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CN112573751B - Recycling treatment device and treatment process for waste tin stripping liquid - Google Patents

Recycling treatment device and treatment process for waste tin stripping liquid Download PDF

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Publication number
CN112573751B
CN112573751B CN202011440030.6A CN202011440030A CN112573751B CN 112573751 B CN112573751 B CN 112573751B CN 202011440030 A CN202011440030 A CN 202011440030A CN 112573751 B CN112573751 B CN 112573751B
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tank
raw material
adjusting
condenser
neutralization
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CN112573751A (en
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蒙晓炜
叶成伟
朱正旭
曾楚姗
查正炯
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Guangzhou Kecheng Environmental Protection Technology Co ltd
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Guangzhou Kecheng Environmental Protection Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/20Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
    • C01B21/38Nitric acid
    • C01B21/46Purification; Separation ; Stabilisation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/36Regeneration of waste pickling liquors
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F2001/007Processes including a sedimentation step
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Metallurgy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Removal Of Specific Substances (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention discloses a resource treatment device and a resource treatment process for waste tin stripping liquid. The resource treatment device of the waste tin stripping liquid comprises a raw material preparation tank, a rectifying tower, a condenser, a neutralization stirring tank, a precipitation adjusting tank, a filter press, a replacement tank and a triple-effect evaporator which are sequentially connected; and a high-level settling tank is connected between the condenser and the precipitation adjusting tank, the raw material blending tank is used for adjusting the concentration of the nitric acid to 15-25%, and the rectifying tower is used for producing the nitric acid, distilled water and kettle residual liquid. The resource treatment device for the waste tin stripping liquid provided by the invention can realize separation and recovery of nitric acid from the waste tin stripping liquid, realizes resource utilization of the waste tin stripping liquid, and has the advantages that the recovery rate of the nitric acid reaches more than 96% and the treatment cost is low.

Description

Recycling treatment device and treatment process for waste tin stripping liquid
Technical Field
The invention relates to the field of environmental protection chemical industry, in particular to a resource treatment device and a treatment process of waste tin stripping liquid.
Background
The waste tin stripping solution is one of main waste liquids generated in the printed circuit board industry, and has the advantages of large residual acidity, complex components, large treatment technical difficulty and high treatment cost. In the traditional technology, the treatment method of the waste tin stripping water mainly comprises a neutralization method and a chemical precipitation method. The basic principle of the neutralization method is that alkali is added into the waste tin stripping water to make the waste liquid close to neutrality, so that metal ions in the waste liquid are converted into metal hydroxide, and then the procedures of precipitation, impurity removal and the like are carried out to prepare stannate, and copper, iron and the like are recovered; the method has complicated treatment process, the waste liquid contains about 20 percent of nitric acid and is wasted in the neutralization process, a large amount of alkali is consumed for neutralizing the part of nitric acid, the treatment cost is increased, and the resource utilization rate is low. The chemical precipitation method is a method of removing heavy metals by adding a certain amount of precipitant and coagulant into waste liquid to convert metal ions into precipitates, for example, adding sulfur-based precipitant (P) and Polyacrylamide (PAM) flocculant into waste tin stripping water, removing metal ions (Cu, Fe, Pb, Sn, etc.) in the waste water, and supplementing nitric acid and ferric nitrate into the treated mother liquid to realize recycling; the method has the advantages of high technical difficulty, non-ideal flocculation effect of colloid, difficult filtration, and secondary pollution to a certain degree due to the addition of various medicaments in the treatment process.
Disclosure of Invention
Accordingly, it is necessary to provide a recycling apparatus and a recycling process for waste tin-stripping solution, which can separate and recover nitric acid from the waste tin-stripping solution, can recycle the waste tin-stripping solution, and can achieve a high recovery rate and a low treatment cost.
