CN101935121A - Process for recycling alkali waste etching liquid - Google Patents
Process for recycling alkali waste etching liquid Download PDFInfo
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- CN101935121A CN101935121A CN 201010269561 CN201010269561A CN101935121A CN 101935121 A CN101935121 A CN 101935121A CN 201010269561 CN201010269561 CN 201010269561 CN 201010269561 A CN201010269561 A CN 201010269561A CN 101935121 A CN101935121 A CN 101935121A
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Abstract
The invention discloses a process for recycling alkali waste etching liquid. The process comprises the following steps of: acidizing and regulating the pH value; separating solid and liquid; purifying and converting; and recycling supernatant liquid. By adopting the process for recycling the waste alkali etching liquid, copper ions in the waste alkali etching liquid can be recovered, and the supernatant liquid can be recycled; the process has zero waste water discharge, thereby reducing the production cost of enterprises; and the waste liquid can be utilized 100 percent to guarantee no pollution.
Description
Technical field
The present invention relates to a kind of waste liquor recovery process, particularly a kind of circulation and recovery process that is used for alkaline etching waste liquid for producing.
Background technology
PCB production has formed industrial scale in China at present, and annual production reaches 200,000,000 m
2, PCB production produces a large amount of etching solutions, and the PCB etching solution mainly contains alkaline etching liquid, acidic etching liquid, and annual etching waste liquor cupric total amount is about 50,000 tons.These etching solutions have characteristics such as kind is many, toxicity is big, corrodibility is strong, belong to a national class Hazardous wastes, just do not handle discharging arbitrarily if add, to produce very serious destruction to ecology, even serious threat is to people's life security, a large amount of waste liquids also can cause the pollution of great lot of water resources as not carrying out efficient recovery.
The main method that etching solution is reclaimed has evaporating, concentrating and crystallizing method, the direct neutralisation of spent acid alkaline etching liquid and extraction-acid copper method etc. at present, but all there are various defectives in various degree in these methods at present.As Chinese invention patent, application number 91100122.0 and 200710030323.5 all adopts directly with acidic etching liquid and alkaline etching liquid neutralisation, and this method only relates to copper and reclaims, and waste liquid can't use in recirculation.Its method is to obtain mantoquita precipitation etc. by alkaline etching liquid and is neutralized to twice liquid at acid quarter, the mantoquita that is reclaimed is the chlorination cuprammonium, but adopt the mantoquita post precipitation in this method etching solution, these upper strata waste liquids are because of in the spent acid etching solution, contain the sodium salt (oxygenant is brought into) of a large amount of accumulations, so be difficult to carry out cycling and reutilization.And its upper strata waste liquid contains tens thousand of PPM ammonia nitrogens; thousands of PPM copper; if the organism of tens of PPM can't reuse the time, will seriously increase client's waste water burden; because when the upper strata waste liquor contamination is seriously handled; processing costs is surprising, and enterprise's production cost can't be reduced, and has increased the weight of the burden of enterprise; more seriously this upper strata waste liquid uses present state-of-the-art treatment technology, and also intractable is qualified, causes very big hidden danger to environment protection.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the technical problem to be solved in the present invention provides a kind of complete recycle of high density etching waste liquor that makes, and can reach zero disposal of pollutants, meet the alkaline etching waste liquid for producing circulation and recovery process of environmental protection policy and cleaner production condition.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of alkaline etching waste liquid for producing circulation and recovery process, it comprises the steps:
A) acidifying, PH adjust, and add hydrochloric acid and sinking agent in the alkalitropism etching solution, adjust pH value, make the mantoquita sedimentation in the alkaline etching liquid;
B) solid-liquid separation adopts mechanical type method separate solid mantoquita, obtains supernatant liquid;
C) purifying, the transformation of ownership are carried out purifying, the transformation of ownership with the solid mantoquita after separating, and make basic copper chloride or cupric oxide;
D) metallic impurity and organism in the supernatant liquid are removed in supernatant liquid reuse, analyze the composition that lacks in the supernatant liquid, add corresponding etching additive, send etching line cocycle utilization back to.
