CN203938483U - A kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid - Google Patents

A kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid Download PDF

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Publication number
CN203938483U
CN203938483U CN201420402894.2U CN201420402894U CN203938483U CN 203938483 U CN203938483 U CN 203938483U CN 201420402894 U CN201420402894 U CN 201420402894U CN 203938483 U CN203938483 U CN 203938483U
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China
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nitric acid
heating unit
inner chamber
storage tank
waste liquid
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Expired - Fee Related
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CN201420402894.2U
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Chinese (zh)
Inventor
陈时全
张瑞辰
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KUNSHAN MINGKUAN ENVIRONMENTAL PROTECTION ENERGY-SAVING TECHNOLOGY CO LTD
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KUNSHAN MINGKUAN ENVIRONMENTAL PROTECTION ENERGY-SAVING TECHNOLOGY CO LTD
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Abstract

The utility model discloses a kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid, it does not need repeat to add the vitriol oil or adopt the technique of stripping, cost-saving and equipment occupation space, and step simplifies the operation, realize resources optimization, design brief being rationally convenient to and control.It comprises vitriol oil storage tank, spent pickle liquor storage tank, it is characterized in that: vitriol oil storage tank, the outlet at bottom of spent pickle liquor storage tank is respectively arranged with pump of constant delivery type, and be communicated to the inner chamber of heating unit, in the inner chamber of heating unit, be furnished with heater strip, the bottom of heating unit is provided with crystallisate outlet conduit, the top outlet of heating unit is furnished with matrass in turn, rectification cell, the top outlet of matrass is communicated with the lower inlet of rectification cell, the top of rectification cell exports the inner chamber entrance on the top of external condensing unit, the inner chamber outlet of the bottom of condensing unit accesses the bottom of nitric acid finished pot by conduit, in the exocoel of condensing unit, be provided with mobile cold water.

