetyl pyridinium solid after 30min and dry in 60 ° of C, the sulphuric acid cetyl pyridinium response rate is 98.3%, constant volume absorbing liquid, chemical examination fluoboric acid total ion concentration is 0.467mol, illustrate that the Sodium fluoroborate response rate reaches 98.1%.
Sodium bicarbonate suspension absorbs fluoboric acid gas and is converted into Sodium fluoroborate, is concentrated into saturated recovery and obtains Sodium fluoroborate.
Embodiment 2
The method preparing potassium sulfate for raw material with salt, process chart is as it is shown in figure 1, take salt 1.5L described in table 1, adding the saturated Sodium fluoroborate solution that embodiment 1 reclaims, the mole of Sodium fluoroborate is 0.467mol, after being stirred at room temperature reaction 20min, filter out precipitation, retain filtrate；105 ° of C will be deposited in dry, and weigh, 51.78gKBF can be obtained4Solid, by KBF4Solid mixes with the concentrated sulphuric acid that 21.05g mass fraction is 98.3%, it is heated to 700 ° of C, and collect fluoboric acid gas with the suspension containing 25.0g sodium bicarbonate, after 50min, stopped reaction, it is 36.45g that 105 ° of C weigh potassium sulfate solid masses after drying, and purity is 98.3%, and the potassium ion response rate is 78.1%.
To extracting, the filtrate of gained adds after potassium the solution containing 0.0282mol sulphuric acid cetyl pyridinium that embodiment 1 reclaims, it is immediately generated cetyl pyridinium borofluoride precipitation, filter out precipitation, 60 ° of C are dried, cetyl pyridinium borofluoride precipitation is reacted under conditions of 60 ° of C and vacuum are-0.096MP with concentrated sulphuric acid, and absorb fluoboric acid gas with the suspension of above-mentioned sodium bicarbonate, filter out sulphuric acid cetyl pyridinium solid after 30min and dry in 60 ° of C, the sulphuric acid cetyl pyridinium response rate is 98.2%, constant volume absorbing liquid, chemical examination fluoboric acid total ion concentration is 0.459mol, illustrate that the Sodium fluoroborate response rate reaches 98.3%.
Sodium bicarbonate suspension absorbs fluoboric acid gas and is converted into Sodium fluoroborate, is concentrated into saturated recovery and obtains Sodium fluoroborate.
Embodiment 3
The method preparing potassium sulfate for raw material with salt, process chart, as it is shown in figure 1, take salt 1L described in table 1, adds saturated ammonium fluoroborate solution, and ammonium fluoroborate mole is 0.380mol, after being stirred at room temperature reaction 20min, filters out precipitation, retains filtrate；105 ° of C will be deposited in dry, and weigh, 39.54gKBF can be obtained4Solid, by KBF4Solid mixes with the concentrated sulphuric acid that 15.94g mass fraction is 98.3%, it is heated to 600 ° of C, and collect fluoboric acid gas with the solution containing 30.0g ammonium hydrogen carbonate, after 90min, stopped reaction, it is 28.15g that 105 ° of C weigh potassium sulfate solid masses after drying, and purity is 97.2%, and the potassium ion response rate is 89.4%.
To extracting, the filtrate of gained adds after potassium dodecyl trimethyl ammonium sulfate solution, it is immediately generated trimethyl ammonium fluoroborate precipitation, filter out precipitation, 70 ° of C are dried, trimethyl borofluoride precipitation is reacted under conditions of 65 ° of C and vacuum are-0.095MP with concentrated sulphuric acid, and absorb fluoboric acid gas with the solution of above-mentioned ammonium hydrogen carbonate, filter out dodecyl trimethyl ammonium sulfate solid after 30min and dry in 65 ° of C, the dodecyl trimethyl ammonium sulfate response rate is 94.0%, constant volume absorbing liquid, chemical examination fluoboric acid total ion concentration is 0.372mol, illustrate that the ammonium fluoroborate response rate is 97.9%.
