CN114314637A - Method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid - Google Patents
Method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid Download PDFInfo
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Abstract
The invention belongs to the field of chemical industry and environmental protection, and particularly relates to a method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid. The method realizes the utilization of resources such as copper, sodium, ammonium, chlorine and the like in the acidic copper chloride etching waste liquid, has high product quality, high utilization rate of the process, energy conservation, environmental protection and easy industrialization.
Description
Technical Field
The invention belongs to the fields of chemical industry and environmental protection, and particularly relates to a method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid.
Background
The circuit board etching solution is divided into an acidic etching solution and an alkaline etching solution. With the increasingly strict requirements on safety and environmental protection, the influence of cost control and the factors for the innovation of the etching process, the specific gravity of the acidic etching solution is steadily increased, so that the proportion of the acidic copper chloride etching waste solution generated in the PCB industry is gradually increased, and the problems of high production cost, low product added value, secondary pollution and the like generally exist in the conventional treatment technology, so that the novel requirements cannot be met.
In order to solve the problems, the Chinese patent with the publication number of CN106587105B discloses a method for recovering copper chloride acidic etching waste liquid in a printed circuit board, and the key points of the technical scheme are as follows: adding sodium chloride into the waste liquid, distilling to obtain hydrochloric acid, crystallizing to obtain sodium chloride, and finally electrolyzing to obtain elemental copper. The patent has the following disadvantages: the concentration of the byproduct hydrochloric acid is not high, and the application range is small; secondly, the sodium chloride product contains various impurities such as heavy metal, ammonium and the like, is qualified as dangerous waste, and has the risk of secondary pollution; and thirdly, the impurity removal process is lacked in the preparation process of the simple substance copper, so that the quality of the simple substance copper is not high.
In addition, chinese patent No. CN112593233B also discloses a method for recovering copper chloride acidic etching waste liquid in printed circuit boards, which has the key points of the technical scheme: mixing basic etching waste liquid and acidic etching waste liquid to react to obtain basic copper chloride, adding into sulfuric acid to obtain copper sulfate, and adding into agent to obtain NH in mother liquid4 +Recovered as magnesium ammonium phosphate precipitate. The process also has a number of disadvantages: firstly, the preparation process of the copper sulfate is lack of impurity removal process, so that the product quality of the copper sulfate is difficult to ensure; secondly, the wastewater treatment cost is high; ③ residual NH in mother liquor4 +High, the subsequent waste water still needs further treatment.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid, so that the high-purity copper sulfate is obtained, and the full recycling of all components in the waste liquid is realized.
The technical purpose of the invention is realized by the following technical scheme, and the method for preparing the high-purity copper sulfate from the acidic copper chloride etching waste liquid comprises the following steps:
(1) providing a first acidic copper chloride etching solution, introducing liquid ammonia into the first acidic copper chloride etching solution for reaction and filtering to obtain a copper-containing refined solution;
(2) providing a second acidic copper chloride etching solution, and adjusting the pH value of the second acidic copper chloride etching solution to 0-2.5 by using the liquid ammonia to obtain an acid-adjusted second acidic copper chloride etching solution;
(3) reacting the copper-containing refined solution and the acid-adjusted second acidic copper chloride etching solution serving as raw materials, controlling a crystallization process to obtain basic copper chloride, and filtering the basic copper chloride;
(4) washing the basic copper chloride, and carrying out solid-liquid separation treatment on the basic copper chloride to obtain washed basic copper chloride;
(5) adding the washed basic copper chloride into a sulfuric acid solution for reaction to obtain copper sulfate slurry and hydrochloric acid, adding water into the copper sulfate slurry, and performing cooling crystallization and solid-liquid separation to obtain a crude product of copper sulfate;
(6) and adding the first solution into the crude copper sulfate, heating for dissolving, controlling the temperature for filtering to obtain a first filtrate, cooling and crystallizing the first filtrate, and centrifuging to obtain the high-purity copper sulfate.
In one embodiment, the liquid ammonia is industrial grade and the content of the liquid ammonia is more than 99.0%.
In one embodiment, the pH value of the reaction endpoint of the first acidic copper chloride etching solution in the step (1) is 8.0-9.6.
In one embodiment, the temperature of the process for preparing the basic copper chloride in the step (3) is 10 ℃ to 100.0 ℃.
In one embodiment, the process for preparing the basic copper chloride in step (3) has a pH of 3.0 to 7.0.