Description

A kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid
Technical field
The utility model relates to the technical field that waste liquid reclaims, and is specially a kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid.
Background technology
Plating piece strip waste liquid is one of topmost wastewater source in electroplating wastewater, accounts for the more than 80% of factory effluent total release, and cupric strip waste liquid is a kind of in plating piece strip Cleaning Wastewater.When strip, with nitric acid, the copper on plating piece surface is dissolved through pickling, carrying out along with acid cleaning process, when cupric ion reaches certain concentration, pickle solution just loses pickling ability, become waste liquid, under existing country strictly monitors about electroplating industry emission standard, strip waste liquid discharges after will processing again.What industrial waste was abandoned causes harm; with be precious; one cubic metre of strip waste water of every processing; the approximately thousands of units of clean recovery value; and the important industrial raw material of copper and nitric acid Dou Shi China, be protection of the environment, save capital; realize the policy of resource recycling and national cleaner production, to strip cupric pickling waste waters, must recycle.
In existing treatment process, the close circulation technologies that adopt more, add the vitriol oil after distillation waste liquid, be comparatively pure nitric acid finished product after distilling out nitric acid vapor condensation, for industrial production, realize enterprises recycle, distill out dense waste liquid secondary and add the vitriol oil to stir together post crystallization, then solid-liquid separation obtains copper sulfate finished product, and separated rear filtrate is discharged into waste liquid tank again, realize closed cycle, see Fig. 1.Also have in some comparatively complicated strip waste liquids, the dense waste liquid distilling out is adopted to the method for extracting and separating, isolated multiple extraction liquid adopts different methods to process, and obtains object product.
Existing technique first distills out nitric acid vapor in distillation plant, after condensation, become nitric acid finished product, the concentration of nitric acid finished product is wayward, and the dense waste liquid secondary distilling out adds vitriol oil mix and blend, crystal carries out solid-liquid separation after separating out, and separating liquid (filtrate) enters raw material waste liquid tank to be continued to process.And must meet optimal evaporation processing condition and best 4 Crystallization when selecting processing condition simultaneously, in still-process, need to add the vitriol oil, should can not produce intercrystalline again by high efficiente callback nitric acid, after underpressure distillation, dense waste liquid also needs to continue to add the vitriol oil to continue exsiccation.
Existing technique, integrated operation complex steps needs many cover systems to move simultaneously, and evaporation technology condition and best crystallization condition are wayward, and occupation of land space is large.
Summary of the invention
For the problems referred to above, it is a kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid that the utility model provides, and it does not need repeat to add the vitriol oil or adopt the technique of stripping, cost-saving and equipment occupation space, the step that simplifies the operation, realizes resources optimization, designs brief being rationally convenient to and controls.
A kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid, its technical scheme is such: it comprises vitriol oil storage tank, spent pickle liquor storage tank, it is characterized in that: described vitriol oil storage tank, the outlet at bottom of spent pickle liquor storage tank is respectively arranged with pump of constant delivery type, and be communicated to the inner chamber of heating unit, in the inner chamber of described heating unit, be furnished with heater strip, the bottom of described heating unit is provided with crystallisate outlet conduit, the top outlet of described heating unit is furnished with matrass in turn, rectification cell, the top outlet of described matrass is communicated with the lower inlet of described rectification cell, the top of described rectification cell exports the inner chamber entrance on the top of external condensing unit, the bottom of the inner chamber delivery channel access nitric acid finished pot of the bottom of described condensing unit, in the exocoel of described condensing unit, be provided with mobile cold water, connecting pipeline between described vitriol oil storage tank and described heating unit is provided with the first valve, connecting pipeline between described spent pickle liquor storage tank and described heating unit is provided with the second valve, described crystallisate outlet conduit is provided with the 3rd valve.
It is further characterized in that: the upper space of described matrass, rectification cell is provided with the thermometer well of indent, is placed with respectively thermometer in described thermometer well, and thermometer is mainly to measure steam gradient temperature, is convenient to adjust the temperature of heating unit inner chamber;
The bottom of the exocoel of described condensing unit is provided with cold water inlet, and the top of the exocoel of described condensing unit is provided with cooling water outlet;
Described nitric acid finished pot is closed unit, and the top of described nitric acid finished pot is provided with pipeline and is external at least one section of acid gas capturing device, in described acid gas capturing device, is distilled water;
The pipeline that described nitric acid finished pot is even external to described acid gas capturing device is provided with the 4th valve;
The top exit of described rectification cell is communicated to the inner chamber entrance on the top of described condensing unit by thrust-augmenting nozzle, the top exit of described rectification cell is higher than the inner chamber entrance on the top of described condensing unit;
