CN100497735C - Method of treating stainless steel chemical pigmentation aging liquid - Google Patents
Method of treating stainless steel chemical pigmentation aging liquid Download PDFInfo
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- CN100497735C CN100497735C CNB2007100620165A CN200710062016A CN100497735C CN 100497735 C CN100497735 C CN 100497735C CN B2007100620165 A CNB2007100620165 A CN B2007100620165A CN 200710062016 A CN200710062016 A CN 200710062016A CN 100497735 C CN100497735 C CN 100497735C
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- steel chemical
- electrolytic oxidation
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The present invention discloses a processing method for non-corrodible steel chemical tinting aging solution. The method comprises the following steps: above all, adopting a evaporation partition method to separate the solid mixture of hexavalent chromium and ferric iron salts, trivalent chromium solution (also containing bivalence nickle and small quantity of ferric iron ion ) and distilled water out of the tinting aging solution, wherein the solid mixture and the distilled water can be cyclic-used for preparing new tinting solution (in which the ferric iron salt has small dissolvability and then can be removed by filtration ); then, adopting an electrolytic oxidation method for directly oxidating the diluent of trivalent chromium solution into hexavalent chromium and separating the bivalence nickle and the residual ferric iron ions by enriching them at cathodes, wherein the anode liquor after oxidation can be used directly for preparing new tinting solution and the catholyte can be cyclic-used for preparing new anode liquor. The present invention realizes circulation utilization of chromium and sulphuric acid as well as separation and reclaiming of nickle and iron, is characterized by its simple operations, mild conditions, simple equipments and zero discharge and the like, perfects entire process of INCO chemical tinting method, and has industrialisation foreground.
Description
Technical field
The present invention relates to a kind of stainless steel chemical pigmenting liquid, especially a kind of recycle treatment process that is used for stainless steel chemical pigmentation aging liquid.
Background technology
Color Stainless Steel is because of its unique advantages energy, has marketable value and more and more is subjected to people's favor.Among numerous preparation methods of relevant Color Stainless Steel, with acidic chemical painted (INCO) method because have bright in luster, wear resistant corrosion resistant good and be not subjected to characteristics such as the steel part shape influences and be most widely used.But, therefore greatly restricted applying of this method owing to contain more unmanageable high-concentration sulfuric acid and sexavalent chrome in its painted aging liquid.Treatment process to the existing chrome waste liquid of reporting can reduce following several:
(1) reduction method: because Cr
3+Toxicity is less relatively, so usually with the Cr in the waste liquid
6+Directly be reduced into Cr
3+, and then do next step processing.Wherein reduction mode comprises: chemical reduction method (seeing patent CN88106261.8, CN87105091.9, CN1263685C, CN1562510A, CN1073414A, CN1112608A, CN1003237B, JP54139261, JP55031439, JP2004223472, FR2865727, US2007051676, US2006016757, CA787884 etc.); Electrolytic reduction (seeing patent CN1255327C, CN86106414B, CN1763262A, JP2003260465 etc.); Biological reducing method (seeing patent CN1657430A, CN1733375A, CN1759942A, CN1644534A, JP2005177740, WO2007020588, KR20030005447 etc.) and water vapor transform reduction method (seeing patent CN1007134B) etc.But this method generally only is applicable to handles Cr
6+Alkalescence or neutral waste liquid that content is little are not fit to strongly-acid, high Cr
6+The processing of the aging liquid of the stainless steel coloring of content.
(2) precipitator method: with Cr
6+With PbCrO
4, BaCrO
4Or the precipitation forms of chromic sulfide is removed (seeing patent CN1166572C, CN1009730B, CN1039401A, CN1052102A, CN1526656A, CN1104384C, CN1597555A etc.).But this method can not be used for processing and contain sulfuric acid and chromic waste liquid simultaneously, because PbSO
4, BaSO
4Can separate out the final more difficult separation of gained precipitation mixture equally with precipitation forms.