Preferably, in step b), after solid copper salt separates, need in the liquid of upper strata, to add purifying agent or remove other metallic pollutions, and after activated carbon filtration, secondary filter, can obtain supernatant liquid through methods such as Solid-Phase Extraction.
Preferably, the setting range of pH value is 4.0-6.0 in step a), and optimum value is 5.5-6.0.
Technique scheme has following beneficial effect: adopt this alkaline etching waste liquid for producing circulation and recovery process that the cupric ion in the alkaline etching liquid is recovered, and and its upper strata liquid is recycled, non-wastewater discharge, effectively reduced the processing costs of enterprise wastewater, reduced the production cost of enterprise, and can make waste liquid obtain hundred-percent utilization, guarantee without any pollution, reach the overall circulation economy that waste liquid and mantoquita can both re-use
Above-mentioned explanation only is the general introduction of technical solution of the present invention, for can clearer understanding technique means of the present invention, and can be implemented according to the content of specification sheets, below with preferred embodiment of the present invention and conjunction with figs. describe in detail as after.The specific embodiment of the present invention is provided in detail by following examples and accompanying drawing thereof.
Description of drawings
Fig. 1 is the schema of the embodiment of the invention.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
As shown in Figure 1, be process flow sheet of the present invention, this alkaline etching waste liquid for producing circulation and recovery process comprises the steps:
A) acidifying, PH adjust, and add hydrochloric acid and sinking agent in the alkalitropism etching solution, adjust pH value and make the interior mantoquita sedimentation of alkaline etching liquid; The setting range of pH value is 4.0-6.0.PH value is between 5.5-6.0 the time, and the muriate of generation (duplex grain structure of cupric chloride and ammonium chloride) is purer, helps making more rare basic copper chloride.
B) solid-liquid separation adopts mechanical type method separate solid mantoquita, adds purifying agent in the upper strata liquid after separating or removes other metallic pollutions through methods such as Solid-Phase Extraction, and obtain supernatant liquid after activated carbon filtration, secondary filter;
C) purifying, the transformation of ownership are carried out purifying, the transformation of ownership with the solid mantoquita after separating, and make environment-friendly feed additive basic copper chloride or purposes cupric oxide very widely.
D) metallic impurity and organism in the supernatant liquid are removed in supernatant liquid reuse, analyze the composition that lacks in the supernatant liquid, add corresponding etching additive, return etching line cocycle utilization.
Adopt this alkaline etching waste liquid for producing circulation and recovery process that the cupric ion in the alkaline etching liquid is recovered, and its upper strata liquid is recycled, therefore can carry out recycle inside, save freight charges, waste liquid can obtain hundred-percent utilization, guarantee without any pollution, effectively reduced the processing costs of enterprise wastewater, reduced the production cost of enterprise.
This technical process upper strata waste liquid is capable of circulation to be utilized again, so present technique can solve the ammonia and nitrogen pollution problem of high-concentration waste liquid, so can eliminate main one of the generation source of present stage China's ammonia and nitrogen pollution.This technical scheme meets cleaner production and recycling economy principle, can solve the printed circuit board (PCB) industry serious ammonia and nitrogen pollution problem that alkaline etching waste liquid for producing caused effectively, meets Green Product Design, guarantees the industry Sustainable development.
More than a kind of alkaline etching waste liquid for producing circulation and recovery process that the embodiment of the invention provided is described in detail; for one of ordinary skill in the art; thought according to the embodiment of the invention; part in specific embodiments and applications all can change; in sum; this description should not be construed as limitation of the present invention, and all any changes of making according to design philosophy of the present invention are all within protection scope of the present invention.
Claims (3)
1. an alkaline etching waste liquid for producing circulation and recovery process is characterized in that it comprises the steps:
A) acidifying, PH adjust, and add hydrochloric acid and sinking agent in the alkalitropism etching solution, adjust pH value, make the mantoquita sedimentation in the alkaline etching liquid;
B) solid-liquid separation adopts mechanical type method separate solid mantoquita, obtains supernatant liquid;
C) purifying, the transformation of ownership are carried out purifying, the transformation of ownership with the solid mantoquita after separating, and make basic copper chloride or cupric oxide;
D) organism and metallic impurity in the supernatant liquid are removed in supernatant liquid reuse, analyze the composition that lacks in the supernatant liquid, add corresponding etching additive, send etching line cocycle utilization back to.
