CN115367831A - Equipment and process for recovering microetching liquid by freezing crystallization and application of equipment and process - Google Patents
Equipment and process for recovering microetching liquid by freezing crystallization and application of equipment and process Download PDFInfo
- Publication number
- CN115367831A CN115367831A CN202210905936.3A CN202210905936A CN115367831A CN 115367831 A CN115367831 A CN 115367831A CN 202210905936 A CN202210905936 A CN 202210905936A CN 115367831 A CN115367831 A CN 115367831A
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- China
- Prior art keywords
- liquid
- microetching
- freezing
- recovering
- cyclone
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- 239000007788 liquid Substances 0.000 title claims abstract description 120
- 230000008014 freezing Effects 0.000 title claims abstract description 61
- 238000007710 freezing Methods 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000002425 crystallisation Methods 0.000 title claims abstract description 26
- 230000008025 crystallization Effects 0.000 title claims abstract description 26
- 239000002699 waste material Substances 0.000 claims abstract description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims abstract description 15
- 238000011084 recovery Methods 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 12
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims abstract description 11
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000005457 ice water Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 8
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005530 etching Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000005192 partition Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 description 5
- 239000003814 drug Substances 0.000 description 4
- 239000011265 semifinished product Substances 0.000 description 4
- 238000004065 wastewater treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 239000010963 304 stainless steel Substances 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 150000004686 pentahydrates Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/22—Treatment of water, waste water, or sewage by freezing
Abstract
The invention discloses equipment, a process and application for recovering microetching liquid by freezing crystallization, wherein the process comprises the following specific flows: collecting microetching liquid, freezing and crystallizing, carrying out solid-liquid separation and recovering the microetching liquid. The copper sulfate pentahydrate is separated by the solubility characteristic of the components of the microetching solution by utilizing a freezing crystallization process. The equipment matched with the process comprises a waste liquid storage tank, a first centrifugal pump, a freezing kettle, a second centrifugal pump, a cyclone and a recovery liquid storage tank which are sequentially connected, wherein a coil pipe is arranged in the freezing kettle, ice water is filled in the coil pipe, the coil pipe is contacted with the waste liquid and cools the waste liquid, the solubility of anhydrous copper sulfate in the microetching liquid is greatly reduced after the anhydrous copper sulfate is cooled, crystals are formed, a solid-liquid mixture is obtained and then sent into the cyclone for solid-liquid separation, the main component of the crystals at the bottom is copper sulfate pentahydrate, and the main component of the solution at the top is sulfuric acid, sodium persulfate and a small amount of copper sulfate pentahydrate, namely the recovered microetching liquid. The equipment has simple connection mode and is suitable for large-scale treatment and recovery of the microetching liquid.
Description
Technical Field
The invention relates to the technical field of flexible circuit board production, in particular to equipment and process for recovering microetching liquid by freezing crystallization and application thereof.
Background
With the rapid development of the electronic industry, the quality requirement of electronic products on flexible circuit boards is higher and higher, and the demand is also higher and higher. In the FPC industry, the surface of the semi-finished product is often cleaned, and the surface of the semi-finished product is usually immersed in a chemical solution (microetching solution) or sprayed on the surface of the semi-finished product.
After the chemical liquid medicine is used for treating the semi-finished product, the service life is expired, the chemical liquid medicine is directly discharged to a wastewater treatment process, the wastewater treatment process is used for carrying out concentrated precipitation, filtration, pH adjustment and the like, and the chemical liquid medicine is discharged after meeting the environmental protection requirement, so that the waste of effective components in the chemical liquid medicine is caused, and the cost of wastewater treatment is increased.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a process for recovering microetching liquid by freezing crystallization, wherein the characteristic of component solubility in the microetching liquid is utilized, the frozen crystallization is adopted to crystallize copper sulfate pentahydrate in the microetching liquid, and sulfuric acid and sodium persulfate are recovered in a liquid form, so that the component loss of the microetching liquid is reduced, and the water treatment cost is reduced; the second purpose of the invention is to provide a device for recovering microetching liquid by freezing crystallization; the invention also aims to provide an application of the microetching liquid recovered by freezing crystallization, which aims at the recovery treatment of the microetching liquid.