Described pump of constant delivery type also can be under meter.
A using method from containing reclaiming the device of nitric acid cupric nitrate waste liquid, is characterized in that:
It comprises following steps:
1 opens the first valve, the second valve and the 4th valve, close the 3rd valve, measure the concentration of spent pickle liquor, finished product nitric acid simultaneously, according to the ratio of the concentration requirement of pickling acid solution in strip process and then adjustment mixed solution, by calculating the total amount ratio of the vitriol oil and spent pickle liquor, by pump of constant delivery type, the vitriol oil and spent pickle liquor are imported to heating unit afterwards, due to heated liquid diffusion, therefore utilize well heater that fluid temperature is raise, both are mixed in the inner chamber of heating unit.
2 control heating unit temperature to 100 ℃~140 ℃, distill out nitric acid vapor, make nitric acid vapor through the concentrated high concentrated acid steam of rectification cell rectifying, and enter in nitric acid finished pot after condensing unit condensation.
3 mixed solutions in heating unit through heat generation replacement(metathesis)reaction at heating unit, in matrass, there is distillation crystallization, wherein vitriol oil storage tank and spent pickle liquor storage tank liquid flow rate are controlled with pump of constant delivery type, distillation crystallization forms copper sulfate, heating unit, what in matrass, reaction was separated out is deposited to heating unit bottom containing crystal water copper sulfate crystal, according to the difference containing the crystallization water yield, can manifest the layering of different colours, in technique, continue to add the vitriol oil, and there is the part vitriol oil to sink to heating unit bottom, make copper sulfate crystal dehydration and form white anhydrous copper sulfate crystal in the bottom of heating unit, when reaching a certain amount of, open the 3rd valve, white anhydrous copper sulfate crystal is flowed out by crystallisate outlet conduit.
It is further characterized in that: the spent pickle liquor temperature adding in step 1 is 30 ℃~50 ℃, mix and can produce a large amount of heat, thereby the electric energy used of reduction heating unit reduces thermal losses with the vitriol oil;
In step 2, the preferred temperature of heating unit is 120 ℃;
In process operation process, open the 4th valve, be beneficial to nitric acid phlegma and enter nitric acid finished pot, wherein acid gas enters at least one section of acid gas capturing device through conduit, in receiving tank, is distilled water, and the acid gas of being convenient to overflow fully absorbs, and avoids contaminate environment.
Adopt after the utility model, the vitriol oil and strip spent pickle liquor mix in heating unit and matrass, and fully reaction, the rear nitric acid vapor of reaction is made finished product and is collected in nitric acid finished pot after rectifying and condensation, the copper sulfate crystal that reaction forms in heating unit can regularly be discharged collection, be conducive to device and reach higher distilling effect, and the copper sulfate of collecting recyclable heavy metal copper and sulfuric acid after electrolysis, the copper sulfate obtaining in technique itself can second stage employ, simultaneously, it does not need repeat to add the vitriol oil or adopt the technique of stripping, to sum up, its cost-saving and equipment occupation space, step simplifies the operation, realize resources optimization, designing brief being rationally convenient to controls, and because the outlet at bottom at vitriol oil storage tank, spent pickle liquor storage tank is respectively arranged with pump of constant delivery type, thereby according to the ratio of the concentration requirement of pickling acid solution in strip process and then adjustment mixed solution, and then make the concentration of nitric acid controlled, guarantee to reach optimum concentration of nitric acid.
Accompanying drawing explanation
Fig. 1 is existing from the process flow sheet containing reclaiming nitric acid cupric nitrate waste liquid;
Fig. 2 is the structural representation of device specific embodiment of the present utility model;
In figure, the corresponding reference name of each sequence number is as follows:
Heating unit 1, matrass 2, rectification cell 3, thrust-augmenting nozzle 4, condensing unit 5, vitriol oil storage tank 6, spent pickle liquor storage tank 7, the first valve 8, thermometer well 9, the 3rd valve 10, cold water inlet 11, cooling water outlet 12, crystallisate outlet conduit 13, nitric acid finished pot 14, acid gas capturing device 15, the 4th valve 16, pump of constant delivery type 17, heater strip 18, the second valve 19, conduit 20.
Embodiment
A kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid, see Fig. 2: it comprises vitriol oil storage tank 6, spent pickle liquor storage tank 7, vitriol oil storage tank 6, the outlet at bottom of spent pickle liquor storage tank 7 is respectively arranged with pump of constant delivery type 17, and be communicated to the both sides of the inner chamber of heating unit 1, in the inner chamber of heating unit 1, be furnished with heater strip 18, the bottom of heating unit 1 is provided with crystallisate outlet conduit 13, the top outlet of heating unit 1 is furnished with matrass 2 in turn, rectification cell 3, the top outlet of matrass 2 is communicated with the lower inlet of rectification cell 3, the top of rectification cell 3 exports the inner chamber entrance on the top of external condensing unit 5, the bottom of the bottom conduit access nitric acid finished pot 14 of the inner chamber of condensing unit 5, in the exocoel of condensing unit 5, be provided with mobile cold water, connecting pipeline between vitriol oil storage tank 6 and heating unit 1 is provided with the first valve 8, connecting pipeline between spent pickle liquor storage tank 7 and heating unit 1 is provided with the second valve 19, crystallisate outlet conduit 13 is provided with the 3rd valve 10.