2. alkaline etching waste liquid for producing circulation and recovery process according to claim 1 is characterized in that, in step b), after solid copper salt separates, needs to add purifying agent and can obtain supernatant liquid in the liquid of upper strata after activated carbon filtration, secondary filter.
3. alkaline etching waste liquid for producing circulation and recovery process according to claim 1 is characterized in that, the setting range of pH value is 4.0-6.0 in step a), and optimum value is 5.5-6.0.
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CN 201010269561 CN101935121A (en) | 2010-09-02 | 2010-09-02 | Process for recycling alkali waste etching liquid |
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CN 201010269561 CN101935121A (en) | 2010-09-02 | 2010-09-02 | Process for recycling alkali waste etching liquid |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102502998A (en) * | 2011-11-28 | 2012-06-20 | 昆山联鼎环保科技有限公司 | Totally enclosed type alkali etching liquid recycling process |
CN103253696A (en) * | 2013-05-14 | 2013-08-21 | 温州大学 | Method for recovering cuprous chloride from alkaline waste etching solution |
CN105002500A (en) * | 2015-07-17 | 2015-10-28 | 中南大学 | Alkaline CuC12 spent etching solution copper removal regeneration method |
CN106673048A (en) * | 2017-03-24 | 2017-05-17 | 东莞市广华化工有限公司 | Method for converting basic copper chloride into basic copper carbonate |
CN109095642A (en) * | 2018-08-30 | 2018-12-28 | 惠州大亚湾亿田环保技术有限公司 | A kind of alkalinity erosion copper waste liquid environmental protection recovery process of zero-emission |
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CN1156766A (en) * | 1996-02-03 | 1997-08-13 | 深圳市工业废物处理站 | Process for preparing regenerated alkaline etching supplementary liquid and device system thereof |
CN1445031A (en) * | 2002-03-15 | 2003-10-01 | 林裕城 | Recycling handles method for dirty mire containing heavy metals |
CN101215062A (en) * | 2007-12-26 | 2008-07-09 | 郝屿 | Method and system for reclaiming valuable resource in acidic etching waste liquid |
CN201381235Y (en) * | 2008-06-05 | 2010-01-13 | 徐毅 | System for cyclic regeneration of spent etching solution and recovery processing of copper |
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2010
- 2010-09-02 CN CN 201010269561 patent/CN101935121A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN1156766A (en) * | 1996-02-03 | 1997-08-13 | 深圳市工业废物处理站 | Process for preparing regenerated alkaline etching supplementary liquid and device system thereof |
CN1445031A (en) * | 2002-03-15 | 2003-10-01 | 林裕城 | Recycling handles method for dirty mire containing heavy metals |
CN101215062A (en) * | 2007-12-26 | 2008-07-09 | 郝屿 | Method and system for reclaiming valuable resource in acidic etching waste liquid |
CN201381235Y (en) * | 2008-06-05 | 2010-01-13 | 徐毅 | System for cyclic regeneration of spent etching solution and recovery processing of copper |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102502998A (en) * | 2011-11-28 | 2012-06-20 | 昆山联鼎环保科技有限公司 | Totally enclosed type alkali etching liquid recycling process |
CN103253696A (en) * | 2013-05-14 | 2013-08-21 | 温州大学 | Method for recovering cuprous chloride from alkaline waste etching solution |
CN105002500A (en) * | 2015-07-17 | 2015-10-28 | 中南大学 | Alkaline CuC12 spent etching solution copper removal regeneration method |
CN105002500B (en) * | 2015-07-17 | 2017-09-15 | 中南大学 | A kind of alkaline CuCl2Spent etching solution decopper(ing) renovation process |
CN106673048A (en) * | 2017-03-24 | 2017-05-17 | 东莞市广华化工有限公司 | Method for converting basic copper chloride into basic copper carbonate |
CN109095642A (en) * | 2018-08-30 | 2018-12-28 | 惠州大亚湾亿田环保技术有限公司 | A kind of alkalinity erosion copper waste liquid environmental protection recovery process of zero-emission |
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