A resource treatment device for waste tin stripping liquid comprises a raw material preparation tank, a rectifying tower, a condenser, a neutralization stirring tank, a precipitation adjusting tank, a filter press, a replacement tank and a triple-effect evaporator which are sequentially connected; the system comprises a condenser, a sedimentation adjusting tank, a raw material blending tank, a rectification tower, a neutralization stirring tank, a biochemical treatment system, a sedimentation adjusting tank, a displacement tank, a raw material adjusting tank, a neutralization stirring tank, a biochemical treatment system and a biochemical treatment system, wherein the condenser is connected with the sedimentation adjusting tank, the raw material blending tank is used for adjusting the concentration of nitric acid to 15-25%, the rectification tower is used for producing nitric acid, distilled water and kettle residual liquid, the neutralization stirring tank is used for neutralizing at least part of the distilled water condensed by the condenser to obtain neutralization water, the part of the neutralization water of the neutralization stirring tank is discharged after reaching the standard or enters the biochemical treatment system after failing to reach the standard, the part of the neutralization water of the neutralization stirring tank enters the sedimentation adjusting tank and washes the sediment in the sedimentation adjusting tank, the displacement tank is used for settling the kettle residual liquid to obtain the sediment, the sedimentation adjusting tank is used for adjusting the acidity of the sediment from the high settling adjusting tank, the filter press filter is used for carrying out filter pressing on the sediment from the sedimentation adjusting tank to obtain ferric nitrate solution, the triple-effect evaporator is used for evaporating the ferric nitrate solution displaced by the displacement tank to obtain a ferric nitrate product.
In one embodiment, the recycling device for the waste tin-stripping liquid further comprises a heat exchanger, the heat exchanger is connected between the condenser and the raw material blending tank, and the heat exchanger is used for exchanging heat in the condenser and conveying the heat to the raw material blending tank to preheat the waste tin-stripping liquid.
In one embodiment, the heat exchanger is a heat pump.
In one embodiment, the number of the raw material preparation tanks is at least two, and a plurality of raw material preparation tanks are arranged in parallel and are connected to the rectifying tower.
In one embodiment, the number of the condensers is multiple, and the condensers are arranged in parallel.
In one embodiment, the recycling device for the waste tin-stripping solution further comprises a water storage tank connected between the condenser and the neutralization stirring tank for receiving the distilled water which is from the rectifying tower and condensed by the condenser.
In one embodiment, the water storage tank is further connected to the raw material preparation tank, and part of the distilled water in the water storage tank is sent to the raw material preparation tank to adjust the nitric acid concentration of the waste tin stripping solution in the raw material preparation tank.
In one embodiment, the recycling treatment device for the waste tin stripping liquid further comprises a filtrate storage tank, and the filtrate storage tank is connected between the precipitation regulation tank and the replacement tank.
In one embodiment, the recycling device for the waste tin stripping liquid further comprises a supernatant storage tank, and the supernatant storage tank is connected between the high-level settling tank and the replacement tank.
In one embodiment, the supernatant storage tank is further connected to the raw material blending tank.
In one embodiment, the triple-effect evaporator is also connected to the raw material blending tank, and evaporated water of the triple-effect evaporator flows back to the raw material blending tank.
A resource treatment process of the waste tin stripping liquid comprises the following steps:
controlling the waste tin stripping liquid to enter a raw material blending tank, and adjusting the concentration of nitric acid to 15-25%;
feeding the waste tin stripping liquid in the raw material preparation tank into a rectifying tower for distillation, condensing nitric acid, distilled water and kettle residual liquid produced by the rectifying tower through a condenser, wherein, the residual liquid in the kettle enters a high-level settling tank for settling, the sediment enters a sediment adjusting tank, the distilled water enters a neutralization stirring tank for neutralization to obtain neutralized water, part of the neutralized water in the neutralization stirring tank is discharged after reaching the standard or enters a biochemical treatment system after failing to reach the standard, the partial neutralization water of the neutralization stirring tank enters the precipitation adjusting tank and washes the precipitation from the high-level settling tank to adjust the acidity of the precipitation, the sediment of the sediment adjusting tank is subjected to filter pressing by a filter press, the filtrate of the filter press enters a replacement tank added with iron, and (3) performing iron replacement on the filtrate in the replacement tank to obtain copper and produce a replacement solution, oxidizing the replacement solution to obtain a ferric nitrate solution, and evaporating the ferric nitrate solution through the triple-effect evaporator to obtain a ferric nitrate product.
In one embodiment, the method further comprises the following steps:
and combining part of supernatant of the high-level settling tank with filtrate of the filter press, introducing the combined supernatant into the displacement tank for displacement, and refluxing part of supernatant of the high-level settling tank to the raw material blending tank to adjust the concentration of the nitric acid.
In one embodiment, the method further comprises the following steps:
and the heat in the condenser is transferred to the raw material blending tank through the heat exchanger so as to preheat the waste tin stripping liquid in the raw material blending tank.