(3) ion exchange method: with Cr
6+With CrO
4 2-Or Cr
2O
7 2-Form, after anti-strong acid scale resistance resin absorption collection, do next step processing (seeing patent CN1810683A, CN1762830A, JP52090164, EP0705793, US4036751, RU2291113, KR20040087440, KR20040034767 etc.) again.But this method generally is used to handle the less waste liquid of content of 6-valence Cr ions, and when containing the processing of the painted aging liquid of chromium for stainless high density, resin demand is very big, cost is high and the regeneration difficulty.
(4) extraction process: earlier isolate Cr in the waste liquid with extraction agent
6+, collect Cr with strippant again
6+, and then do next step processing (seeing patent CN1106361A, CN1220174A, JP2006320805, KR20050003079, KR100312274B etc.).This method generally also only is applicable to Cr
6+The waste liquid that content is low, and extraction agent and strippant consumption are big, efficient is low, operate loaded down with trivial details, the cost height.
As seen, aforesaid method all is not suitable for handling strongly-acid, high Cr
6+The stainless steel chemical pigmentation aging liquid of content.
Summary of the invention
The problem to be solved in the present invention is the pollution problem of chemical pigmentation aging liquid, the recovery and the cycling and reutilization problem thereof of useful component, its objective is the green treatment process that a kind of stainless steel chemical pigmentation aging liquid is provided.
The present invention at first adopts the evaporation partition method, isolates the solid mixture, trivalent chromium solutions (also containing nickelous and a small amount of ferric ion) and the distilled water that contain sexavalent chrome and trivalent iron salt from painted aging liquid; Adopt electrolytic oxidation then, the trivalent chromic ion in the above-mentioned trivalent chromium solutions is direct oxidation into sexavalent chrome at anode, simultaneously nickelous and a spot of ferric ion are enriched in negative electrode and separated.
The treatment process of stainless steel chemical pigmentation aging liquid of the present invention, its concrete grammar follow these steps to carry out:
(1) evaporation separating treatment:, isolate solid mixture, trivalent chromium solutions (also containing nickelous and a small amount of ferric ion) and the distilled water of sexavalent chrome and trivalent iron salt from aging liquid by with stainless steel chemical pigmentation aging liquid heating evaporation, cooling, crystallization and filtration.
The mode of its evaporation separating treatment has: atmospheric evaporation separates or reduction vaporization separates; Wherein the temperature of atmospheric evaporation is 95 ℃～140 ℃, and the temperature of reduction vaporization is 60 ℃～110 ℃; Treatment time is 30min～50min.
Solid mixture and the distilled water preparation that is used for new coloring liquid capable of circulation that its evaporation separating treatment reclaims because of trivalent iron salt solubleness is little, can remove by filter when the new coloring liquid of preparation.
(2) electrolytic oxidation is handled: the diluent of above-mentioned trivalent chromium solutions is placed electrolytic oxidation apparatus, carrying out electrolytic oxidation handles, at anode trivalent chromic ion is direct oxidation into sexavalent chrome, simultaneously bivalent nickel ion is enriched in catholyte, and remaining a small amount of ferric ion is reduced and is deposited on negative electrode.
Used anode material was during its electrolytic oxidation was handled: platinum, lead, plumbic oxide, titanium base platinum, ti-supported lead dioxide electric or graphite etc.; Used cathode material is: platinum, lead, plumbic oxide or graphite etc.; Used diaphragm material is: cationic exchange membrane or ceramic membrane etc.
The processing range that its electrolytic oxidation is handled is: make anolyte with the diluent that contains chromic liquid; Sulphuric acid soln with 5%～30% is made catholyte; By electrolytic oxidation, trivalent chromium is oxidized to sexavalent chrome, temperature is: 40 ℃～80 ℃, anodic current density is: 150～350A/m
2, the treatment time is looked Cr in the anolyte
3+Amount and annode area and deciding.
Anolyte after its electrolytic oxidation is handled can be directly used in the preparation of new coloring liquid; Catholyte after electrolytic oxidation is handled can repeatedly circulate and be used to prepare new anolyte, Ni in catholyte
2+Concentration when higher, can further reclaim nickel by chemistry or electrochemical reducing.