One of the purposes of the invention is realized by adopting the following technical scheme:
a process for recovering microetching liquid by freezing crystallization comprises the following steps:
1) Collecting waste liquid of the micro-etching tank; the waste liquid is the microetching liquid with the expired service life, and comprises the following components: sodium persulfate, sulfuric acid, copper sulfate pentahydrate and water;
2) Freezing the waste liquid to 0-10 ℃ to obtain a solid-liquid mixture;
3) And (3) carrying out solid-liquid separation on the solid-liquid mixture, discharging the crystals after the crystals are deposited at the bottom, and recovering the liquid at the top to obtain the recovered microetching liquid.
Further, in the step 1), when the mass percent of the anhydrous copper sulfate in the microetching solution is 3.5-30% of the total mass of the microetching solution, the service life of the microetching solution is expired, and the recovery step is carried out.
Further, in the step 2), the ice water in the freezing kettle is adopted for freezing and cooling to 0-10 ℃.
Further, in the step 3), the solid-liquid mixture is conveyed to a cyclone for solid-liquid separation.
Still further, the material of swirler is stainless steel, the thickness of the cask and the toper section of thick bamboo of swirler is 2 ~ 5mm, and the thickness of middle partition plate is 5 ~ 10mm.
Further, the flow rate of the cyclone is 10-30 m 3 /m。
The second purpose of the invention is realized by adopting the following technical scheme:
the device for recovering the microetching liquid by freezing crystallization comprises a waste liquid storage tank, a first centrifugal pump, a freezing kettle, a second centrifugal pump, a cyclone and a recovery liquid storage tank; the waste liquid storage tank is connected with the freezing kettle through a first centrifugal pump; the freezing kettle is connected with the swirler through a second centrifugal pump, a coil pipe is arranged in the freezing kettle, and ice water is filled in the coil pipe; the liquid outlet of the cyclone is connected with the recovery liquid storage tank.
Further, the freezing kettle comprises a stirring device and a thermometer, wherein the stirring device and the thermometer are arranged in the freezing kettle.
Still further, still include the third centrifugal pump, the third centrifugal pump is connected with the recycle liquid storage tank.
The third purpose of the invention is realized by adopting the following technical scheme:
the application of the process for recovering the microetching liquid by freezing crystallization is to recover the microetching liquid used in the process of producing the flexible circuit board.
Compared with the prior art, the invention has the beneficial effects that:
(1) The process for recovering the microetching liquid mainly utilizes freezing crystallization, and comprises the following specific processes: collecting microetching liquid, freezing and crystallizing, carrying out solid-liquid separation and recovering the microetching liquid. In the step of freezing and crystallizing, the solubility of anhydrous copper sulfate in the microetching solution is reduced along with the reduction of the temperature, and the solubility of the rest sodium persulfate and sulfuric acid is not changed too much along with the temperature, so when the temperature is reduced to be below 10 ℃, a large amount of blue vitriol is crystallized, the rest components are still remained in the solution, after solid-liquid separation, the crystals at the bottom are discharged after deposition, and the solution at the top is recovered. The waste of sulfuric acid and sodium persulfate is reduced, and the water treatment cost is reduced.
(2) The equipment matched with the process comprises a waste liquid storage tank, a first centrifugal pump, a freezing kettle, a second centrifugal pump, a cyclone and a recovery liquid storage tank which are sequentially connected, wherein a coil pipe is arranged in the freezing kettle, ice water is filled in the coil pipe, the coil pipe is contacted with the waste liquid and cools the waste liquid, the solubility of anhydrous copper sulfate in the microetching liquid is greatly reduced after the anhydrous copper sulfate is cooled, crystals are formed, a solid-liquid mixture is obtained and then sent into the cyclone for solid-liquid separation, the main component of the crystals at the bottom is copper sulfate pentahydrate, and the main component of the solution at the top is sulfuric acid, sodium persulfate and a small amount of copper sulfate pentahydrate, namely the recovered microetching liquid. The equipment has simple connection mode and is suitable for large-scale treatment and recovery of the microetching liquid.
Drawings
FIG. 1 is a connection diagram of the apparatus of the present invention;
in the figure: 1. a waste liquid storage tank; 2. a first centrifugal pump; 3. freezing the kettle; 31. a coil pipe; 32. a stirring device; 33. a thermometer; 34. a water chiller; 4. a second centrifugal pump; 5. a swirler; 6. a recovery liquid storage tank; 7. and a third centrifugal pump.
Detailed Description
The present invention is further described with reference to the accompanying drawings and the detailed description, and it should be noted that, in the case of no conflict, any combination between the embodiments or technical features described below may form a new embodiment.