The resource treatment device for the waste tin-stripping liquid can realize the separation and recovery of nitric acid from the waste tin-stripping liquid to realize the resource utilization of the waste tin-stripping liquid, the recovery rate reaches more than 96 percent, and the treatment cost is low. The invention utilizes the distillation method to separate and recycle the nitric acid in the waste tin-stripping liquid from the waste liquid to prepare the nitric acid product, thereby realizing the resource utilization of the waste tin-stripping liquid; meanwhile, metal ions and other impurities in the waste tin stripping liquid are concentrated into the distillation residual liquid, and the distillation residual liquid is easy to filter after being heated, washed and precipitated, so that the treatment cost and the treatment difficulty of the production wastewater are effectively reduced.
The resource treatment process of the waste tin stripping liquid has the following beneficial effects:
(1) the high-efficiency recycling of nitric acid in the waste tin stripping liquid is realized. The method can recycle a large amount of nitric acid in the waste tin stripping liquid to prepare the nitric acid product which meets the national standard of 'industrial nitric acid dilute nitric acid' (GB/T337.2-2014), the resource degree is higher, and the recovery rate of the nitric acid in the waste tin stripping liquid reaches more than 96 percent.
(2) Effectively separate nitric acid and other impurities in the waste tin stripping liquid, and ensure the product quality. According to the invention, the distillation method is used for treating the waste tin stripping liquid, so that nitric acid, heavy metal ions and other impurity components in the waste liquid can be effectively separated, and the quality of a resource product is guaranteed; meanwhile, heavy metal ions and other impurity components are locked in the precipitated filter cake, so that the reduction of the waste tin stripping liquid is realized, and the difficulty in recovering the heavy metals in the waste tin stripping liquid is reduced.
(3) Realizes the recycling of heat in the reaction system and reduces the production energy consumption. The invention transfers the heat between the condenser and the raw material blending tank through the heat exchanger such as a heat pump, so that the heat is transferred from the condenser to the raw material blending tank, thereby realizing the cyclic utilization of the heat, reducing the production energy consumption and saving the production cost.
Drawings
Fig. 1 is a schematic view of a recycling apparatus for waste solder stripping solution according to an embodiment of the present invention.
10. A resource treatment device for the waste tin stripping liquid; 100. a raw material blending tank; 200. a rectifying tower; 300. a condenser; 400. a neutralization stirring tank; 500. a sedimentation adjustment tank; 600. a filter press; 700. a replacement tank; 800. a triple effect evaporator; 900. a high-level settling tank; 1000. a heat exchanger; 1100. a water storage tank; 1200. a filtrate storage tank; 1300. and a supernatant storage tank.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
In the description of the present invention, it should be understood that the terms used in the present invention are used in the description of the present invention, and it should be understood that the directions or positional relationships indicated by the terms "center", "upper", "lower", "bottom", "inner", "outer", etc. in the present invention are based on the directions or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
It should be understood that the terms "first", "second", etc. are used herein to describe various information, but the information should not be limited to these terms, which are only used to distinguish one type of information from another. For example, "first" information may also be referred to as "second" information, and similarly, "second" information may also be referred to as "first" information, without departing from the scope of the present invention.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected" and "connected" are to be interpreted broadly, e.g., as being fixed or detachable or integrally connected; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening elements, or they may be in communication within two elements, i.e., when an element is referred to as being "secured to" another element, it may be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an embodiment of the present invention provides a recycling apparatus 10 for waste solder stripping solution.
A resource treatment device 10 for waste tin stripping liquid comprises a raw material preparation tank 100, a rectifying tower 200, a condenser 300, a neutralization stirring tank 400, a precipitation adjusting tank 500, a filter press 600, a replacement tank 700 and a triple-effect evaporator 800.
Referring to fig. 1, a raw material blending tank 100, a rectifying tower 200, a condenser 300, a neutralization stirring tank 400, a precipitation adjusting tank 500, a filter press 600, a displacement tank 700, and a triple-effect evaporator 800 are sequentially connected. A high-level settling tank 900 is also connected between the condenser 300 and the precipitation adjusting tank 500.
The raw material blending tank 100 is used to adjust the concentration of nitric acid to 15-25%. The rectifying tower 200 is used for producing nitric acid, distilled water and still bottoms. The water in the rectifying tower 200 is condensed by the condenser 300 from the top of the rectifying tower 200 and then enters a reflux tank of the rectifying tower 200, reflux and extraction are performed according to a reflux ratio of 2-5, and the extracted water enters a downstream neutralization stirring tank 400 or a water storage tank 1100 described below.