The treatment process of stainless steel chemical pigmentation aging liquid of the present invention is compared with traditional chrome waste liquid treatment process, has (1) this technology and can be directly used in processing strongly-acid and high density Cr
6+Aging liquid and other waste liquid are realized separating and recovery of chromium and vitriolic recycle and nickel and iron; (2) sexavalent chrome that reclaims in the evaporating concentration process (containing trivalent iron salt) and the distilled water preparation that is used for new coloring liquid all capable of circulation, little because of trivalent iron salt solubleness simultaneously, directly filtering when the new coloring liquid of preparation; (3) in the electrolytic acid cleaning oxydation process, be oxidized to the chromic while at trivalent chromic ion, remaining ferric ion is deposited on negative electrode, and bivalent nickel ion mainly is enriched in the catholyte; (4) anolyte behind the electrolytic oxidation can be directly used in the preparation of new coloring liquid; Catholyte can repeatedly circulate and be used to prepare new anolyte, when bivalent nickel ion concentration is higher in the catholyte, can further reclaim nickel by chemistry or electrochemical reducing; (5) this technology also has easy and simple to handle, mild condition, equipment is simple and characteristics such as zero release, has remedied the deficiency of INCO chemical coloring process preferably, and perfect whole technology has industrial prospect.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Fig. 2 is an electrolytic oxidation apparatus synoptic diagram of the present invention
Among the figure: 1: the stainless steel coloring liquid 2 that wears out: evaporation separating treatment 3: distilled water 4: chromic trioxide and trivalent iron salt 5: the aging liquid 6 of residue: electrolytic oxidation handles 7: anolyte 8 after the oxidation: catholyte 9 after the oxidation: catholyte repeatedly circulates and is used to prepare new anolyte 10: further by chemistry or electrochemical reducing recovery nickel 11: power supply 12: current meter 13: anode 14: anolyte 15: agitator 16: barrier film 17: catholyte 18: negative electrode
Embodiment
The present invention further describes as follows in conjunction with the accompanying drawings with embodiment:
The first step, evaporation separating treatment: get the 160mL stainless steel chemical pigmentation aging liquid, place 250mL to be assembled with the there-necked flask of agitator, thermometer and prolong.When stirring down with electric mantle direct heating to 95 ℃, solution comes to life subsequently temperature-stable at 98 ℃.Behind about 40min, temperature slowly rises to 140 ℃, and this moment, substantially anhydrous drip went out.Stop heating, after leaving standstill cool to room temperature, ice bath cools off 4h～5h again, suction filtration, with solid dry 5h～6h under 90 ℃～100 ℃, can get the sorrel particulate solid mixture of 28.7g chromic trioxide and trivalent iron salt, it is capable of circulation to be used for the preparation (this moment is because of chromic trioxide and trivalent iron salt dissolubility difference, but filtering trivalent iron salt) of new coloring liquid.It is stand-by to collect the thick trivalent chromium solutions of deep green (also containing nickelous and a small amount of ferric ion) simultaneously.
In second step, electrolytic oxidation is handled: get the trivalent chromium solutions of 70mL after the first step is handled, place electrolytic oxidation apparatus as anolyte after diluting one times, catholyte is made barrier film with 30% sulphuric acid soln with the tetrafluoroethylene cationic exchange membrane, and platinized platinum is made anode, stereotype is made negative electrode, connects circuit.Stir heating in water bath down, be warmed up to 80 ℃ after, connect power supply, the control anodic current density is 350A/m
2, electrolytic oxidation is handled 6h, during should suitably add less water.After reaction finishes, get the garnet anolyte, record Cr
6+Content 52.08g/L, Cr
3+Content 0.89g/L, Fe
3+Content 0.27g/L, Ni
2+Content 0.31g/L, transformation efficiency 72.37%, current efficiency 94.19%.As seen, this moment, this anolyte can be directly used in the preparation of new coloring liquid.In addition, the preparation that is used for next time new anolyte capable of circulation of the catholyte after the oxidation.