Example 1
As shown in figure 1, the invention provides a device for recovering microetching liquid by freezing crystallization, which is used in the method as the process for recovering microetching liquid by freezing crystallization, and comprises a waste liquid storage tank 1, a first centrifugal pump 2, a freezing kettle 3, a second centrifugal pump 4, a cyclone 5, a recovery liquid storage tank 6 and a third centrifugal pump 7; the waste liquid storage tank 1 is connected with a freezing kettle 3 through a first centrifugal pump 2; the freezing kettle 3 is connected with the cyclone 5 through the second centrifugal pump 4, a coil pipe 31 is arranged in the freezing kettle 3, ice water is filled in the coil pipe 31 and comes from an ice water machine 34, a stirring device 32 is also arranged in the freezing kettle 3, the stirring device 32 is connected with a speed reducer and used for controlling the stirring speed, and a thermometer 33 is used for monitoring the temperature of liquid in the freezing kettle 3; the liquid outlet of cyclone 5 is connected to a recycle liquid sump 6. The recovery liquid storage tank 6 is connected with the micro-etching tank through a third centrifugal pump 7.
The material of swirler 5 is 304 stainless steel, the thickness of the cask and the cone of swirler 5 is 3mm, and the thickness of the middle partition plate is 8mm. The flow rate of the cyclone 5 is 20m 3 /m。
A process for recovering microetching liquid by freezing crystallization comprises the following steps:
1) Collecting the waste liquid of the micro-etching tank, and storing the waste liquid in a waste liquid storage tank 1; the waste liquid is the microetching liquid with the expired service life, and comprises the following components in percentage by mass: 10 percent of sodium persulfate, 5.5 percent of sulfuric acid, 3.5 percent of copper sulfate pentahydrate and the balance of water; wherein the mass concentration of the sulfuric acid is 3%, the content of copper sulfate pentahydrate is 35g/L, and the content of sodium persulfate is 100g/L;
2) Conveying the waste liquid from a waste liquid storage tank 1 to a freezing kettle 3 through a first centrifugal pump 2, freezing and cooling the waste liquid to 10 ℃ through ice water in a coil 31 by the freezing kettle 3, stirring the waste liquid under the drive of a stirring device 32, and ensuring that the internal temperature of the freezing kettle 3 is lower than 10 ℃ through 33 degrees of a thermometer to obtain a solid-liquid mixture;
3) And conveying the solid-liquid mixture to a cyclone 5 through a second centrifugal pump 4, carrying out solid-liquid separation, discharging the crystal deposited at the bottom to a collecting tank, and recovering and storing the liquid at the top in a recovered liquid storage tank 6.
Wherein the deposited crystals are copper sulfate pentahydrate, and the components of the liquid at the top are verified as follows: 3 percent of sulfuric acid, 100g/L of sodium persulfate and 23g/L of copper sulfate pentahydrate.
The specific principle of the invention is according to the solubility of each component in the microetching solution, which is specifically shown in the table 1.
TABLE 1 solubility of various components of the microetching solution at different temperatures
The operating temperature of the microetching solution is known to be 35 to 40 ℃, and as can be seen from table 1, the microetching solution is collected intensively and then cooled in a freezing kettle 3 by an ice water freezing mode, when the temperature of the solution is reduced to 10 ℃, the solubility of the copper sulfate pentahydrate is reduced to 23.1g, and about 12g of the copper sulfate pentahydrate is crystallized and precipitated. The content of the recovered microetching liquid pentahydrate and copper sulfate is not over standard any more and can be recycled. The process and the equipment can reduce the discharge of the microetching liquid, reduce the waste of sulfuric acid and sodium persulfate and reduce the water treatment cost.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. A process for recovering microetching liquid by freezing crystallization is characterized by comprising the following steps:
1) Collecting waste liquid of the micro-etching tank; the waste liquid is the microetching liquid with the expired service life, and comprises the following components: sodium persulfate, sulfuric acid, copper sulfate pentahydrate and water;
2) Freezing the waste liquid to 0-10 ℃ to obtain a solid-liquid mixture;
3) And (3) carrying out solid-liquid separation on the solid-liquid mixture, discharging the crystals after the crystals are deposited at the bottom, and recovering the liquid at the top to obtain the recovered microetching liquid.