The upper space of matrass 2, rectification cell 3 is provided with the thermometer well 9 of indent, thermometer well 9 is interior, and to be placed with respectively thermometer (not shown in FIG., belong to existing mature technology), thermometer is mainly to measure steam gradient temperature, is convenient to adjust the temperature of heating unit 1 inner chamber; The bottom of the exocoel of condensing unit 5 is provided with cold water inlet 11, and the top of the exocoel of condensing unit 5 is provided with cooling water outlet 12; Nitric acid finished pot 14 is closed unit, and the top of nitric acid finished pot 14 is provided with pipeline and is external at least one section of acid gas capturing device 15, in acid gas capturing device 15, is distilled water; The conduit 20 that nitric acid finished pot 14 is even external to acid gas capturing device 15 is provided with the 4th valve 16; The top exit of rectification cell 3 is communicated to the inner chamber entrance on the top of condensing unit 5 by thrust-augmenting nozzle 4, the top exit of rectification cell 3 is higher than the inner chamber entrance on the top of condensing unit 5; Pump of constant delivery type 17 also can be under meter.
From the using method containing reclaiming the device of nitric acid cupric nitrate waste liquid, it comprises following steps:
1 opens the first valve 8, the second valve 19 and the 4th valve 16, close the 3rd valve 10, measure the concentration of spent pickle liquor, finished product nitric acid, according to the ratio of the concentration requirement of pickle solution in strip process and then adjustment mixed solution, by calculating the total amount ratio of the vitriol oil and spent pickle liquor, by pump of constant delivery type 17 or under meter, the vitriol oil and spent pickle liquor are passed into heating unit 1 afterwards, due to heated liquid diffusion, be that heater strip 18 energisings raise fluid temperature, both are mixed in the inner chamber of heating unit 1; The spent pickle liquor temperature wherein adding is 30 ℃~50 ℃, mix and can produce a large amount of heat, thereby the electric energy used of reduction heating unit reduces thermal losses with the vitriol oil;
2 control heating unit 1 temperature to 100 ℃~140 ℃, distill out nitric acid vapor, make nitric acid vapor through the concentrated high concentrated acid steam of rectification cell 3 rectifying, and enter in nitric acid finished pot 14 after condensing unit 5 condensations; Wherein the preferred temperature of heating unit 1 is 120 ℃;
3 mixed solutions in heating unit 1 through heat generation replacement(metathesis)reaction at heating unit 1, in matrass 2, there is distillation crystallization, wherein vitriol oil storage tank 6 and spent pickle liquor storage tank 7 liquid flow raties are controlled with pump of constant delivery type 17, distillation crystallization forms copper sulfate, heating unit 1, what in matrass 2, reaction was separated out is deposited to heating unit 1 bottom containing crystal water copper sulfate crystal, according to the difference containing the crystallization water yield, can manifest the layering of different colours, in technique, continue to add the vitriol oil, there is the part vitriol oil to sink to heating unit 1 bottom, make copper sulfate crystal dehydration and form white anhydrous copper sulfate crystal in the bottom of heating unit 1, when reaching a certain amount of, open the 3rd valve 10, white anhydrous copper sulfate crystal is discharged by crystallisate outlet conduit 13.
Because nitric acid finished pot 14 is closed unit, open the 4th valve 16, be beneficial to nitric acid phlegma and enter nitric acid finished pot 14, wherein acid gas enters at least one section of acid gas capturing device 15 through conduit 20, in acid gas capturing device 15, be distilled water, the acid gas of being convenient to overflow fully absorbs, and avoids contaminate environment.
Adopt after this device, produce following beneficial effect:
1, the vitriol oil and strip spent pickle liquor mix in heating unit and matrass, and fully reaction; The rear acid vapour of reaction is made finished product and is collected in nitric acid finished pot after rectifying and condensation, the crystal that reaction forms can regularly be discharged collection, is conducive to device and reaches higher distilling effect, and can collect heavy metal copper and sulfuric acid after electrolysis, meanwhile, this device is comparatively easy;
2, matrass and rectification cell are equipped with thermometer, for monitoring distillation acid gas gradient temperature, and control heating unit temperature;
3, the concentration of nitric acid that nitric acid finished pot is collected is higher, direct circulation utilization in can enterprise, simultaneously, the polarity formula specific gravity hydrometer being equipped with can Real-Time Monitoring finished pot in the density of nitric acid, be convenient to adjust the liquid flow rate of sulfuric acid storage tank and spent pickle liquor storage tank, to improve nitric acid finished product utilising efficiency, save production cost;
4, the copper sulfate crystal that in technical process, Crystallization Separation goes out can separately make metallic copper and sulfuric acid by electrolytic process, and meanwhile, the copper sulfate obtaining in technique is through further also can be used as secondary product application after segmentation;
5, floor space is little, simple to operate, meets environmental protection concept and the policy of cleaner production and recycle, saves cost of investment;
6, a small amount of acid vapour that afterbody is discharged absorbs by multistage distilled water, can accomplish zero release, and environment protection, meets national environmental protection policy.
Above specific embodiment of the utility model is had been described in detail, but the preferred embodiment that described content is only created for the utility model can not be considered to the practical range of creating for limiting the utility model.All equalization variations of doing according to the utility model creation application range and improvement etc., within all should still belonging to patent covering scope of the present utility model.