The neutralization agitation tank 400 is used to neutralize at least a portion of the distilled water condensed by the condenser 300 to obtain neutralized water. And part of the neutralized water in the neutralization stirring tank 400 is discharged after reaching the standard or enters a biochemical treatment system after failing to reach the standard. Part of the neutralized water of the neutralization agitation tank 400 enters the precipitation adjustment tank 500 and washes the precipitate in the upper settling tank 900. And adding alkali into the neutralization stirring tank 400 for neutralization, wherein if the neutralized water in the neutralization stirring tank 400 meets the emission standard, the neutralized water can be discharged outside, and if the neutralized water does not meet the emission standard, the neutralized water can be sent to a biochemical treatment system of a wastewater station for further advanced treatment or used for other purposes.
The high settling tank 900 is used for settling the still bottoms to obtain a precipitate. Specifically, since the bottoms contains precipitates, it is necessary to properly withdraw the precipitates to avoid the enrichment of the precipitates in the rectifying tower 200, so as to control the viscosity and the precipitate content of the feed liquid in the rectifying tower 200. Thereby the cauldron bottom liquid of adopting carries out the heat exchange through the condensation and realizes the cooling, then goes to high-order subsider 900, and high-order subsider 900 subsides cauldron raffinate and obtains the sediment.
After the amount of the precipitate in the high-level settling tank 900 reaches a certain amount, the precipitate is collected into the precipitation adjustment tank 500. The precipitation adjustment tank 500 is used to adjust the acidity of the precipitate from the high-level settler 900.
The precipitate after the acidity dilution is sent to a filter press 600, the filter press 600 is used for filter pressing the precipitate from the precipitation adjustment tank 500, the filter cake is collected and then centrally disposed, and the filtrate enters the replacement tank 700.
The substitution tank 700 is used to substitute the filtrate from the filter press 600 to obtain an iron nitrate solution. For example, the copper in the filtrate can be replaced by adding iron to the replacement tank 700 to produce a copper sponge product. And oxidizing the replacement liquid to obtain a ferric nitrate solution. The ferric nitrate solution enters a triple effect evaporator 800.
The triple-effect evaporator 800 is used for evaporating the ferric nitrate solution displaced by the displacement tank 700 to obtain a ferric nitrate product. Distilled water evaporated from the triple-effect evaporator 800 is hydrated and treated with the distilled water of the rectifying tower 200.
Referring to fig. 1, in one embodiment, the recycling apparatus 10 for waste tin-stripping solution further includes a heat exchanger 1000. The heat exchanger 1000 is connected between the condenser 300 and the raw material blending tank 100, and the heat exchanger 1000 is used for exchanging heat in the condenser 300 and transferring the heat to the raw material blending tank 100 to preheat the waste tin stripping liquid. The heat in the condenser 300 can preheat the raw material, i.e., the waste tin-stripping solution, in the raw material blending tank 100 through the coil pipe, and preheat the waste tin-stripping solution of the raw material to 70-80 ℃. The heat exchanger 1000 realizes the recycling of heat energy, thereby saving energy consumption.
In one particular embodiment, the heat exchanger 1000 is a heat pump. It will be appreciated that in other embodiments, the heat exchanger 1000 may take other forms.
In one embodiment, the raw material blending tank 100 is in plurality. Plural means two or more in number. A plurality of raw material blending tanks 100 are arranged in parallel and are all connected to the rectifying tower 200. For example, referring to fig. 1, in one embodiment, the number of the raw material blending tanks 100 is two, two raw material blending tanks 100 are arranged in parallel, and while one raw material blending tank 100 is feeding, the other raw material blending tank 100 performs concentration blending, that is, the two raw material blending tanks 100 work alternately, so that the continuous operation of the whole recycling device 10 for waste tin-stripping solution is realized, and the treatment efficiency is improved. It will be appreciated that in other embodiments, the number of ingredient blending tanks 100 may also be three, four, etc.
In one embodiment, the number of the condensers 300 is plural, and the plurality of condensers 300 are arranged in parallel. For example, in one embodiment, the number of condensers 300 is three. In fig. 1, three numbers of condensers 300 are shown. It will be appreciated that in other embodiments, the number of condensers 300 may also be other numbers, such as two, four, five, etc.