2. The process for recovering microetching liquid by means of freeze crystallization according to claim 1, wherein in the step 1), when the mass percentage of the anhydrous copper sulfate in the microetching liquid is 3.5 to 30% of the total mass of the microetching liquid, the life of the microetching liquid is expired, and the recovery step is performed.
3. The process for recovering microetching liquid by freezing crystallization as claimed in claim 1, wherein in the step 2), ice water in a freezing kettle is adopted for freezing and cooling to 0-10 ℃.
4. The process for recovering microetching liquid by freezing crystallization according to claim 1, wherein in the step 3), the solid-liquid mixture is conveyed to a cyclone for solid-liquid separation.
5. The process for recovering microetching liquid by freezing crystallization according to claim 4, wherein the cyclone is made of stainless steel, the thickness of the cylindrical barrel and the conical barrel of the cyclone is 2-5 mm, and the thickness of the middle partition plate is 5-10 mm.
6. The process for recovering microetching liquid by freezing crystallization according to claim 4, wherein the flow rate of the cyclone is 10 to 30m 3 /m。
7. An apparatus for recovering microetching liquid by freezing crystallization, which is characterized in that the use method of the apparatus is the process for recovering the microetching liquid by freezing crystallization as claimed in any one of claims 1 to 6, and comprises a waste liquid storage tank, a first centrifugal pump, a freezing kettle, a second centrifugal pump, a cyclone and a recovery liquid storage tank; the waste liquid storage tank is connected with the freezing kettle through a first centrifugal pump; the freezing kettle is connected with the swirler through a second centrifugal pump, a coil pipe is arranged in the freezing kettle, and ice water is filled in the coil pipe; the liquid outlet of the cyclone is connected with the recovery liquid storage tank.
8. The apparatus for recovering microetching liquid by freezing crystallization according to claim 7, wherein said apparatus further comprises a stirring device and a thermometer, and wherein said stirring device and said thermometer are disposed in said freezing tank.
9. The apparatus for recovering microetch solution from frozen crystals as claimed in claim 7, wherein said apparatus further comprises a third centrifugal pump connected to said recovery solution storage tank.
10. The use of the process for recovering microetching solution by freezing crystallization as claimed in any one of claims 1 to 6, wherein the process is used for recovering microetching solution used in the production of flexible circuit boards.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210905936.3A CN115367831A (en) | 2022-07-29 | 2022-07-29 | Equipment and process for recovering microetching liquid by freezing crystallization and application of equipment and process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210905936.3A CN115367831A (en) | 2022-07-29 | 2022-07-29 | Equipment and process for recovering microetching liquid by freezing crystallization and application of equipment and process |
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| Publication Number | Publication Date |
|---|---|
| CN115367831A true CN115367831A (en) | 2022-11-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210905936.3A Pending CN115367831A (en) | 2022-07-29 | 2022-07-29 | Equipment and process for recovering microetching liquid by freezing crystallization and application of equipment and process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115367831A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004359989A (en) * | 2003-06-03 | 2004-12-24 | Nittetsu Mining Co Ltd | Method for regenerating copper-etching waste liquid |
| CN103435092A (en) * | 2013-09-01 | 2013-12-11 | 深圳市危险废物处理站有限公司 | Resource recovery method of sodium persulfate-sulfuric acid serial copper-containing microetch waste liquor for PCB (Printed Circuit Board) |
| CN210529064U (en) * | 2019-08-27 | 2020-05-15 | 深圳市祺鑫天正环保科技有限公司 | Microetching liquid copper recovery circulating device and circuit board microetching equipment |
-
2022
- 2022-07-29 CN CN202210905936.3A patent/CN115367831A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004359989A (en) * | 2003-06-03 | 2004-12-24 | Nittetsu Mining Co Ltd | Method for regenerating copper-etching waste liquid |
| CN103435092A (en) * | 2013-09-01 | 2013-12-11 | 深圳市危险废物处理站有限公司 | Resource recovery method of sodium persulfate-sulfuric acid serial copper-containing microetch waste liquor for PCB (Printed Circuit Board) |
| CN210529064U (en) * | 2019-08-27 | 2020-05-15 | 深圳市祺鑫天正环保科技有限公司 | Microetching liquid copper recovery circulating device and circuit board microetching equipment |
Non-Patent Citations (1)
| Title |
|---|
| 天津化工研究院等, 化学工业出版社 * |
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Application publication date: 20221122 |