CN110228814B - Impurity removal method and impurity removal equipment applied to copper sulfate preparation process - Google Patents
Impurity removal method and impurity removal equipment applied to copper sulfate preparation process Download PDFInfo
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- CN110228814B CN110228814B CN201910663625.9A CN201910663625A CN110228814B CN 110228814 B CN110228814 B CN 110228814B CN 201910663625 A CN201910663625 A CN 201910663625A CN 110228814 B CN110228814 B CN 110228814B
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Abstract
The invention relates to an impurity removal method applied to a copper sulfate preparation process, which comprises the following steps: adding excessive dilute sulfuric acid solution and cuprous oxide into copper sulfate mother liquor containing chloride ions and ferrous ions to obtain a first solution; filtering to obtain a first filtrate; adding hydrogen peroxide and copper oxide to the first filtrate to obtain a second solution containing precipitates; filtering the second solution to obtain the high-purity copper sulfate product. The invention also provides impurity removal equipment applied to the copper sulfate preparation process; the invention finally obtains the high-purity copper sulfate product by twice precipitation, filtration and impurity removal, and can more thoroughly remove impurities such as chloride ions, ferrous ions and the like.
Description
Technical Field
The invention provides an impurity removal method and impurity removal equipment, and particularly relates to an impurity removal method and impurity removal equipment applied to a copper sulfate preparation process.
Background
At present, in the process of preparing copper sulfate by using a copper-containing etching solution, the final copper sulfate product contains impurities such as chloride ions, ferrous ions and the like, the two impurities affect the content and the performance of the copper sulfate, and the existing impurity removal methods cannot completely remove the impurities, so that high-purity copper sulfate cannot be obtained.
Therefore, it is necessary to invent an impurity removal method and an impurity removal device applied to the copper sulfate preparation process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an impurity removal method and an impurity removal device applied to the copper sulfate preparation process, which can more thoroughly remove impurities such as chloride ions, ferrous ions and the like to obtain high-purity copper sulfate.
The above object of the present invention is achieved by the following technical solutions:
the invention provides an impurity removal method applied to a copper sulfate preparation process, which comprises the following steps:
the method comprises the following steps: adding a dilute sulfuric acid solution and cuprous oxide into a copper sulfate mother liquor containing chloride ions and ferrous ions to obtain a first solution containing a precipitate;
step two: filtering the first solution containing the precipitate to obtain a first filtrate;
step three: adding hydrogen peroxide and copper oxide to the first filtrate to obtain a second solution containing precipitates;
step four: filtering the second solution containing the precipitate to obtain the high-purity copper sulfate product.
Further, in step one, when an excess of dilute sulfuric acid solution and cuprous oxide are added to the copper sulfate mother liquor, the addition is stopped until no new precipitate is produced.
Further, in the second step and the fourth step, a plurality of layers of filter screens are used for filtering in the filtering operation.
Further, in the third step, the reaction temperature is controlled to be 50-60 ℃, so that ferrous ions are completely oxidized into ferric ions, and the ferric ions are hydrolyzed to form ferric hydroxide precipitates.
The invention also provides impurity removing equipment applied to the copper sulfate preparation process, which comprises a first filtering device, a second filtering device and an impurity removing device;
the first filtering device and the second filtering device are respectively provided with a tank body, the upper end of the tank body is an inlet, the lower end of the tank body is an outlet, a coarse filtering layer frame body, a fine filtering layer frame body and an ultrafiltration layer frame body are sequentially arranged in the tank body from top to bottom, and the coarse filtering layer frame body, the fine filtering layer frame body and the ultrafiltration layer frame body can be transversely pulled out of the tank body from one side;
the impurity removing device comprises a reaction kettle, a rotating shaft is vertically arranged in the reaction kettle, a plurality of rotating blades are horizontally arranged at the bottom of the rotating shaft, a plurality of openings are formed in the lower surfaces of the rotating blades, and the rotating shaft is arranged in a hollow mode and communicated with the openings of the rotating blades;
wherein, the lower extreme outlet of first filter equipment is connected to the upper end of reation kettle, the lower extreme outlet of reation kettle is connected to the upper end of second filter equipment.
Furthermore, the filtering aperture of the coarse filtering layer frame body, the fine filtering layer frame body and the filtering aperture of the ultra-filtering layer frame body are sequentially reduced.
