CN109628753A - A kind of method of alkaline etching waste liquid for producing production Kocide SD - Google Patents
A kind of method of alkaline etching waste liquid for producing production Kocide SD Download PDFInfo
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- CN109628753A CN109628753A CN201811651131.0A CN201811651131A CN109628753A CN 109628753 A CN109628753 A CN 109628753A CN 201811651131 A CN201811651131 A CN 201811651131A CN 109628753 A CN109628753 A CN 109628753A
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- China
- Prior art keywords
- kocide
- waste liquid
- etching waste
- alkaline etching
- alkaline
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0093—Treating solutions by chemical methods by gases, e.g. hydrogen or hydrogen sulfide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a kind of methods of alkaline etching waste liquid for producing production Kocide SD, the method of alkaline etching waste liquid for producing production Kocide SD be utilized cupric ammine complex react with liquid alkaline can release the free ammonia of this reaction of free ammonia removal after filtered and rinsed and finished product is made in drying and other steps, it is characteristic of the invention that it is less to add reactive material in the alkaline etching waste liquid for producing, final finished purity is higher, and stability is good.It is precipitated by the above-mentioned means, the present invention effectively can convert the Cu2+ in the alkaline etching waste liquid for producing to crystallize after Kocide SD, improves the level of resources utilization.
Description
Technical field
The present invention relates to resource reclaim fields, more particularly to a kind of method of alkaline etching waste liquid for producing production Kocide SD.
Background technique
With the fast development of electronics industry, China has become the maximum printed circuit board production base of the global output value.Erosion
Quarter is an important step in printed circuit board production process, and in process of production, the copper ion concentration in etching solution is more next
It is higher, need more to bring etching solution the higher etching speed of guarantee, this creates the terminal a large amount of erosions for being rich in copper ion
Carve waste liquid.Wherein etching waste liquor has acidic etching waste liquid and two kinds of alkaline etching waste liquid for producing, wherein alkaline etching waste liquid for producing main component
For cupric ammine complex and ammonium chloride etc., the main component of acidic etching waste liquid is copper chloride and hydrochloric acid etc..In annual etching waste liquor
Recyclable amount of copper is up to 200,000 tons, has great significance to the copper recycling and reusing in etching waste liquor.
Summary of the invention
The invention mainly solves the technical problem of providing a kind of alkaline etching waste liquid for producing recoverying and utilizing methods, can recycle benefit
With the copper in etching waste liquor.
In order to solve the above technical problems, one technical scheme adopted by the invention is that: it is raw to provide a kind of alkaline etching waste liquid for producing
The method for producing Kocide SD, the method for alkaline etching waste liquid for producing production Kocide SD the following steps are included:
Step 1 quantitative alkaline etching waste liquid for producing is added in quantitative reaction container,
Step 2 liquid alkaline is slowly added to it is in solution and evenly dispersed,
Step 3 uses blow-off method to remove the free ammonia in system under alkaline condition, 3 ~ 4h of stripping time,
Step 4 rinses 3 times to except the solution after ammonia, is isolated Kocide SD from solution using filter plant after rinsing
Come,
Step 5 uses room temperature or the dry Kocide SD of low temperature drying mode,
Product after step 6 is dry is stored as finished product packing.
In a preferred embodiment of the present invention, the amount of the liquid alkaline addition is determined by solution pH value, the solution pH value
It is 11 ~ 13.
In a preferred embodiment of the present invention, organic composite denitrifier is added while liquid alkaline is added in the step 2,
The pH value that solution after the organic composite denitrifier is added is 9 ~ 11.
In a preferred embodiment of the present invention, the organic composite denitrifier is by ethyl acetate, amide, propenyl, second
It mixes for two or three in acetoacetic ester, isobutyl-benzene and ethylene oxide.
In a preferred embodiment of the present invention, solution temperature is maintained at 40 ~ 55 DEG C when the step three stripping.
In a preferred embodiment of the present invention, the rinsing times of the step 4 are 3 times, wherein rinsing uses for the first time
Washing lotion be that second and third road rinse filtered recirculated water.