The first step evaporation separating treatment: get the aging liquid of 160mL stainless steel coloring, place 250mL to be assembled with the there-necked flask of agitator, thermometer and prolong.Decompression (the about 0.01MPa of vacuum tightness) is stirred down, and when being warmed up to 60 ℃ with oil bath, solution comes to life, and temperature-stable is at 72 ℃ subsequently.Behind about 30min, temperature slowly rises to 107 ℃, and this moment, substantially anhydrous drip went out.Stop heating, leave standstill cool to room temperature, ice bath cools off 4h～5h again, suction filtration, with solid dry 5h～6h under 90 ℃～100 ℃, can get the sorrel granular mixture of 27.9g chromic trioxide and trivalent iron salt, it is capable of circulation to be used for the preparation (this moment is because of chromic trioxide and trivalent iron salt dissolubility difference, but filtering trivalent iron salt) of new coloring liquid.It is stand-by to collect the thick trivalent chromium solutions of deep green (also containing nickelous and a small amount of ferric ion) simultaneously.
The second one-step electrolysis oxide treatment: get the trivalent chromium solutions of 50mL after the first step is handled, place electrolytic oxidation apparatus as anolyte after the dilution twice, catholyte is with 20% sulphuric acid soln, with A
4Ceramic membrane is made barrier film, and titanium base platinized electrode is made anode, and graphite is made negative electrode, connects circuit.After stirring down warming-in-water to 65 ℃, connect power supply, the control anodic current density is 300A/m
2, electrolytic oxidation is handled 4h, during should suitably add some water.After reaction finishes, get the garnet anolyte, record Cr
6+Content 32.08g/L, Cr
3+Content 0.63g/L, Fe
3+Content 0.16g/L, Ni
2+Content 0.24g/L, transformation efficiency 75.84%, current efficiency 91.43%.This anode liquid can be directly used in the preparation of new coloring liquid, and the catholyte after the oxidation is capable of circulation to be used for the preparation of new anolyte next time
The first step evaporation separating treatment is with embodiment 1.
The second one-step electrolysis oxide treatment: get the trivalent chromium solutions of 35mL after the first step is handled, place electrolytic oxidation apparatus as anolyte after diluting three times, catholyte is with 10% sulphuric acid soln, make barrier film with the common cation exchange membrane, ti-supported lead dioxide electric pole is made anode, stereotype is made negative electrode, connects circuit.After stirring down warming-in-water to 50 ℃, connect power supply, the control anodic current density is 250A/m
2, electrolytic oxidation is handled 2.5h, during should suitably add some water.After reaction finishes, get the garnet anolyte, record Cr
6+Content 26.13g/L, Cr
3+Content 0.51g/L, Fe
3+Content 0.09g/L, Ni
2+Content 0.19g/L, transformation efficiency 78.64%, current efficiency 96.36%.This moment, this anolyte can also be directly used in the preparation of new coloring liquid, and the catholyte after the oxidation is capable of circulation to be used for the preparation of new anolyte next time.
The first step evaporation separating treatment is with embodiment 2.
The second one-step electrolysis oxide treatment: get the trivalent chromium solutions of 30mL after the first step is handled, place electrolytic oxidation apparatus as anolyte after diluting four times, catholyte is with 5% sulphuric acid soln, with A
3Ceramic membrane is made barrier film, and lead dioxide electrode is made anode, and graphite is made negative electrode, connects circuit.After stirring down warming-in-water to 40 ℃, connect power supply, the control anodic current density is 200A/m
2, electrolytic oxidation is handled 2h, during should suitably add some water.After reaction finishes, get bolarious anolyte, record Cr
6+Content 21.09g/L, Cr
3+Content 0.47g/L, Fe
3+Content 0.05g/L, Ni
2+Content 0.11g/L, transformation efficiency 81.08%, current efficiency 97.34%.This moment, this anolyte can be directly used in the preparation of new coloring liquid, and the catholyte after the oxidation is capable of circulation to be used for the preparation of new anolyte next time.
