CN110577290A - method and device for recycling development waste liquid - Google Patents
method and device for recycling development waste liquid Download PDFInfo
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- CN110577290A CN110577290A CN201810594412.0A CN201810594412A CN110577290A CN 110577290 A CN110577290 A CN 110577290A CN 201810594412 A CN201810594412 A CN 201810594412A CN 110577290 A CN110577290 A CN 110577290A
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- 239000007788 liquid Substances 0.000 title claims abstract description 100
- 239000002699 waste material Substances 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000004064 recycling Methods 0.000 title claims abstract description 30
- 239000012528 membrane Substances 0.000 claims abstract description 148
- 239000000919 ceramic Substances 0.000 claims abstract description 112
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 106
- 238000001728 nano-filtration Methods 0.000 claims abstract description 63
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 53
- 238000001914 filtration Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000108 ultra-filtration Methods 0.000 claims description 60
- 238000001471 micro-filtration Methods 0.000 claims description 36
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 18
- 238000005189 flocculation Methods 0.000 claims description 18
- 230000016615 flocculation Effects 0.000 claims description 18
- 230000000149 penetrating effect Effects 0.000 claims description 13
- 239000011148 porous material Substances 0.000 claims description 13
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 11
- 238000005842 biochemical reaction Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 9
- 239000002351 wastewater Substances 0.000 claims description 9
- 238000009295 crossflow filtration Methods 0.000 claims description 8
- 238000005273 aeration Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000011045 prefiltration Methods 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000000265 homogenisation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 abstract description 8
- 239000012071 phase Substances 0.000 description 11
- 239000000084 colloidal system Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000004907 flux Effects 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 229910052839 forsterite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- -1 liriopitotium Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a method and a device for recycling development waste liquid, in particular to a sodium carbonate recycling process for development stripping waste liquid in PCB production. Mainly comprises the following steps: A. sending the development waste liquid into a homogenizing tank to homogenize the water quality; B. and (3) roughly filtering the homogenized waste liquid to remove suspended matters C, sending the roughly filtered developing waste liquid into a ceramic nanofiltration membrane separation system, intercepting the ink to form a ceramic membrane concentrated solution, wherein the clear liquid of the ceramic membrane is a purified sodium carbonate solution and can be directly reused in the developing process. By adopting the process, the recovery rate of the sodium carbonate solution is more than 50%, the use efficiency of the sodium carbonate in the developing and stripping process is improved, the discharge amount of waste liquid in the developing and stripping process is reduced, and the process has great social and economic benefits.
Description
Technical Field
the invention belongs to the technical field of films, relates to a method and a device for recycling developing waste liquid, and more particularly relates to a process for recycling sodium carbonate from developing and stripping waste liquid in PCB production.
background
In the fields of Liquid Crystal Displays (LCDs), Printed Circuit Boards (PCBs), Integrated Circuits (ICs), and the like, development is one of the very important processes in the manufacturing process, and the development process is to remove the unexposed part of the photosensitive film by a chemical reaction method to expose the copper surface pattern circuit to be etched and removed. The developing waste liquid is usually a high-concentration alkaline waste liquid, and if the developing waste liquid is discharged randomly, the environment is polluted, and a great deal of resource waste is caused. At present, the mainstream methods for treating the developer waste liquid at home and abroad comprise an oxidation method, a biological treatment method, a filtration and adsorption method and the like. However, the above method does not realize recycling of the developer, and the investment and running costs are also large. Therefore, it is necessary to recover the sodium carbonate effective component in the developer and reduce the amount of wastewater discharge.
disclosure of Invention
The invention aims to provide a sodium carbonate recovery process for developing and stripping waste liquid in the production of the fields of Liquid Crystal Displays (LCDs), Printed Circuit Boards (PCBs), Integrated Circuits (ICs) and the like.
the technical scheme is as follows:
A method for recycling development waste liquid comprises the following steps:
Step 1, carrying out pre-filtration treatment on the development waste liquid;
and 2, filtering the filtrate obtained by pre-filtering by adopting a ceramic nanofiltration membrane, and obtaining a penetrating fluid containing sodium carbonate at the penetrating side of the ceramic nanofiltration membrane.
in one embodiment, the developing waste liquid contains 0.1 to 1wt% of sodium carbonate and 1000 to 50000ppm of COD.
In one embodiment, the pre-filtration in step 1 is a filtration treatment using a ceramic ultrafiltration or microfiltration membrane.
In one embodiment, the average pore size of the ceramic ultrafiltration or microfiltration membrane is in the range of 50 to 500 μm.
In one embodiment, before the step 1, the development waste liquid is subjected to homogenization treatment.