Furthermore, the parts of the coarse filter layer frame body, the fine filter layer frame body and the ultra-filter layer frame body, which are contacted with the tank body, are hermetically arranged.
Furthermore, the upper end of the rotating shaft is positioned outside the reaction kettle, and the rotating shaft is connected with a rotating motor.
Further, when copper oxide is added, the copper oxide sequentially enters the hollow part of the rotating shaft and the rotating blades from the upper end of the rotating shaft and is transmitted into the reaction kettle from the opening.
Compared with the prior art, the invention has the beneficial effects that:
according to the impurity removal method and the impurity removal equipment applied to the copper sulfate preparation process, excessive dilute sulfuric acid solution and cuprous oxide are added, so that chloride ions completely form cuprous chloride precipitate, and the cuprous chloride precipitate is completely filtered out through the first filtering device; through adding hydrogen peroxide and cupric oxide at the edulcoration device to with the help of the structure of edulcoration device itself, can make ferrous ion form the ferric hydroxide precipitate completely, and filtered out completely through second filter equipment, obtain high purity copper sulfate product at last, impurity such as chloride ion and ferrous ion can be comparatively thoroughly got rid of.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
Fig. 1 is a schematic structural diagram of an impurity removal device applied to a copper sulfate preparation process according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in FIG. 1, the invention provides an impurity removal method applied to a copper sulfate preparation process and impurity removal equipment applied to the copper sulfate preparation process, wherein the impurity removal equipment comprises a first filtering device, a second filtering device and an impurity removal device.
The impurity removal method applied to the copper sulfate preparation process comprises the following steps:
the method comprises the following steps: excess dilute sulfuric acid solution and cuprous oxide are added to the copper sulfate mother liquor containing chloride and ferrous ions to produce a first solution containing precipitate. Wherein, chloride ions in the copper sulfate mother liquor fully react with dilute sulfuric acid and cuprous oxide to obtain cuprous chloride precipitate, and the precipitate can be removed by filtration. Because the cuprous oxide is insoluble in water, the excessive cuprous oxide can be uniformly removed by precipitation and filtration; while hydrogen ions in the dilute sulfuric acid participate in the reaction, and sulfate ions belong to a part of copper sulfate, so that the purity of the product is not influenced.
Step two: filtering the first solution containing the precipitate through a first filtering device 1 to obtain a first filtrate; the precipitate may contain water-insoluble substances such as cuprous chloride and cuprous oxide. The first solution containing the precipitate enters from the upper end of the first filtration device 1. First filter equipment 1 has a jar body, the upper end of jar body is the entry, and the lower extreme is the export, and its inside coarse filtration layer framework 4, essence layer framework 5 and ultrafiltration layer framework 6 have set gradually from top to bottom, coarse filtration layer framework 4, essence layer framework 5 and ultrafiltration layer framework 6 all can transversely be taken out from one side the jar body. Coarse filtration layer framework 4, essence layer framework 5 and ultrafiltration layer framework 6 all include structures such as filter screen, and its filtration pore size reduces in proper order, and density increases gradually promptly, and the size in its pore size can be selected according to industrial production's actual demand, coarse filtration layer framework 4 can get rid of the precipitate of big granule basically, essence layer framework 5 can get rid of 90% precipitate, 99% precipitate impurity can be filtered to ultrafiltration layer framework 6. For the selection of the filter screen, the person skilled in the art can select the filter screen according to actual needs, and the description is not repeated.
Furthermore, the parts of the coarse filtration layer frame body 4, the fine filtration layer frame body 5 and the ultrafiltration layer frame body 6, which are in contact with the tank body, are hermetically arranged. When the precipitate impurities received in the rough filtering layer frame body 4, the fine filtering layer frame body 5 and the ultrafiltration layer frame body 6 are excessive, the frame bodies can be drawn out to clean the impurities. Meanwhile, the frame body can be pulled away from the tank body, so that the replacement is very convenient. Specifically, the one end of framework connects with jar body virtual, and the other end can make things convenient for external force to take out from a jar body, and the other end all seals up the setting with the part of jar body coupling, and here can realize sealed function with the help of high performance sealing washer, can effectually guarantee that the internal liquid of jar can not leak from here.