In one embodiment, the washing of the basic copper chloride is divided into two times, and the amount of the washing water is 1.0-5.0 times of the mass of the basic copper chloride.
In one embodiment, the sulfuric acid solution is concentrated sulfuric acid or a mixture of sulfuric acid and copper sulfate, and the concentration of the sulfuric acid is 25.0% -98.0%.
In one embodiment, the mass ratio of the basic copper chloride to the high-concentration sulfuric acid (in terms of sulfuric acid content) is 0.75:1 to 1.4: 1.
In one embodiment, the first solution is water or copper sulfate mother liquor.
In one embodiment, the temperature-controlled filtration temperature of the crude copper sulfate in step (6) is 80.0-100.0 ℃.
The method for preparing high-purity copper sulfate from the acidic copper chloride etching waste liquid has the following beneficial effects:
firstly, liquid ammonia is used as a raw material, so that energy is saved, impurities are less and the cost is low; liquid ammonia is adopted in the step (1) and the step (2) to ensure that the patented process has no extra water evaporation; the purity of the liquid ammonia is high, and the introduction of impurities is reduced from the source;
secondly, the concentration of the byproduct hydrochloric acid is high, and the additional value is high; controlling the concentration of hydrochloric acid prepared by acid conversion to reach over 31.0% by using basic copper chloride, and meeting the requirements of industrial products;
thirdly, removing impurities and controlling the quality step by step, so that the quality of the copper sulfate product is high; pre-reacting in the step (1), controlling crystallization of the basic copper chloride in the step (3), carrying out acid conversion in the step (5) and crystallization in the step (6), and carrying out multi-step impurity removal and control, so that the prepared copper sulfate product has high quality.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a XRD plot of a copper sulfate product prepared in accordance with example 1 of the present invention;
FIG. 3 is a thermogravimetric analysis of the copper sulfate product prepared in example 1 of the present invention-atmosphere N2 (DSC);
FIG. 4 is a thermogravimetric analysis of the copper sulfate product prepared in example 1 of the present invention-N2 atmosphere (TG).
Detailed Description
The invention is described in detail below with reference to the figures and examples.
Referring to fig. 1, the method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid provided by the invention comprises the following steps:
(1) providing a first acidic copper chloride etching solution, introducing liquid ammonia into the first acidic copper chloride etching solution for reaction and filtering to obtain a copper-containing refined solution;
(2) providing a second acidic copper chloride etching solution, and adjusting the pH value of the second acidic copper chloride etching solution to 0-2.5 by using liquid ammonia to obtain the second acidic copper chloride etching solution after acid adjustment;
(3) reacting the copper-containing refined solution and the acid-adjusted second acidic copper chloride etching solution serving as raw materials, controlling the crystallization process to obtain basic copper chloride, and filtering the basic copper chloride;
specifically, the filtrate is subjected to copper extraction, impurity removal, evaporation concentration and salt separation crystallization to respectively obtain industrial ammonium chloride and industrial sodium chloride, wherein cold energy required by cooling the ammonium chloride and the sodium chloride is carried away by gasifying the liquid ammonia in the step (1);
(4) washing basic copper chloride, and carrying out solid-liquid separation treatment on the basic copper chloride to obtain washed basic copper chloride;
(5) adding the washed basic copper chloride into a sulfuric acid solution for reaction to obtain copper sulfate slurry and hydrochloric acid, adding water into the copper sulfate slurry, and performing cooling crystallization and solid-liquid separation to obtain a crude product of copper sulfate;
specifically, the crystallization mother liquor can replace part of sulfuric acid solution transferred by basic copper chloride acid, and can also be used as a stripping agent of the extraction copper loaded organic phase in the step (3);
(6) adding the first solution into the crude copper sulfate, heating for dissolving, controlling the temperature for filtering to obtain a first filtrate, cooling and crystallizing the first filtrate, and centrifuging to obtain the high-purity copper sulfate.
The method for preparing high-purity copper sulfate from the acidic copper chloride etching waste liquid has the following beneficial effects:
firstly, liquid ammonia is used as a raw material, so that energy is saved, impurities are less and the cost is low; liquid ammonia is adopted in the step (1) and the step (2) to ensure that the patented process has no extra water evaporation; the purity of the liquid ammonia is high, and the introduction of impurities is reduced from the source;
secondly, the concentration of the byproduct hydrochloric acid is high, and the additional value is high; controlling the concentration of hydrochloric acid prepared by acid conversion to reach over 31.0% by using basic copper chloride, and meeting the requirements of industrial products;
thirdly, removing impurities and controlling the quality step by step, so that the quality of the copper sulfate product is high; pre-reacting in the step (1), controlling crystallization of the basic copper chloride in the step (3), carrying out acid conversion in the step (5) and crystallization in the step (6), and carrying out multi-step impurity removal and control, so that the prepared copper sulfate product has high quality.