In a preferred embodiment of the present invention, the filter plant that the step 4 uses is that high speed centrifugation dry filter is set
It is standby.
In a preferred embodiment of the present invention, in the step 5 Kocide SD drying means be vacuum drying or
Freeze-drying.
The beneficial effects of the present invention are: the present invention devises alkali by comprehensively considering the composition characteristic of alkaline etching waste liquid for producing
Property etching waste liquor deamination and the method that is converted to Kocide SD, entire processing step is clearly quick, reaction process addition it is anti-
Answer substance less, ammonia removal efficiency is high, and final finished purity is high has stronger stability, and the Cu2+ ion in the solution turns
Precipitation is crystallized after turning to Kocide SD, the target of resource recycling is realized, reduces the pressure of environmental protection.
Detailed description of the invention
Fig. 1 is the flow diagram of a preferred embodiment of the present invention.
Specific embodiment
The preferred embodiments of the present invention will be described in detail with reference to the accompanying drawing, so that advantages and features of the invention energy
It is easier to be readily appreciated by one skilled in the art, so as to make a clearer definition of the protection scope of the present invention.
Main thought of the invention is that cuprammonium network is utilized using the method for alkaline etching waste liquid for producing production Kocide SD
Conjunction object is reacted with liquid alkaline can release this response characteristic of free ammonia design production line, and the reaction that the production method uses is public
Formula is as follows: [Cu (NH3)4]Cl2+2NaOH Cu(OH)2+4 NH3 + 2Na Cl
Rear attached process route chart is please referred to, a preferred embodiment of the present invention includes:
A kind of method of alkaline etching waste liquid for producing production Kocide SD, the method for the alkaline etching waste liquid for producing production Kocide SD include
Following steps:
Step 1 quantitative alkaline etching waste liquid for producing is added in quantitative reaction container,
Step 2 by liquid alkaline be slowly added to be easy in and it is evenly dispersed,
Step 3 uses blow-off method to remove the free ammonia in system under alkaline condition, 3 ~ 4h of stripping time,
Step 4 rinses 3 times to except the solution after ammonia, is isolated Kocide SD from solution using filter plant after rinsing
Come,
Step 5 uses room temperature or the dry Kocide SD of low temperature drying mode,
Product after step 6 is dry is stored as finished product packing.
The amount that the liquid alkaline is added is determined that the solution pH value is 11 ~ 13, the deamination under this alkaline condition by solution pH value
Efficiency is higher, can 3h or so by be more than in blow-off method removal system 97% free ammonia.
Solution temperature is maintained at 40 ~ 55 DEG C when described step three stripping, at this temperature in solution free ammonia activity compared with
By force, it is easy in conjunction with the gas for entering liquid phase, is rapidly separated solution.
The rinsing times of the step 4 are 3 times, wherein rinsing the washing lotion used for the first time is that second and third road float
Filtered recirculated water is washed, the first time rinsing is thickness, and second and third road are fine purifiation, the second and third road
Washing lotion through circulating line be collected into circulation water collection tank in after through filtering precipitate removal major impurity water quality can achieve first
Road cleans water quality requirement, this mode can save a large amount of water resource, improves productivity effect.
The filter plant that the step 4 uses is high speed centrifugation dry filter equipment, the centrifugation of the high speed centrifugation equipment
The rate of filtration is 800 ~ 1200r/min, can be removed the major liquid component on crystal under this speed, and later process is reduced
Tonnage.
The drying means of Kocide SD is vacuum drying or freeze-drying in the step 5, because of this society of Kocide SD
It is easy to decompose, so the method that cannot use high temperature drying, when heated-air drying, which is also easy to produce heat accumulation, leads to Kocide SD
It decomposes, can quickly remove excessive moisture using boulton process to avoid disadvantage mentioned above, reduce the generation of copper oxide, improve and produce
The purity of product.
