CN110241308B - Method and system for recovering tin metal in nitric acid type tin stripping wastewater - Google Patents

Method and system for recovering tin metal in nitric acid type tin stripping wastewater Download PDF

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CN110241308B
CN110241308B CN201910275995.5A CN201910275995A CN110241308B CN 110241308 B CN110241308 B CN 110241308B CN 201910275995 A CN201910275995 A CN 201910275995A CN 110241308 B CN110241308 B CN 110241308B
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tin
nitric acid
acid type
metal
alkaline solution
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CN110241308A (en
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戴明飞
蒋伟
邱立京
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Wuxi Ansheng Renewable Resources Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B25/00—Obtaining tin
    • C22B25/04—Obtaining tin by wet processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B25/00—Obtaining tin
    • C22B25/06—Obtaining tin from scrap, especially tin scrap
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Metallurgy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention provides a method and a system for recovering tin metal in nitric acid type tin stripping waste water, wherein the pH value of a system is controlled within a certain range by combining a neutralization method and a flocculation method, and then metal ions are precipitated by adding a polymeric flocculant, so that the tin content in a tin hydroxide product can be higher than 50 percent, and compared with the tin recovery treatment process of tin stripping waste water only by one method, the consumption of an alkaline solution and the consumption of a flocculant are greatly reduced, the consumption of the alkaline solution is about 1/2 in the prior art, and the consumption of the flocculant is about 1/3 in the prior art.