Referring to fig. 1, in one embodiment, the recycling apparatus 10 for waste solder stripping solution further includes a water tank 1100. The water storage tank 1100 is connected between the condenser 300 and the neutralization agitation tank 400, and the water storage tank 1100 functions to buffer the distilled water condensed by the condenser 300. The nitric acid content in the water storage tank 1100 is extremely low, and part of the distilled water in the water storage tank 1100 is sent to the raw material blending tank 100 for adjusting the nitric acid content of the raw material; the remainder of the distilled water is sent to the neutralization agitation tank 400.
Referring to fig. 1, in an embodiment, the recycling apparatus 10 for waste tin-stripping solution further includes a filtrate storage tank 1200. The filtrate storage tank 1200 is connected between the precipitation adjusting tank 500 and the displacement tank 700. The filtrate from the filter press 600 is buffered and stored in the filtrate tank 1200.
Referring to fig. 1, in an embodiment, the recycling apparatus 10 for waste solder stripping solution further includes a supernatant storage tank 1300. The supernatant tank 1300 is connected between the high-level settling tank 900 and the displacement tank 700. The filtrate in the filtrate tank 1200 is combined with the supernatant from the supernatant tank 1300 and then introduced into the substitution tank 700. Part of the supernatant storage tank 1300 may also enter the raw material blending tank 100 for adjusting the nitric acid concentration in the spent tin stripping solution.
Referring to FIG. 1, in one embodiment, a supernatant storage tank 1300 is also connected to the raw material blending tank 100. The supernatant in the supernatant storage tank 1300 is used to adjust the concentration of the raw nitric acid in the raw material blending tank 100. If the concentration in the raw material blending tank 100 is higher than the preset value, water is added for dilution, and if the concentration in the raw material blending tank 100 is lower than the preset value, nitric acid in the supernatant storage tank 1300 is added for thickening.
In one particular embodiment, triple effect evaporator 800 is also connected to neutralization blender tank 400 and/or raw material blending tank 100. The evaporated water from the triple effect evaporator 800 is refluxed to the neutralization and agitation tank 400 and/or the raw material blending tank 100.
The resource treatment device 10 for the waste tin stripping liquid can realize the separation and recovery of nitric acid from the waste tin stripping liquid to realize the resource utilization of the waste tin stripping liquid, and has the recovery rate of more than 96 percent and low treatment cost. The invention utilizes the distillation method to separate and recycle the nitric acid in the waste tin-stripping liquid from the waste liquid to prepare the nitric acid product, thereby realizing the resource utilization of the waste tin-stripping liquid; meanwhile, metal ions and other impurities in the waste tin stripping liquid are concentrated into the distillation residual liquid, and the distillation residual liquid is easy to filter after being heated, washed and precipitated, so that the treatment cost and the treatment difficulty of the production wastewater are effectively reduced.
The invention also provides a resource treatment process of the waste tin stripping liquid.
A resource treatment process of waste tin stripping liquid comprises the following steps:
referring to fig. 1, the waste solder stripping solution is controlled to enter the raw material blending tank 100, and the concentration of the nitric acid is adjusted to 15-25%.
The waste tin stripping liquid in the raw material blending tank 100 enters a rectifying tower 200 for distillation.
Nitric acid, distilled water and still bottoms produced by the rectifying tower 200 are condensed by a condenser 300, wherein the nitric acid can be directly output. And (3) allowing the kettle residual liquid to enter a high-level settling tank 900 for settling, allowing the sediment to enter a settling adjusting tank 500, and allowing the distilled water to enter a neutralization stirring tank 400 for neutralization to obtain neutralized water.
Referring to fig. 1, a part of the neutralized water of the neutralization agitation tank 400 is discharged after reaching the standard or is introduced into a biochemical treatment system after failing to reach the standard, and a part of the neutralized water of the neutralization agitation tank 400 is introduced into a precipitation adjustment tank 500 and the precipitate from the high-level settling tank 900 is washed to adjust the acidity of the precipitate.
The precipitate of the precipitation adjusting tank 500 is pressure-filtered through a pressure filter 600. The filtrate from the filter press 600 is introduced into a substitution tank 700 to which iron is added and substituted. The filtrate in the displacement tank 700 is subjected to iron displacement to obtain copper sponge and produce a displacement liquid. And oxidizing the replacement liquid to obtain a ferric nitrate solution. The ferric nitrate solution is evaporated by a triple effect evaporator 800 to obtain ferric nitrate product.