Step three: introducing the first filtrate (separated from the lower end of the first filtering device) into an impurity removal device 3, and adding hydrogen peroxide and copper oxide to obtain a second solution containing a precipitate; the impurity removing device 3 comprises a reaction kettle, a rotating shaft 31 is vertically arranged in the reaction kettle, a plurality of rotating blades 32 are horizontally arranged at the bottom of the rotating shaft 31, a plurality of openings 33 are formed in the lower surfaces of the rotating blades 32, and the rotating shaft 31 is arranged in a hollow mode and communicated with the openings 33 of the rotating blades 32. The hydrogen peroxide fully reacts with ferrous ions in the copper sulfate mother liquor under the condition of acidity adjustment, so that the ferrous ions are completely oxidized to ferric ions, and meanwhile, the pH value of the whole solution can be adjusted by adding copper oxide, so that the ferric ions are completely hydrolyzed to form ferric hydroxide precipitates. The calculated pH value of ferric ion beginning to precipitate is 2.87; complete precipitation pH 3.87. When the pH of the solution is adjusted by copper oxide, the ferric ions are completely precipitated as ferric hydroxide when the pH is > 3.87.
Further, the upper end of the rotating shaft 31 is located on the outer side of the reaction kettle, and the rotating shaft 31 is connected with a rotating motor. When copper oxide and hydrogen peroxide are added, the copper oxide and the hydrogen peroxide sequentially enter the hollow part of the rotating shaft 31 and the rotating blades 32 from the upper end of the rotating shaft 31 and are transmitted into the reaction kettle from the opening 33. Copper oxide is added from the inside of the rotating shaft 31, so that the copper oxide is transmitted into the reaction kettle through the opening 33 and reacts with the solution in the reaction kettle, and the reaction sufficiency can be ensured. The copper oxide and the hydrogen peroxide are uniformly dispersed in the channel and are transmitted out through the plurality of openings 33, so that the contact area of the copper oxide and the hydrogen peroxide with the solution in the reaction kettle can be increased, and the reaction effect is enhanced. Meanwhile, the rotating shaft 31 can drive the rotating blades 32 to rotate, so that the stirring effect can be enhanced. In order to prevent the copper oxide from directly falling into the reaction vessel from the rotating shaft 31 from the top to the bottom, in the embodiment, the opening 33 is not formed in the portion of the rotating blade 32 facing the rotating shaft 31, so that the copper oxide first moves in the horizontal direction by centrifugal force when falling into the rotating blade 32, and then is mixed with the solution in the reaction vessel through the opening 33.
In the third step, the reaction temperature is controlled to be 50-60 ℃, so that ferrous ions are completely oxidized into ferric ions, and the ferric ions are hydrolyzed to form ferric hydroxide precipitates. Experiments prove that when the reaction temperature is controlled to be 50-60 ℃, the reaction process of ferric ions completely hydrolyzing to form ferric hydroxide precipitates is the most thorough, and the ferric ions can be effectively and completely removed.
Step four: and filtering the second solution containing the precipitate by a second filtering device to obtain a high-purity copper sulfate product (separated and recovered from the bottom of the second filtering device). The second filtering device is provided with a tank body, the upper end of the tank body is an inlet, the lower end of the tank body is an outlet, a coarse filtering layer frame body 4, a fine filtering layer frame body 5 and an ultrafiltration layer frame body 6 are sequentially arranged in the tank body from top to bottom, and the coarse filtering layer frame body 4, the fine filtering layer frame body 5 and the ultrafiltration layer frame body 6 can be transversely pulled out from one side of the tank body. The second filtering device has basically the same structure and basically the same function and effect as the first filtering device 1, and will not be described in a repeated way here. By means of the second filtering device, ferric hydroxide precipitate can be completely removed, and high-purity copper sulfate product can be obtained.