Description

Method and system for recovering tin metal in nitric acid type tin stripping wastewater
Technical Field
The application relates to the field of renewable resource utilization and recovery of nonferrous metals, in particular to a method and a system for recovering tin metal in nitric acid type tin stripping wastewater.
Background
The tin-stripping waste liquid is acidic waste water generated in the production process of printed circuit boards, contains a large amount of metal ions such as nitric acid, tin, iron, copper and the like, and various organic matters such as copper corrosion inhibitors, tin suspending agents and the like, can cause tin waste when directly discharged into the environment, can seriously pollute the environment, and has great harm to human beings and the environment. The neutralization method is a traditional method for recovering tin in tin-stripping waste liquid of a circuit board, but the neutralization method in the prior art often has the defects of high precipitation pH and large using amount of alkaline solution, tin obtained by precipitation contains more heavy metal ions such as iron, copper and the like, so that the problems of low tin purity and low tin content are caused, the direct filtration performance is poor, the production time cost is high, the recovery and utilization of tin are seriously influenced, and a plurality of defects exist in the existing tin metal recovery technology for nitric acid type tin-stripping waste water.
Disclosure of Invention
In order to solve the defects, the application provides a method and a system for recovering tin metal in nitric acid type tin stripping wastewater based on the technical concept of the traditional neutralization method.
The first aspect of the invention provides a method for recovering tin metal in nitric acid type tin stripping wastewater, which comprises the following steps:
adding an alkaline solution into the nitric acid type tin stripping wastewater of the tin metal to be recovered at a set liquid inlet speed to form a mixed solution with the pH value of 0.5-0.8;
adding a flocculating agent with a set content into the mixed solution after a preset time length to form a precipitation phase product and a liquid phase product;
and extracting and washing the precipitated phase product to obtain a tin-containing metal product.
In certain embodiments, the alkaline solution is NaOH solution, Na2CO3Solution and NaHCO3One or more of the solutions.
In certain embodiments, the mass fraction of the flocculant is less than 3% o.
In certain embodiments, the preset length of time is greater than 30 minutes.
In certain embodiments, the set feed rate is a feed rate at which the mixed solution can be formed in 40-60 minutes.
The second aspect of the present invention provides a system for recovering tin metal from nitric acid type tin stripping wastewater, comprising:
a neutralization device, which adds alkaline solution into the nitric acid type tin stripping wastewater of tin metal to be recovered at a set liquid inlet speed to form mixed solution with the pH value of 0.5-0.8;
the sedimentation device is used for adding a flocculating agent with a set content into the mixed solution after the preset time length to form a sedimentation phase product and a liquid phase product;
and a washing device for extracting and washing the precipitation phase product to obtain the tin-containing metal product.
The invention has the following beneficial effects:
the invention provides a method and a system for recovering tin metal in nitric acid type tin stripping waste water, wherein the pH value of the system is controlled within a certain range by combining a neutralization method and a flocculation method, then metal ions are precipitated by adding a polymeric flocculant, the tin content in a tin hydroxide product can be higher than 50%, and compared with the tin recovery treatment process of tin stripping waste water only by one method, the consumption of an alkaline solution and the consumption of a flocculant are greatly reduced, the consumption of the alkaline solution is about 1/2 in the prior art, and the consumption of the flocculant is about 1/3 in the prior art, the method and the system realize effective control of actual production cost, greatly reduce the amount of waste water generated again in the actual production treatment process, and shorten the treatment period of the tin stripping waste water.
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, 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 the drawings without creative efforts.
FIG. 1 shows a schematic flow chart of a method for recovering tin metal from nitric acid type tin stripping wastewater in an embodiment of the present application.
FIG. 2 shows a schematic block diagram of a system for recovering tin metal from nitric acid type tin stripping wastewater in an embodiment of the present application.
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.
The tin-stripping waste liquid is acidic waste water generated in the production process of printed circuit boards, contains a large amount of metal ions such as nitric acid, tin, iron, copper and the like, and various organic matters such as copper corrosion inhibitors, tin suspending agents and the like, can cause tin waste when directly discharged into the environment, can seriously pollute the environment, and has great harm to human beings and the environment. In the PCB tin stripping process, according to the composition and working temperature of the nitric acid type tin stripping solution, the principle that tin is stripped by the nitric acid type tin stripping solution is mainly oxidation of tin (0 valence) by dilute nitric acid under the condition of an oxidation assisting agent, and the equation is as shown in formula (1):
Sn+HNO3+H2O→Sn(H2O)6 2++HNO2 (1)