In a specific embodiment, the recycling treatment process of the waste tin stripping solution further comprises the following steps:
referring to fig. 1, a part of the supernatant of the high-position settling tank 900 is combined with the filtrate of the filter press 600 and enters the displacement tank 700 for displacement, and a part of the supernatant of the high-position settling tank 900 is returned to the raw material blending tank 100 to adjust the concentration of the nitric acid.
In a specific embodiment, the recycling treatment process of the waste tin stripping solution further comprises the following steps:
referring to fig. 1, the heat in the condenser 300 is transferred to the raw material blending tank 100 through the heat exchanger 1000 to preheat the waste tin-stripping solution in the raw material blending tank 100.
The resource treatment process of the waste tin stripping liquid has the following beneficial effects:
(1) the high-efficiency recycling of nitric acid in the waste tin stripping liquid is realized. The method can recycle a large amount of nitric acid in the waste tin stripping liquid to prepare the nitric acid product which meets the national standard of 'industrial nitric acid dilute nitric acid' (GB/T337.2-2014), the resource degree is higher, and the recovery rate of the nitric acid in the waste tin stripping liquid reaches more than 96 percent.
(2) Effectively separate nitric acid and other impurities in the waste tin stripping liquid, and ensure the product quality. According to the invention, the distillation method is used for treating the waste tin stripping liquid, so that nitric acid, heavy metal ions and other impurity components in the waste liquid can be effectively separated, and the quality of a resource product is guaranteed; meanwhile, heavy metal ions and other impurity components are locked in the precipitated filter cake, so that the reduction of the waste tin stripping liquid is realized, and the difficulty in recovering the heavy metals in the waste tin stripping liquid is reduced.
(3) Realizes the recycling of heat in the reaction system and reduces the production energy consumption. According to the invention, heat exchange between the condenser 300 and the raw material blending tank 100 is transferred through the heat exchanger 1000 such as a heat pump, so that heat is transferred from the condenser 300 to the raw material blending tank 100, the cyclic utilization of heat is realized, the production energy consumption is reduced, and the production cost is saved.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
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 various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A resource treatment device for waste tin stripping liquid is characterized by comprising a raw material preparation tank, a rectifying tower, a condenser, a neutralization stirring tank, a precipitation adjusting tank, a filter press, a replacement tank and a triple-effect evaporator which are sequentially connected; the system comprises a condenser, a sedimentation adjusting tank, a raw material blending tank, a rectification tower, a neutralization stirring tank, a biochemical treatment system, a sedimentation adjusting tank, a displacement tank, a raw material adjusting tank, a neutralization stirring tank, a biochemical treatment system and a biochemical treatment system, wherein the condenser is connected with the sedimentation adjusting tank, the raw material blending tank is used for adjusting the concentration of nitric acid to 15-25%, the rectification tower is used for producing nitric acid, distilled water and kettle residual liquid, the neutralization stirring tank is used for neutralizing at least part of the distilled water condensed by the condenser to obtain neutralization water, the part of the neutralization water of the neutralization stirring tank is discharged after reaching the standard or enters the biochemical treatment system after failing to reach the standard, the part of the neutralization water of the neutralization stirring tank enters the sedimentation adjusting tank and washes the sediment in the sedimentation adjusting tank, the displacement tank is used for settling the kettle residual liquid to obtain the sediment, the sedimentation adjusting tank is used for adjusting the acidity of the sediment from the high settling adjusting tank, the filter press filter is used for carrying out filter pressing on the sediment from the sedimentation adjusting tank to obtain ferric nitrate solution, the triple-effect evaporator is used for evaporating the ferric nitrate solution displaced by the displacement tank to obtain a ferric nitrate product.
2. The apparatus for recycling spent tin-stripping solution as claimed in claim 1, further comprising a heat exchanger connected between the condenser and the raw material blending tank, the heat exchanger being configured to exchange heat in the condenser and transfer the heat to the raw material blending tank to preheat the spent tin-stripping solution;
and/or the raw material preparation tanks are arranged in parallel and are connected to the rectifying tower.
3. A resource processing apparatus for spent solder stripping liquid according to claim 1, characterized in that there are a plurality of condensers, and the plurality of condensers are arranged in parallel.
4. A device for recycling spent tin-stripping solution as set forth in any one of claims 1 to 3, further comprising a water storage tank connected between said condenser and said neutralizing agitator tank for receiving distilled water from said rectifying tower after being condensed by said condenser.