Ammonium bicarbonate soln absorbs fluoboric acid gas and is converted into ammonium fluoroborate, is concentrated into saturated recovery and obtains ammonium fluoroborate.
Embodiment 4
The method preparing potassium sulfate for raw material with salt, process chart, as it is shown in figure 1, take salt 1L described in table 1, adds saturated fluoboric acid magnesium solution, and fluoboric acid magnesium mole is 0.231mol, after being stirred at room temperature reaction 20min, filters out precipitation, retains filtrate；105 ° of C will be deposited in dry, and weigh, 40.88gKBF can be obtained4Solid, by KBF4Solid is that 98.3% concentrated sulphuric acid mixes with 17.10g mass fraction, is heated to 650 ° of C, and collects fluoboric acid gas with the suspension containing 19.40g magnesium carbonate, after 60min, stopped reaction, it is 29.07g that 105 ° of C weigh potassium sulfate solid masses after drying, purity is 97.3%, and the potassium ion response rate is 92.4%.
To extracting, the filtrate of gained adds after potassium octadecyl trimethyl ammonium sulfate, it is immediately generated octadecyl trimethyl ammonium fluoroborate precipitation, filter out precipitation, 75 ° of C are dried, octadecyl trimethyl ammonium fluoroborate precipitation is reacted under conditions of 70 ° of C and vacuum are-0.092MP with concentrated sulphuric acid, and absorb fluoboric acid gas with the suspension of above-mentioned magnesium carbonate, filter out octadecyl trimethyl ammonium sulfate solids after 30min and dry in 75 ° of C, the octadecyl trimethyl ammonium sulfate response rate is 98.9%, constant volume absorbing liquid, chemical examination fluoboric acid total ion concentration is 0.455mol, illustrate that the fluoboric acid magnesium response rate is 98.5%.
Magnesium carbonate suspension absorbs fluoboric acid gas and is converted into fluoboric acid magnesium, is concentrated into saturated recovery and obtains fluoboric acid magnesium.
Embodiment 5
The method preparing potassium sulfate for raw material with salt, process chart, as it is shown in figure 1, take salt 1L described in table 1, adds saturated fluoboric acid calcium solution, and fluoboric acid calcium mole is 0.210mol, after being stirred at room temperature reaction 20min, filters out precipitation, retains filtrate；105 ° of C will be deposited in dry, and weigh, 40.27gKBF can be obtained4Solid, by KBF4Solid is that 98.3% concentrated sulphuric acid mixes with 16.71g mass fraction, it is heated to 500 ° of C, and collect fluoboric acid gas with the suspension containing 16.0g calcium hydroxide, after 60min, stopped reaction, it is 28.73g that 105 ° of C weigh potassium sulfate solid masses after drying, and purity is 97.0%, and the potassium ion response rate is 91.1%.
To extracting, the filtrate of gained adds after potassium cetyl trimethyl ammonium sulfate, it is immediately generated cetyl trimethyl ammonium fluoroborate precipitation, filter out precipitation, 75 ° of C are dried, cetyl trimethyl ammonium fluoroborate precipitation is reacted under conditions of 75 ° of C and vacuum are-0.088MP with concentrated sulphuric acid, and absorb fluoboric acid gas with the suspension of above-mentioned calcium hydroxide, filter out cetyl trimethyl ammonium sulfate solids after 30min and dry in 75 ° of C, the cetyl trimethyl ammonium sulfate response rate is 98.9%, constant volume absorbing liquid, chemical examination fluoboric acid total ion concentration is 0.415mol, illustrate that the fluoboric acid calcium response rate is 98.8%.
Calcium hydroxide suspension absorbs fluoboric acid gas and is converted into fluoboric acid calcium, is concentrated into saturated recovery and obtains fluoboric acid calcium.
Claims (9)
1. the method preparing potassium sulfate for raw material with salt, it is characterised in that be included in salt addition borofluoride and at room temperature react, reacted and filtered out Potassium borofluoride solid, and retained filtrate；Potassium borofluoride solid and strong sulfuric acid response are directly obtained potassium sulfate solid and fluoboric acid gas.