Preferably, the liquid ammonia is industrial grade, and the content of the liquid ammonia is more than 99.0%.
Preferably, the pH value of the reaction endpoint of the first acidic copper chloride etching solution in the step (1) is 8.0-9.6.
Preferably, the temperature of the process for preparing the basic copper chloride in the step (3) is 10-100.0 ℃.
Preferably, the pH value of the process for preparing the basic copper chloride in the step (3) is 3.0-7.0.
Preferably, the washing of the basic copper chloride is divided into two times, and the amount of the washing water is 1.0-5.0 times of the mass of the basic copper chloride.
The sulfuric acid solution is preferably concentrated sulfuric acid or a mixture of sulfuric acid and copper sulfate, and the concentration of the sulfuric acid is 25.0% -98.0%.
Preferably, the mass ratio of the basic copper chloride to the high-concentration sulfuric acid (in terms of sulfuric acid content) is 0.75:1 to 1.4: 1.
The first solution is preferably water or copper sulfate mother liquor.
Preferably, the temperature-controlled filtration temperature of the crude copper sulfate in the step (6) is 80.0-100.0 ℃.
The following are specific examples:
example 1
A typical acidic copper chloride etching waste liquid A of a certain circuit board factory is taken as a treatment object, and the main components of the acidic copper chloride etching waste liquid A are as follows: copper 10.06%, chlorine 21.88%, free hydrochloric acid7.46%, sodium 2.18%, iron 10.85 mg/kg-12.19 mg/kg of lead-115.19 mg/kg of calcium-1。
Reducing pressure of bottled liquid ammonia with the content of 99.8 percent by a pressure reducing valve, introducing the bottled liquid ammonia into 330.0ml of first acidic copper chloride etching liquid A by a conduit, closing the liquid ammonia pressure reducing valve when the pH value of the system is 9.1, continuously reacting for 5.0min, filtering, and collecting filtrate to obtain copper-containing refined liquid B;
regulating the free acid of 500.0ml of second acidic copper chloride etching solution C by using 99.8% bottled liquid ammonia, stopping introducing the liquid ammonia when the pH value of the system is reduced to 0.5, filtering, and collecting filtrate to obtain the second acidic copper chloride etching solution D after the acid is regulated;
adding the copper-containing refined solution B and the acid-adjusted second acidic copper chloride etching solution D serving as raw materials into a 1000.0ml four-neck flask with stirring in a counter-addition mode, controlling the pH to be 5.4 and the reaction temperature to be about 87.0 ℃, reacting for 10.0min after adding the materials, and filtering to obtain 176.7g of basic copper chloride containing 5.5% of water;
extracting copper from the filtrate by lIx984, removing impurities, evaporating for concentration, and separating salt for crystallization to obtain industrial ammonium chloride and industrial sodium chloride; wherein cold energy required by cooling ammonium chloride and sodium chloride is carried away by liquid ammonia gasification in the processes of pre-reaction and acidity adjustment;
washing the basic copper chloride twice by using 220.0g of clear water respectively to obtain 176.1g of basic copper chloride;
adding 176.1g of washed basic copper chloride into a sulfuric acid solution containing 290.0g of 70.0 percent sulfuric acid, and distilling during stirring to respectively obtain copper sulfate slurry and 97.5g of 31.0 percent hydrochloric acid; finally, 50.0ml of water is supplemented into the copper sulfate slurry after acid evaporation, and then the copper sulfate slurry is cooled, crystallized and filtered to prepare 398.2g of crude copper sulfate;
the crystallization mother liquor can replace part of sulfuric acid transferred by the basic copper chloride acid, and can also be used as a back extractant of the extraction copper loaded organic phase in the step (3);
adding a proper amount of water, heating to dissolve the crude copper sulfate, performing solid-liquid separation to obtain a first filtrate, cooling and crystallizing the first filtrate, and centrifuging to obtain 390.2g of high-purity copper sulfate.