Sn(H2O)6 2+the tin ion is in the initial existence form of tin ions after tin stripping, and simultaneously, some electric pairs are also present in a tin stripping waste liquid system: fe2+/Fe3+、Cu2+/Cu+、HNO3/HNO2、O2/H2O, etc., all of which have electrode potentials lower than that of Sn4+/Sn2+Is high. So Sn (H)2O)6 2+Is easily oxidized into Sn (H)2O)6 4+When the acidity of the system is reduced, the acid hydrolyzes into Sn (H)2O)2(OH)4(white orthostannic acid precipitated, amphoteric, acid or base soluble). The stannic acid becomes metastannic acid after being placed and dehydrated, the metastannic acid has two types of alpha and beta, wherein the type alpha-metastannic acid is amorphous, can be dissolved in acid and alkali and is insoluble in water. The beta-metastannic acid is of a crystal structure, is insoluble in acid and alkali and is insoluble in water. The metastannic acid which is just formed is generally of the alpha type and is converted to the beta type over a longer period of time. Therefore, in the tin stripping waste water newly taken out of the cylinder, a large amount of valuable metallic tin exists in the form of normal stannic acid or metastannic acid, and a very small amount of beta metastannic acid and tin dioxide formed after dehydration exist. The existing technology for treating the tin-stripping waste liquid of the circuit board mainly comprises a neutralization method, a distillation method, an electrolysis method, a membrane separation method and a solvent extraction method. The neutralization method is mature, is widely applied and brings economic and environmental benefits to a certain extent, but the neutralization method in the prior art generally has the following two problems: firstly, the pH value is high when tin ions are precipitated, and is usually between 1.0 and 2.0, so that a large amount of alkaline solution is required to be used, and the tin ions precipitated under the pH condition often comprise oneSome other metal ions have high impurity content and low purity of tin ions.
The application has the defects of higher precipitation pH and large dosage of alkaline solution in a neutralization method, and the tin obtained by precipitation contains more contents of iron, copper and other heavy metal ions, so that the tin has low purity, low tin content, poor direct filtration performance, higher production time cost, serious influence on the problems of recycling of tin and the like. The traditional neutralization method is improved, the pH value of the system is adjusted to be 0.5-0.8, the adding speed of the alkaline solution is strictly controlled, and then the filtering performance of the filtrate is improved by adding a certain amount of flocculating agent, compared with the method that the pH value is required to be adjusted to be 1-2 at present, the tin content in a tin hydroxide product is higher than 50%, the using amount of the alkaline solution is about the traditional 1/2, the tin recovery process is optimized, and the grade of tin mud is improved.
Embodiments of the present application will be described in detail below with reference to the accompanying drawings.
Fig. 1 shows a schematic flow chart of a method for recovering tin metal in nitric acid type tin stripping wastewater in an embodiment of the first aspect of the present application.
The method for recovering tin metal in nitric acid type tin stripping wastewater in the embodiment of the first aspect of the application specifically comprises the following steps:
and S100, adding an alkaline solution into the nitric acid type tin stripping wastewater to be recovered with tin metal at a set liquid inlet speed to form a mixed solution with the pH value of 0.5-0.8.
And S200, adding a flocculating agent with a set content into the mixed solution after a preset time length to form a precipitation phase product and a liquid phase product.
S300, extracting and washing the precipitated phase product to obtain a tin-containing metal product.
In the conventional neutralization method, a large amount of experimental data shows that: because the particle size of the tin hydroxide powder is small, iron ions in the waste liquid can not be coprecipitated within the range that the pH value is less than 0.8, and further the formation of large-particle ferric hydroxide colloid is hindered, so that the filtering performance is poor, and the production time cost is high. This embodiment is in 0.5 to 0.8 through adjusting pH, the less tin hydroxide powder of a large amount of particle diameters has in the messenger mixed solution, then make tin hydroxide powder form flocculent large granule colloid through the flocculating agent, the effect of flocculating agent has played the effect of iron ion in traditional neutralization method, and then do not need the iron ion in the waste liquid to participate in the formation of colloidal substance when pH is in 0.5 to 0.8, can effectively realize the sediment of tin hydroxide on the one hand, on the other hand does not contain (or contains few) iron ion in the precipitate, the tin purity in the tin hydroxide product has further been improved, and then make the tin content be higher than 50%. Meanwhile, the dosage of the alkaline solution is greatly reduced because the pH is between 0.5 and 0.8, and the dosage of the alkaline solution is about 1/2 which is traditional. Furthermore, as the flocculating agent in the application only needs to achieve the same action degree with the iron ions in the waste liquid, the coprecipitation tin hydroxide colloid can be formed with extremely small dosage, and the dosage of the flocculating agent is small, compared with the traditional flocculation method (directly adding the flocculating agent), the dosage of the flocculating agent only needs the traditional 1/3.
In this embodiment, the set feeding rate is a feeding rate at which the mixed solution can be formed within 40 to 60 minutes. This example avoids local precipitation of other metals due to too high a local alkaline solution concentration by tightly controlling the alkaline solution addition rate.
In alternative embodiments, the alkaline solution may be a conventional alkaline solution with little or no side reactions, such as NaOH solution, Na2CO3Solution and NaHCO3One or more of the solutions.
In addition, in one embodiment, the mass fraction of the flocculant is less than 3% o. The dosage of the flocculating agent in the embodiment is far lower than that of the traditional flocculation method, and the mass fraction is less than 3 per mill, so that the embodiment can be realized.
Further, the preset time is longer than 30 minutes, after 30 minutes, the pH value of the mixed solution is uniformly distributed, and at the moment, a flocculating agent is added to facilitate uniform precipitation.
Based on the same technical concept as that of the first aspect embodiment of the present application, a second aspect embodiment of the present application provides a system for recovering tin metal in nitric acid type tin stripping wastewater, as shown in fig. 2, including:
a neutralization device 100 for adding an alkaline solution into the nitric acid type tin stripping wastewater of tin metal to be recovered at a set liquid inlet speed to form a mixed solution with the pH value of 0.5-0.8;
the settling device 200 adds a flocculating agent with a set content into the mixed solution after a preset time length to form a settling phase product and a liquid phase product;