A kind of method preparing potassium sulfate for raw material with salt the most according to claim 1, it is characterised in that potassium content >=10g/L in described salt.
A kind of method preparing potassium sulfate for raw material with salt the most according to claim 1, it is characterised in that described borofluoride is water-soluble fluorine borate, including Sodium fluoroborate, fluoboric acid calcium, ammonium fluoroborate or fluoboric acid magnesium；And the addition of borofluoride is in terms of 0.9 ~ 1.3:1 by the mol ratio of potassium ion in fluoro boron acid ion and salt.
A kind of method preparing potassium sulfate for raw material with salt the most according to claim 1, it is characterized in that described Potassium borofluoride solid with the condition of strong sulfuric acid response is: Potassium borofluoride is 1:0.5 ~ 0.6 with the mol ratio of concentrated sulphuric acid, reaction temperature is 500 ~ 700 ° of C, and the response time is 30 ~ 120min.
A kind of method preparing potassium sulfate for raw material with salt the most according to claim 1, it is characterised in that described method is additionally included in described filtrate addition water solublity quaternary ammonium sulfate, makes the fluoro boron acid ion in filtrate change into quaternary ammonium cation borofluoride；Quaternary ammonium cation borofluoride obtains the liquid to be recycled of fluoboric acid gas and water solublity quaternary ammonium sulfate further with strong sulfuric acid response；The fluoboric acid gas obtained by secondary in course of reaction again absorbs with absorbent respectively and is allowed to be converted into borofluoride, and reactant liquor is concentrated into saturated rear recovery to the course of reaction of borofluoride Yu salt.
A kind of method preparing potassium sulfate for raw material with salt the most according to claim 5, it is characterized in that described water solublity quaternary ammonium sulfate includes sulphuric acid cetyl pyridinium, dodecyl trimethyl ammonium sulfate, cetyl trimethyl ammonium sulfate or octadecyl trimethyl ammonium sulfate, and the addition of quaternary ammonium salt is counted for 1:1 with the mol ratio of fluoro boron acid ion in filtrate with quaternary ammonium salt ion.
A kind of method preparing potassium sulfate for raw material with salt the most according to claim 5, it is characterized in that described quaternary ammonium cation borofluoride with the condition of strong sulfuric acid response is: quaternary ammonium cation borofluoride is 2.4 ~ 1.5:1 with the mol ratio of concentrated sulphuric acid, reaction temperature is 50 ~ 90 ° of C, preferably 60 ~ 75 ° C, vacuum is-0.098 ~-0.08MP, and the response time is 0.5 ~ 2h.
A kind of method preparing potassium sulfate for raw material with salt the most according to claim 5, it is characterised in that the liquid to be recycled of described water solublity quaternary ammonium sulfate is concentrated into saturated rear recovery to water solublity quaternary ammonium sulfate and filtrate and reacts the course of reaction converting fluoro boron acid ion.
A kind of method preparing potassium sulfate for raw material with salt the most according to claim 5, it is characterized in that described absorbent includes sodium carbonate, sodium bicarbonate, magnesium carbonate, magnesium oxide, calcium hydroxide, calcium carbonate, ammonia, ammonium bicarbonate soln, the addition of absorbent is in terms of 0.9 ~ 1.1:1 by the mol ratio of absorbent cation Yu fluoro boron acid ion.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113215406A (en) * | 2021-04-30 | 2021-08-06 | 江西龙天勇有色金属有限公司 | Improved process method for extracting high-purity palladium from silver-copper-containing industrial waste in one step |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113215406A (en) * | 2021-04-30 | 2021-08-06 | 江西龙天勇有色金属有限公司 | Improved process method for extracting high-purity palladium from silver-copper-containing industrial waste in one step |
| CN113215406B (en) * | 2021-04-30 | 2022-08-09 | 江西龙天勇有色金属有限公司 | Improved process method for extracting high-purity palladium from silver-copper-containing industrial waste in one step |
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