Through detection, the main indexes of the copper sulfate product are as follows:
CuSO4·5H298.6% of O, no As detected, 5.3 mg/kg of Pb-1，Ca 10.0mg·kg-1，Fe 10.0mg·kg-1，Co 0.31mg·kg-1，Ni 2.7mg·kg-1，Zn 6.8mg·kg-1，Cl 15.0mg·kg-1。
Example 2
A typical acidic copper chloride etching waste liquid of a certain circuit board factory is taken as a treatment object, and the main components of the acidic copper chloride etching waste liquid are as follows: copper 10.18%, chlorine 21.08%, free hydrochloric acid 7.52%, sodium 1.55%, NH3-N 27.65mg·kg-1Iron 1.24 mg/kg-1Lead 4.16 mg/kg-11.62 mg/kg of calcium-1。
Decompressing bottled liquid ammonia with the content of 99.8 percent by a decompression valve, introducing the bottled liquid ammonia into 320.0ml of first acidic copper chloride etching liquid A by a guide pipe, closing the liquid ammonia decompression valve when the pH value of the system is 9.5, continuing to react for 35.0min, filtering, and collecting filtrate to obtain copper-containing refined liquid B;
still adopting bottled liquid ammonia with the content of 99.8 percent to adjust 650.0ml of free acid of the second acidic copper chloride etching solution B, stopping introducing the liquid ammonia when the pH value of the system is reduced to 2.0, filtering, and collecting filtrate to obtain a second acidic copper chloride etching solution D after acid adjustment;
adding the copper-containing refined solution B and the acid-adjusted second acidic copper chloride etching solution D serving as raw materials into a 1000.0ml four-neck flask with a stirrer in a feeding mode, controlling the pH to be 4.8 and the reaction temperature to be about 95.0 ℃, reacting for 10.0min after adding the materials, and filtering to obtain 182.7g of basic copper chloride containing 3.7% of water;
extracting copper from the filtrate by lIx984, removing impurities, evaporating for concentration, and separating salt for crystallization to obtain industrial ammonium chloride and industrial sodium chloride; carrying out back extraction on the extracted copper loaded organic phase by using a crystallization mother liquor obtained after acid conversion of basic copper chloride;
washing and filtering the basic copper chloride by 400.0g of water, washing once by 180.0g of clear water, and filtering to obtain 182.0g of basic copper chloride;
adding 182.0g of washed refined basic copper chloride into 602.0g of sulfuric acid stripping solution with the sulfuric acid content of 30.0%, and distilling while stirring to respectively obtain copper sulfate slurry and 97.0g of 31.0% hydrochloric acid; finally, supplementing 75.0ml of water into the copper sulfate slurry subjected to acid steaming, cooling, crystallizing and filtering to obtain 481.6g of crude copper sulfate;
adding a proper amount of water, heating to dissolve the crude copper sulfate, performing solid-liquid separation to obtain a first filtrate, cooling and crystallizing the first filtrate, and centrifuging to obtain 475.0g of high-purity copper sulfate.
Through detection, the main indexes of the copper sulfate product are as follows:
CuSO4·5H298.7% of O, no As detected, 4.0 mg/kg of Pb-1，Ca 6.5mg·kg-1，Fe 16.0mg·kg-1，Co 1.3mg·kg-1，Ni 2.6mg·kg-1，Zn 7.1mg·kg-1，Cl 16.0mg·kg-1。
Example 3
A typical acidic copper chloride etching waste liquid of a certain circuit board factory is taken as a treatment object, and the main components of the acidic copper chloride etching waste liquid are as follows: copper 10.31%, chlorine 21.85%, free hydrochloric acid 6.68%, sodium 2.48%, NH3-N0.44%, Fe 6.42mg kg-13.95 mg/kg of lead-115.42 mg/kg of calcium-1。
Reducing pressure of bottled liquid ammonia with the content of 99.8 percent by a pressure reducing valve, introducing the bottled liquid ammonia into 270.0ml of first acidic copper chloride etching liquid A by a guide pipe, closing the liquid ammonia pressure reducing valve when the pH value of the system is 9.5, continuing to react for 5.0min, filtering, and collecting filtrate to obtain copper-containing refined liquid B;
still adopting bottled liquid ammonia with the content of 99.8 percent to adjust the free acid of 550.0ml of second acidic copper chloride etching solution B, stopping introducing the liquid ammonia when the pH value of the system is reduced to 0.9, filtering, and collecting filtrate to obtain second acidic copper chloride etching solution D after acid adjustment;
the copper-containing refined solution B and the acid-adjusted second acidic copper chloride etching solution D are used as raw materials, the raw materials are added into a stirred 1000.0ml four-neck flask in a feeding mode, the pH value is controlled to be 3.3, the reaction temperature is controlled to be about 78.0 ℃, after the materials are added, the reaction lasts for 10.0min, and then filtration is carried out, thus obtaining 147.0g of basic copper chloride containing 7.5% of water.