5. A resource treatment device for waste tin-stripping liquid as claimed in claim 4, characterized in that said water storage tank is further connected to said raw material blending tank, and part of distilled water in said water storage tank is sent to said raw material blending tank for adjusting the nitric acid concentration of the waste tin-stripping liquid in said raw material blending tank.
6. A resource treatment apparatus for spent tin-stripping solution according to any one of claims 1 to 3, characterized in that the resource treatment apparatus for spent tin-stripping solution further comprises a filtrate storage tank connected between the precipitation adjustment tank and the displacement tank;
and/or, the resourceful treatment device of useless tin liquor that moves back still includes the supernatant storage tank, the supernatant storage tank is connected the high-order subsider with between the replacement groove, the supernatant storage tank still connect in the raw materials blending tank.
7. A resource treatment device of waste tin-stripping liquid as claimed in any one of claims 1 to 3, characterized in that the triple-effect evaporator is also connected to the raw material preparation tank, and evaporated water of the triple-effect evaporator flows back to the raw material preparation tank.
8. A process for recycling spent solder stripping solution using the apparatus for recycling spent solder stripping solution according to any one of claims 1 to 7, comprising the steps of:
controlling the waste tin stripping liquid to enter a raw material blending tank, and adjusting the concentration of nitric acid to 15-25%;
feeding the waste tin stripping liquid in the raw material preparation tank into a rectifying tower for distillation, condensing nitric acid, distilled water and kettle residual liquid produced by the rectifying tower through a condenser, wherein, the residual liquid in the kettle enters a high-level settling tank for settling, the sediment enters a sediment adjusting tank, the distilled water enters a neutralization stirring tank for neutralization to obtain neutralized water, part of the neutralized water in the neutralization stirring tank is discharged after reaching the standard or enters a biochemical treatment system after failing to reach the standard, the partial neutralization water of the neutralization stirring tank enters the precipitation adjusting tank and washes the precipitation from the high-level sedimentation tank to adjust the acidity of the precipitation, the sediment of the sediment adjusting tank is subjected to filter pressing by a filter press, the filtrate of the filter press enters a replacement tank added with iron, and (3) performing iron replacement on the filtrate in the replacement tank to obtain copper and produce a replacement solution, oxidizing the replacement solution to obtain a ferric nitrate solution, and evaporating the ferric nitrate solution through a triple-effect evaporator to obtain a ferric nitrate product.
9. A process for recycling spent tin-stripping solution according to claim 8, further comprising the steps of:
and combining part of supernatant of the high-level settling tank with filtrate of the filter press, introducing the combined supernatant into the displacement tank for displacement, and refluxing part of supernatant of the high-level settling tank to the raw material blending tank to adjust the concentration of the nitric acid.
10. A process as claimed in claim 8 or 9, further comprising the steps of:
and the heat in the condenser is exchanged by a heat exchanger and then is conveyed to the raw material blending tank to preheat the waste solder stripping liquid in the raw material blending tank.
CN202011440030.6A 2020-12-11 2020-12-11 Recycling treatment device and treatment process for waste tin stripping liquid Active CN112573751B (en)

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US6685820B2 (en) * 2002-04-26 2004-02-03 Amia Co., Ltd. Method for treating spent tin/lead stripping solution
CN202626296U (en) * 2012-04-09 2012-12-26 深圳市朗坤环保有限公司 Recycling device of waste tin-stripping liquid
CN103388074B (en) * 2012-05-09 2015-01-21 荆门市格林美新材料有限公司 Method for treating spent tin stripping solution of waste circuit board
CN105293454B (en) * 2015-10-27 2017-03-29 盛隆资源再生(无锡)有限公司 A kind of method that spent solder stripper prepares dust technology, spongy tin and aluminium polychlorid
CN106621434B (en) * 2016-12-26 2019-01-08 中核四0四有限公司 The process and device of nitric acid recycling in a kind of uranium-bearing waste liquid
CN108070721A (en) * 2017-11-10 2018-05-25 河海大学 A kind of nitric acid spent solder stripper tin copper recycling and regeneration method
CN110395837A (en) * 2019-08-01 2019-11-01 广州市中绿环保有限公司 A kind of acid-washing stainless steel waste mixed acid recycling and processing device and technique
CN111170320B (en) * 2019-12-27 2021-01-19 苏州晶洲装备科技有限公司 Device and method for recycling waste acid solution for polycrystalline silicon texturing

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