Claims (7)

1. one kind from the device containing reclaiming nitric acid cupric nitrate waste liquid, it comprises vitriol oil storage tank, spent pickle liquor storage tank, it is characterized in that: described vitriol oil storage tank, the outlet at bottom of spent pickle liquor storage tank is respectively arranged with pump of constant delivery type, and be communicated to the inner chamber of heating unit, in the inner chamber of described heating unit, be furnished with heater strip, the bottom of described heating unit is provided with crystallisate outlet conduit, the top outlet of described heating unit is furnished with matrass in turn, rectification cell, the top outlet of described matrass is communicated with the lower inlet of described rectification cell, the top of described rectification cell exports the inner chamber entrance on the top of external condensing unit, the bottom of the inner chamber delivery channel access nitric acid finished pot of the bottom of described condensing unit, in the exocoel of described condensing unit, be provided with mobile cold water, connecting pipeline between described vitriol oil storage tank and described heating unit is provided with the first valve, connecting pipeline between described spent pickle liquor storage tank and described heating unit is provided with the second valve, described crystallisate outlet conduit is provided with the 3rd valve.
2. as claimed in claim 1 a kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid, it is characterized in that: the upper space of described matrass, rectification cell is provided with the thermometer well of indent, in described thermometer well, be placed with respectively thermometer, thermometer is mainly to measure steam gradient temperature, is convenient to adjust the temperature of heating unit inner chamber.
3. a kind of device that reclaims nitric acid from contain cupric nitrate waste liquid as claimed in claim 1 or 2, is characterized in that: the bottom of the exocoel of described condensing unit is provided with cold water inlet, and the top of the exocoel of described condensing unit is provided with cooling water outlet.
4. as claimed in claim 3 a kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid, it is characterized in that: described nitric acid finished pot is closed unit, the top of described nitric acid finished pot is provided with pipeline and is external at least one section of acid gas capturing device, in described acid gas capturing device, is distilled water.
5. as claimed in claim 4 a kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid, it is characterized in that: the pipeline that described nitric acid finished pot is even external to described acid gas capturing device is provided with the 4th valve.
6. as claimed in claim 1 a kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid, it is characterized in that: the top exit of described rectification cell is communicated to the inner chamber entrance on the top of described condensing unit by thrust-augmenting nozzle, the top exit of described rectification cell is higher than the inner chamber entrance on the top of described condensing unit.
7. as claimed in claim 1 a kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid, it is characterized in that: described pump of constant delivery type also can be under meter.
CN201420402894.2U 2014-07-21 2014-07-21 A kind of from the device containing reclaiming nitric acid cupric nitrate waste liquid Expired - Fee Related CN203938483U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104085865A (en) * 2014-07-21 2014-10-08 昆山明宽环保节能科技有限公司 Device for recycling nitric acid from waste liquor containing copper nitrate and use method of device
CN113511667A (en) * 2021-08-04 2021-10-19 庄仓宏 Method and system for recovering nitric acid and copper sulfate from deplating waste liquid

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104085865A (en) * 2014-07-21 2014-10-08 昆山明宽环保节能科技有限公司 Device for recycling nitric acid from waste liquor containing copper nitrate and use method of device
CN113511667A (en) * 2021-08-04 2021-10-19 庄仓宏 Method and system for recovering nitric acid and copper sulfate from deplating waste liquid

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C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20141112

Termination date: 20200721

CF01 Termination of patent right due to non-payment of annual fee