Extracting copper from the filtrate by lIx984, removing impurities, evaporating for concentration, and separating salt for crystallization to obtain industrial ammonium chloride and industrial sodium chloride; wherein cold energy required by cooling ammonium chloride and sodium chloride is carried away by liquid ammonia gasification in the processes of pre-reaction and acidity adjustment;
washing basic copper chloride twice by using 120.0g of clear water respectively to obtain 146.2g of basic copper chloride;
adding 146.2g of washed basic copper chloride into a mixed solution containing 125.0g of concentrated sulfuric acid and 85.0g of crystallization mother liquor containing 26.0% of sulfuric acid and 2.3% of copper, and distilling during stirring to respectively obtain copper sulfate slurry and 70.5g of 31.0% hydrochloric acid; finally, 30.0ml of water is supplemented into the copper sulfate slurry after acid evaporation, and the crude copper sulfate of 327.8g is prepared after cooling crystallization and suction filtration;
adding a proper amount of copper sulfate mother liquor, heating to dissolve the crude copper sulfate, carrying out solid-liquid separation to obtain a first filtrate, cooling and crystallizing the first filtrate, and centrifuging to obtain 429.0g of high-purity copper sulfate.
Through detection, the main indexes of the copper sulfate product are as follows:
CuSO4·5H298.7% of O, no As detected, 2.6 mg/kg of Pb-1，Ca 10.0mg·kg-1，Fe 35mg·kg-1，Co 1.6mg·kg-1，Ni 2.3mg·kg-1，Zn 10.0mg·kg-1，Cl 10.5mg·kg-1。
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid is characterized by comprising the following steps of:
(1) providing a first acidic copper chloride etching solution, introducing liquid ammonia into the first acidic copper chloride etching solution for reaction and filtering to obtain a copper-containing refined solution;
(2) providing a second acidic copper chloride etching solution, and adjusting the pH value of the second acidic copper chloride etching solution to 0-2.5 by using the liquid ammonia to obtain an acid-adjusted second acidic copper chloride etching solution;
(3) reacting the copper-containing refined solution and the acid-adjusted second acidic copper chloride etching solution serving as raw materials, controlling a crystallization process to obtain basic copper chloride, and filtering the basic copper chloride;
(4) washing the basic copper chloride, and carrying out solid-liquid separation treatment on the basic copper chloride to obtain washed basic copper chloride;
(5) adding the washed basic copper chloride into a sulfuric acid solution for reaction to obtain copper sulfate slurry and hydrochloric acid, adding water into the copper sulfate slurry, and performing cooling crystallization and solid-liquid separation to obtain a crude product of copper sulfate;
(6) and adding the first solution into the crude copper sulfate, heating for dissolving, controlling the temperature for filtering to obtain a first filtrate, cooling and crystallizing the first filtrate, and centrifuging to obtain the high-purity copper sulfate.
2. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein the liquid ammonia is industrial grade and the content of the liquid ammonia is more than 99.0%.
3. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein in the step (1), the pH value of the reaction endpoint of the first acidic copper chloride etching waste liquid is 8.0-9.6.
4. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein the temperature of the process for preparing the basic copper chloride in the step (3) is 10-100.0 ℃.
5. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein in the step (3), the pH value of the process for preparing the basic copper chloride is 3.0-7.0.
6. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein the washing of the basic copper chloride is divided into two times, and the amount of washing water is 1.0-5.0 times of the mass of the basic copper chloride.
7. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein the sulfuric acid solution is concentrated sulfuric acid or a mixture of sulfuric acid and copper sulfate, and the concentration of the sulfuric acid is 25.0% -98.0%.
8. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein the mass ratio of the basic copper chloride to the sulfuric acid solution (in terms of sulfuric acid content) is 0.75:1-1.4: 1.
9. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein the first solution is water or copper sulfate mother liquid.
10. The method for preparing high-purity copper sulfate from acidic copper chloride etching waste liquid as claimed in claim 1, wherein in the step (6), the temperature-controlled filtration temperature of the crude copper sulfate is 80.0-100.0 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115744964A (en) * | 2022-12-16 | 2023-03-07 | 江苏维达环保科技有限公司 | Novel production process of large-particle copper sulfate |
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