Claims (6)
1. the treatment process of stainless steel chemical pigmentation aging liquid is characterized in that the treatment process of this aging liquid follows these steps to carry out:
1) evaporation separating treatment:, from aging liquid, isolate solid mixture, trivalent chromium solutions and the distilled water of sexavalent chrome and trivalent iron salt with stainless steel chemical pigmentation aging liquid heating evaporation, cooling, crystallization and filtration;
2) electrolytic oxidation is handled: the diluent of the trivalent chromium solutions in the step 1) is placed electrolytic oxidation apparatus, carrying out electrolytic oxidation handles, at anode trivalent chromic ion is direct oxidation into sexavalent chrome, simultaneously bivalent nickel ion is enriched in catholyte, and remaining a small amount of ferric ion is reduced and is deposited on negative electrode.
2. the treatment process of stainless steel chemical pigmentation aging liquid as claimed in claim 1 is characterized in that the mode of evaporating separating treatment has: atmospheric evaporation separation or reduction vaporization separation; Wherein the isolating temperature of atmospheric evaporation is 95 ℃～140 ℃, and the isolating temperature of reduction vaporization is 60 ℃～110 ℃; The evaporation separating treatment time is 30min～50min.
3. the treatment process of stainless steel chemical pigmentation aging liquid as claimed in claim 1, it is characterized in that evaporating solid mixture that separating treatment reclaims and distilled water can circulate and be used for the preparation of new coloring liquid, wherein trivalent iron salt is little because of solubleness, can remove by filter in the new coloring liquid process of preparation.
4. the treatment process of stainless steel chemical pigmentation aging liquid as claimed in claim 1 is characterized in that used anode material is in the electrolytic oxidation processing: platinum, lead, plumbic oxide, titanium base platinum, ti-supported lead dioxide electric or graphite; Used cathode material is: platinum, lead, plumbic oxide or graphite; Used diaphragm material is: cationic exchange membrane or ceramic membrane.
5. the treatment process of stainless steel chemical pigmentation aging liquid as claimed in claim 1, it is characterized in that the processing condition that electrolytic oxidation is handled are: the diluent with trivalent chromium solutions is made anolyte; Sulphuric acid soln with 5%～30% is made catholyte; Temperature is 40 ℃～80 ℃, anodic current density 150～350A/m
2, the treatment time is looked Cr in the anolyte
3+Amount and annode area and deciding.
6. the treatment process of stainless steel chemical pigmentation aging liquid as claimed in claim 1 is characterized in that the anolyte after electrolytic oxidation is handled can be directly used in the preparation of new coloring liquid; Catholyte after electrolytic oxidation is handled can circulate and be used to prepare new anolyte, Ni in catholyte
2+Concentration when higher, further reclaim nickel.
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| CNB2007100620165A CN100497735C (en) | 2007-05-24 | 2007-05-24 | Method of treating stainless steel chemical pigmentation aging liquid |
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| CN101892509A (en) * | 2010-07-08 | 2010-11-24 | 无锡出新环保设备有限公司 | Treatment device of chromium aging liquid |
| CN104087938A (en) * | 2014-06-18 | 2014-10-08 | 京东方科技集团股份有限公司 | Etching-liquid storing apparatus and wet-method etching equipment |
| CN109265333B (en) * | 2018-11-20 | 2021-09-07 | 四川省银河化学股份有限公司 | Preparation method of beta-menadione |
| CN112108086B (en) * | 2020-09-24 | 2022-06-21 | 上海理工大学 | Directional solidification segregation device and method for colloidal particle system |
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Non-Patent Citations (2)
| Title |
|---|
| 铝染色和封闭液老化和再生. 潘志信.电镀与环保，第15卷第1期. 1995 |
| 铝染色和封闭液老化和再生. 潘志信.电镀与环保，第15卷第1期. 1995 * |
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Assignee: Qingyuan Qingshan Stainless Steel Co., Ltd. Assignor: Taiyuan University of Technology Contract fulfillment period: 2009.10.20 to 2014.11.20 contract change Contract record no.: 2009440001882 Denomination of invention: Method of treating stainless steel chemical pigmentation aging liquid Granted publication date: 20090610 License type: Exclusive license Record date: 20091211 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.10.20 TO 2014.11.20; CHANGE OF CONTRACT Name of requester: QINGYUAN QINGSHAN STAINLESS STEEL CO., LTD. Effective date: 20091211 |
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