Please refer to appended process route chart, in another preferred embodiment of the invention:
A kind of method of alkaline etching waste liquid for producing production Kocide SD, the method for the alkaline etching waste liquid for producing production Kocide SD include
Following steps:
Step 1 quantitative alkaline etching waste liquid for producing is added in quantitative reaction container,
Step 2 liquid alkaline is slowly added to it is in solution and evenly dispersed,
Step 3 uses blow-off method to remove the free ammonia in system under alkaline condition, 3 ~ 4h of stripping time,
Step 4 rinses 3 times to except the solution after ammonia, is isolated Kocide SD from solution using filter plant after rinsing
Come,
Step 5 uses room temperature or the dry Kocide SD of low temperature drying mode,
Product after step 6 is dry is stored as finished product packing.
Organic composite denitrifier is added while liquid alkaline is added in the step 2, and the organic composite denitrifier of addition can have
Imitating reduces the energy level that free ammonia is detached from from liquid phase, reduction disengaging condition, the ammonia removal efficiency in the raising unit time, described in addition
The best denitrogenation pH range of solution is 9 ~ 11 after organic composite denitrifier, and denitrification effect can achieve 99% or more in 3 ~ 4h, institute
Organic composite denitrifier is stated to be mixed by ethyl acetate, propenyl and acetoacetic ester.
Solution temperature is maintained at 40 ~ 55 DEG C when described step three stripping, at this temperature in solution free ammonia activity compared with
By force, it is easy in conjunction with the gas for entering liquid phase, is rapidly separated solution.
The rinsing times of the step 4 are 3 times, wherein rinsing the washing lotion used for the first time is that second and third road float
Filtered recirculated water is washed, the first time rinsing is thickness, and second and third road are fine purifiation, the second and third road
Washing lotion through circulating line be collected into circulation water collection tank in after through filtering precipitate removal major impurity water quality can achieve first
Road cleans water quality requirement, this mode can save a large amount of water resource, improves productivity effect.
The filter plant that the step 4 uses is high speed centrifugation dry filter equipment, the centrifugation of the high speed centrifugation equipment
The rate of filtration is 800 ~ 1200r/min, can be removed the major liquid component on crystal under this speed, and later process is reduced
Tonnage.
The drying means of Kocide SD is vacuum drying or freeze-drying in the step 5, because of this society of Kocide SD
It is easy to decompose, so the method that cannot use high temperature drying, when heated-air drying, which is also easy to produce heat accumulation, leads to Kocide SD
It decomposes, obtained nanoscale hydrogen-oxygen can also can be further processed on this basis to avoid disadvantage mentioned above using freeze-drying
Change the products such as copper.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field, is included within the scope of the present invention.
Claims (8)
1. a kind of method of alkaline etching waste liquid for producing production Kocide SD, which is characterized in that the alkaline etching waste liquid for producing produces hydrogen-oxygen
Change copper method the following steps are included:
Step 1 quantitative alkaline etching waste liquid for producing is added in quantitative reaction container,
Step 2 liquid alkaline is slowly added to it is in solution and evenly dispersed,
Step 3 uses blow-off method to remove the free ammonia in system under alkaline condition, 3 ~ 4h of stripping time,
Step 4 rinses 3 times to except the solution after ammonia, is isolated Kocide SD from solution using filter plant after rinsing
Come,
Step 5 uses room temperature or the dry Kocide SD of low temperature drying mode,
Product after step 6 is dry is stored as finished product packing.
2. the method for alkaline etching waste liquid for producing production Kocide SD according to claim 1, which is characterized in that the liquid alkaline adds
The amount entered is determined that the solution pH value is 11 ~ 13 by solution pH value.
3. the method for alkaline etching waste liquid for producing production Kocide SD according to claim 1, which is characterized in that the step 2
Organic composite denitrifier is added while liquid alkaline is added, the pH value that solution after the organic composite denitrifier is added is 9 ~ 11.
4. the method for alkaline etching waste liquid for producing production Kocide SD according to claim 3, which is characterized in that described organic multiple
Denitrifier is closed by two or three of mixing in ethyl acetate, amide, propenyl, ethyl acetate, isobutyl-benzene and ethylene oxide
It forms.