In summary, according to the impurity removal method applied to the copper sulfate preparation process provided by the invention, excessive dilute sulfuric acid solution and cuprous oxide are added, so that chloride ions completely form cuprous chloride precipitate, and the cuprous chloride precipitate is completely filtered out through the first filtering device 1; through adding hydrogen peroxide and cupric oxide at edulcoration device 3 to with the help of the structure of edulcoration device 3 itself, can make ferrous ion form the ferric hydroxide precipitate completely, and filtered out completely through second filter equipment, obtain high purity copper sulfate product finally, impurity such as removal chloride ion and ferrous ion that can be comparatively thorough.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (7)
1. An impurity removing device applied to a copper sulfate preparation process is characterized by comprising a first filtering device, a second filtering device and an impurity removing device;
the first filtering device and the second filtering device are respectively provided with a tank body, the upper end of the tank body is an inlet, the lower end of the tank body is an outlet, a coarse filtering layer frame body, a fine filtering layer frame body and an ultrafiltration layer frame body are sequentially arranged in the tank body from top to bottom, and the coarse filtering layer frame body, the fine filtering layer frame body and the ultrafiltration layer frame body can be transversely pulled out of the tank body from one side;
the impurity removing device comprises a reaction kettle, a rotating shaft is vertically arranged in the reaction kettle, a plurality of rotating blades are horizontally arranged at the bottom of the rotating shaft, a plurality of openings are formed in the lower surfaces of the rotating blades, and the rotating shaft is arranged in a hollow mode and communicated with the openings of the rotating blades;
wherein the lower outlet of the first filtering device is connected to the upper end of the reaction kettle, and the lower outlet of the reaction kettle is connected to the upper end of the second filtering device;
the impurity removal method applied to the copper sulfate preparation process comprises the following steps:
the method comprises the following steps: adding a dilute sulfuric acid solution and cuprous oxide into a copper sulfate mother liquor containing chloride ions and ferrous ions to obtain a first solution containing a precipitate;
step two: filtering the first solution containing the precipitate to obtain a first filtrate;
step three: adding hydrogen peroxide and copper oxide to the first filtrate to obtain a second solution containing precipitates;
step four: filtering the second solution containing the precipitate to obtain the high-purity copper sulfate product.
2. The impurity removing apparatus as claimed in claim 1, applied to a copper sulfate preparation process, wherein: and the filtering pore diameters of the coarse filtering layer frame body, the fine filtering layer frame body and the ultrafiltration layer frame body are sequentially reduced.
3. The impurity removing apparatus as claimed in claim 1, applied to a copper sulfate preparation process, wherein: the upper end of the rotating shaft is located on the outer side of the reaction kettle, and the rotating shaft is connected with a rotating motor.
4. The impurity removing apparatus as claimed in claim 3, applied to a copper sulfate preparation process, wherein: and when copper oxide is added, the copper oxide sequentially enters the hollow part of the rotating shaft and the rotating blades from the upper end of the rotating shaft and is transmitted into the reaction kettle from the opening.
5. The impurity removing apparatus as claimed in claim 1, applied to a copper sulfate preparation process, wherein: in step one, when excess dilute sulfuric acid solution and cuprous oxide are added to the copper sulfate mother liquor, the addition is stopped until no new precipitate is produced.
6. The impurity removing apparatus as claimed in claim 1, applied to a copper sulfate preparation process, wherein: in the second step and the fourth step, a plurality of layers of filter screens are used for filtering in the filtering operation.
7. The impurity removing apparatus as claimed in claim 1, applied to a copper sulfate preparation process, wherein: in the third step, the reaction temperature is controlled to be 50-60 ℃, so that ferrous ions are completely oxidized into ferric ions, and the ferric ions are hydrolyzed to form ferric hydroxide precipitates.
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| US7175819B2 (en) * | 2005-03-04 | 2007-02-13 | Phibro-Tech, Inc. | Regeneration of cupric etchants and recovery of copper sulfate |
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| US3839534A (en) * | 1969-09-18 | 1974-10-01 | Tokai Electro Chem Co Ltd | Process for the treatment of consumed etching solution |
| EP0458119A1 (en) * | 1990-05-24 | 1991-11-27 | Gütling Gmbh | Process and apparatus for separating copper, in particular from cupric chloride etching solutions |
| CN101391800A (en) * | 2007-09-20 | 2009-03-25 | 深圳市东江环保股份有限公司 | Method for producing basic copper chloride, cupric sulfate pentahydrate from copper-containing etching waste liquid |
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| CN106637215A (en) * | 2016-10-21 | 2017-05-10 | 东莞市广华化工有限公司 | Circuit board acid etching waste liquid resource electrolysis oxidizing agent reuse method |
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