washing device 300, extracting and washing the precipitated phase product to obtain a tin-containing metal product.
The neutralization device 100 may be a conventional stirring reaction tank or a mixing tank, etc., and the present application is not limited thereto. The alkaline solution can be fed in a manner that the alkaline solution is pumped into a mixing tank or a reaction tank through a micro pump, and the rotating speed of the micro pump is regulated, so that the set speed is regulated to be the feeding speed capable of forming the mixed solution within 40-60 minutes.
The precipitation device 200 may be a settling tank or the like, wherein the liquid phase product is in the upper layer and the precipitated phase product is in the lower layer to form a filter cake.
The washing device 300 may be an ultrasonic washing tank, a centrifugal washing device, or a conventional filter, and washing is performed by filtration, but the present application is not limited thereto.
Based on the same technical concept as the above embodiment, in a preferred or alternative embodiment, the mass fraction of the flocculant is less than 3 per mill, the preset time is longer than 30 minutes, and the alkaline solution is NaOH solution or Na2CO3Solution and NaHCO3One or more of the solutions will not be described in detail herein.
The recovery system of tin metal in nitric acid type tin stripping waste water that this aspect embodiment provided can realize that the tin content in the tin hydroxide product is higher than 50%, compare and only use a method to carry out tin stripping waste liquid's tin recovery processing in-process required alkaline solution quantity and flocculating agent quantity greatly reduced, the alkaline solution quantity is about traditional 1/2, the flocculating agent quantity is about traditional 1/3, the effectual control that has obtained of actual manufacturing cost has been realized, and the waste water volume that produces once more in the actual manufacturing process also significantly reduces, the treatment cycle of tin stripping waste liquid has been shortened.
The above embodiments of the present application are described in detail below with reference to specific scenarios, but it is understood that the following scenarios provide specific experimental parameters, but the present application is not limited thereto, and those skilled in the art can reasonably adjust suitable parameters according to actual situations.
Implementation scenario 1
Taking 1000mL of the tin-stripping waste liquid, controlling the adding speed of alkali liquor by a miniature pump under the stirring condition, adding 4mol/L of alkali liquor, adjusting the pH value to 0.5, stirring for 30min, adding 3 per thousand of flocculant, reacting for 30min after obvious layering, carrying out solid-liquid separation, washing a filter cake by using tap water with the mass ratio of 1:3, and then carrying out solid-liquid separation to obtain the product with the tin content of 50.8% in the filter cake, wherein the tin content in the filtrate is not detected. The filtrate obtained in the experimental process can be used for neutralizing raw materials or diluting water in the subsequent waste alkali treatment process.
Implementation scenario 2
Taking 1000mL of the tin-stripping waste liquid, controlling the adding speed of alkali liquor by a miniature pump under the stirring condition, adding 6mol/L of alkali liquor, adjusting the pH value to 0.7, stirring for 30min, adding 3 per thousand of flocculant, reacting for 30min after obvious layering, carrying out solid-liquid separation, washing a filter cake by using tap water with the mass ratio of 1:3, and then carrying out solid-liquid separation to obtain the filter cake with the tin content of 51.4%, wherein the tin in the filtrate is not detected. The filtrate obtained in the experimental process can be used for neutralizing raw materials or diluting water in the subsequent waste alkali treatment process.
Implementation scenario 3
Taking 1000mL of the tin-stripping waste liquid, controlling the adding speed of alkali liquor by a miniature pump under the stirring condition, adding 8mol/L of alkali liquor, adjusting the pH value to 0.8, stirring for 30min, adding 3 per thousand of flocculant, reacting for 30min after obvious layering, carrying out solid-liquid separation, washing a filter cake by using tap water with the mass ratio of 1:3, and then carrying out solid-liquid separation to obtain the filter cake with the tin content of 54.6%, wherein the tin in the filtrate is not detected. The filtrate obtained in the experimental process can be used for neutralizing raw materials or diluting water in the subsequent waste alkali treatment process.
Implementation scenario 4
Taking 1000mL of the tin-stripping waste liquid, controlling the adding speed of alkali liquor by a miniature pump under the stirring condition, adding 10mol/L of alkali liquor, adjusting the pH value to 0.8, stirring for 30min, adding 3 per thousand of flocculant, reacting for 30min after obvious layering, carrying out solid-liquid separation, washing a filter cake by using tap water with the mass ratio of 1:3, and then carrying out solid-liquid separation to obtain the filter cake with the tin content of 53.6%, wherein the tin in the filtrate is not detected. The filtrate obtained in the experimental process can be used for neutralizing raw materials or diluting water in the subsequent waste alkali treatment process.
According to the implementation scene, the recovery method and the recovery system for tin metal in the nitric acid type tin stripping wastewater can realize that the tin content in a tin hydroxide product is higher than 50%, the mass fraction of the flocculating agent can be 3 per mill, the dosage of an alkaline solution is about traditional 1/2, and the dosage of the flocculating agent is about traditional 1/3.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of an embodiment of the specification. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example.
Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction. The above description is only an example of the embodiments of the present disclosure, and is not intended to limit the embodiments of the present disclosure. Various modifications and variations to the embodiments described herein will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the embodiments of the present specification should be included in the scope of the claims of the embodiments of the present specification.