5. the method for alkaline etching waste liquid for producing production Kocide SD according to claim 1, which is characterized in that the step
Solution temperature is maintained at 40 ~ 55 DEG C when three strippings.
6. the method for alkaline etching waste liquid for producing production Kocide SD according to claim 1, which is characterized in that the step 4
Rinsing times be 3 times, wherein rinse the washing lotion that uses for the first time is second and the filtered recirculated water of third road rinsing.
7. the method for alkaline etching waste liquid for producing production Kocide SD according to claim 1, which is characterized in that the step 4
The filter plant used is high speed centrifugation dry filter equipment.
8. the method for alkaline etching waste liquid for producing production Kocide SD according to claim 1, which is characterized in that the step 5
The drying means of middle Kocide SD is vacuum drying or freeze-drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811651131.0A CN109628753A (en) | 2018-12-31 | 2018-12-31 | A kind of method of alkaline etching waste liquid for producing production Kocide SD |
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| CN201811651131.0A CN109628753A (en) | 2018-12-31 | 2018-12-31 | A kind of method of alkaline etching waste liquid for producing production Kocide SD |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111333219A (en) * | 2020-03-11 | 2020-06-26 | 深圳清华大学研究院 | Online purification and recycling method of PCB washing wastewater |
| CN114853053A (en) * | 2022-06-15 | 2022-08-05 | 云南润久科技有限公司 | High-purity copper hydroxide and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3204815A1 (en) * | 1982-02-11 | 1983-08-25 | Dieter 5650 Solingen Klein | Process for regenerating alkaline etchants for copper |
| CN101428889A (en) * | 2008-11-28 | 2009-05-13 | 江苏工业学院 | Treatment method for removing ammonia nitrogen from wastewater |
| CN103145206A (en) * | 2013-03-29 | 2013-06-12 | 广州氨氮水污染治理有限公司 | Composite nitrogen-removal medicament |
| CN103466683A (en) * | 2013-09-12 | 2013-12-25 | 昆山德阳新材料科技有限公司 | Preparation method of high-purity electroplating-grade copper oxide |
| CN103601349A (en) * | 2013-12-09 | 2014-02-26 | 沈阳铝镁设计研究院有限公司 | Method for denitrifying urea chemical wastewater |
| CN103952704A (en) * | 2014-04-02 | 2014-07-30 | 西安交通大学 | System and method for preparing copper sulphate solution by using acidic and alkalescence etching waste liquid |
-
2018
- 2018-12-31 CN CN201811651131.0A patent/CN109628753A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3204815A1 (en) * | 1982-02-11 | 1983-08-25 | Dieter 5650 Solingen Klein | Process for regenerating alkaline etchants for copper |
| CN101428889A (en) * | 2008-11-28 | 2009-05-13 | 江苏工业学院 | Treatment method for removing ammonia nitrogen from wastewater |
| CN103145206A (en) * | 2013-03-29 | 2013-06-12 | 广州氨氮水污染治理有限公司 | Composite nitrogen-removal medicament |
| CN103466683A (en) * | 2013-09-12 | 2013-12-25 | 昆山德阳新材料科技有限公司 | Preparation method of high-purity electroplating-grade copper oxide |
| CN103601349A (en) * | 2013-12-09 | 2014-02-26 | 沈阳铝镁设计研究院有限公司 | Method for denitrifying urea chemical wastewater |
| CN103952704A (en) * | 2014-04-02 | 2014-07-30 | 西安交通大学 | System and method for preparing copper sulphate solution by using acidic and alkalescence etching waste liquid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111333219A (en) * | 2020-03-11 | 2020-06-26 | 深圳清华大学研究院 | Online purification and recycling method of PCB washing wastewater |
| CN114853053A (en) * | 2022-06-15 | 2022-08-05 | 云南润久科技有限公司 | High-purity copper hydroxide and preparation method thereof |
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Application publication date: 20190416 |