Claims (5)

1. A method for recovering tin metal in nitric acid type tin stripping wastewater is characterized by comprising the following steps:
adding an alkaline solution into the nitric acid type tin stripping wastewater of the tin metal to be recovered at a set liquid inlet speed to form a mixed solution with the pH value of 0.5-0.8;
adding a flocculating agent with a set content into the mixed solution after a preset time length to form a precipitation phase product and a liquid phase product;
and extracting and washing the precipitated phase product to obtain a tin-containing metal product.
2. The recovery method according to claim 1, wherein the alkaline solution is NaOH solution, Na2CO3Solution and NaHCO3One or more of the solutions.
3. The recovery method according to claim 1, wherein the mass fraction of the flocculant is less than 3 ‰.
4. A recycling method according to claim 1, characterized in that said preset duration is greater than 30 minutes.
5. The recovery method according to any one of claims 1 to 4, wherein the set feed rate is a feed rate at which the mixed solution can be formed within 40 to 60 minutes.
CN201910275995.5A 2019-04-08 2019-04-08 Method and system for recovering tin metal in nitric acid type tin stripping wastewater Active CN110241308B (en)

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CN110484736B (en) * 2019-09-29 2021-06-04 湖南仁发材料科技有限公司 Method for purifying zinc sulfate leaching solution to remove copper
CN111875146B (en) * 2020-08-10 2021-04-16 清远市新绿环境技术有限公司 Resource utilization system and method for tin-stripping wastewater
CN112573698B (en) * 2020-11-26 2022-12-27 苏州美源达环保科技股份有限公司 Method for recovering tin in PCB production process
CN112624181A (en) * 2020-12-30 2021-04-09 惠州Tcl环境科技有限公司 Method for preparing tin hydroxide by using tin-containing waste liquid
CN115557635A (en) * 2022-09-30 2023-01-03 广东工业大学 Method for treating nitric acid type tin stripping wastewater
CN115849434A (en) * 2022-12-19 2023-03-28 昆山中环实业有限公司 Method for purifying tin hydroxide from tin-stripping waste liquid

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CN102351344A (en) * 2011-07-08 2012-02-15 无锡市霄鹰环境科技有限公司 Tin-bearing waste liquid recovery system and recovery technology

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