In one embodiment, the ceramic nanofiltration membrane in the step 2 has a molecular weight cut-off of 800-6000 Da.
In one embodiment, the operating pressure of the ceramic nanofiltration membrane is 0.1-1.5 MPa, a cross-flow filtration mode is adopted, and the membrane surface flow rate is 2-6 m/s.
in one embodiment, the ceramic nanofiltration membrane has a concentration factor of 2 to 10.
In one embodiment, before the step 1, ozone oxidation pretreatment is carried out on the development waste liquid; the addition amount of the ozone is 500-1000 ppm, and the reaction temperature is 40-70 ℃.
A recycling apparatus of a development waste liquid, comprising:
the homogenizing tank is used for carrying out homogenizing treatment on the developing waste liquid;
The aeration pipe is connected with the homogenizing tank and is used for aerating in the homogenizing tank;
the ceramic microfiltration membrane or the ceramic ultrafiltration membrane is connected with the homogenizing tank and is used for filtering the homogenized development waste liquid;
The ceramic nanofiltration membrane is connected to the permeation side of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane and is used for performing nanofiltration treatment on the penetrating fluid;
And the nanofiltration penetrating fluid storage tank is connected with the ceramic nanofiltration membrane and used for storing penetrating fluid containing sodium carbonate.
In one embodiment, the average pore size of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane is in the range of 50 to 500 μm.
In one embodiment, the ceramic nanofiltration membrane in the step 2 has a molecular weight cut-off of 800-6000 Da.
in one embodiment, further comprising: the flocculation tank is connected to the concentrated side of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane and is used for performing flocculation sedimentation treatment on the concentrated solution of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane; the flocculation tank is connected with a flocculant adding tank 7 for adding a flocculant into the flocculation tank; the water outlet of the flocculation tank is connected with the biochemical reaction unit.
In one embodiment, the biochemical reaction unit is an A2O biochemical reaction unit.
In one embodiment, the ozone oxidation device further comprises an ozone reactor connected to the wastewater inlet of the ceramic micro-filtration membrane or the ceramic ultrafiltration membrane and used for carrying out ozone oxidation treatment on the development wastewater entering the ceramic micro-filtration membrane or the ceramic ultrafiltration membrane.
Advantageous effects
According to the invention, the ceramic nanofiltration membrane is simple to operate, only is a physical separation process, has a certain interception capacity on ink, the clear liquid of the ceramic nanofiltration membrane can be used in a developing and de-filming process, the recycling proportion of waste sodium carbonate can be adjusted by adjusting the concentration multiple, the discharge amount of waste liquid is reduced, and the economic benefit and the environmental benefit are obvious.
Drawings
FIG. 1 is a flow chart of a process of the present invention;
Fig. 2 is a diagram of the apparatus employed.
Wherein, 1, homogenizing tank; 2. an aeration pipe; 3. a ceramic microfiltration membrane or a ceramic ultrafiltration membrane; 4. a ceramic nanofiltration membrane; 5. a flocculation tank; 6. a biochemical reaction unit; 7. a flocculant adding tank; 8. and (4) a nanofiltration penetrating fluid storage tank.
Detailed Description
The development waste liquid to be treated by the invention is mainly obtained in the development process in the fields of Liquid Crystal Displays (LCDs), Printed Circuit Boards (PCBs), Integrated Circuits (ICs) and the like, wherein the development liquid is mainly prepared from inorganic alkali (sodium carbonate), a surfactant, water and the like, and the conventional formula can be referred to in the prior art documents CN102063024A, CN103207544A, CN107340693A and the like. The developing waste liquid mainly contains inorganic alkali (sodium carbonate), surfactant, a large amount of high molecular polymers, resin, printing ink and the like brought by photoresist, and the water quality of the developing waste liquid is represented by high sodium carbonate content and high COD. In one embodiment, the developing waste liquid contains 0.1 to 1wt% of sodium carbonate and 1000 to 50000ppm of COD.
the invention provides a method for recycling and treating development waste liquid, which mainly comprises the following steps of A, sending the development waste liquid into a homogenizing tank to homogenize water quality; B. and (3) roughly filtering the homogenized waste liquid to remove suspended matters C, sending the roughly filtered developing waste liquid into a ceramic nanofiltration membrane separation system, intercepting the ink to form a ceramic membrane concentrated solution, wherein the clear liquid of the ceramic membrane is a purified sodium carbonate solution and can be directly reused in the developing process. By adopting the process, the recovery rate of the sodium carbonate solution is more than 50%, the use efficiency of the sodium carbonate in the developing and stripping process is improved, the discharge amount of waste liquid in the developing and stripping process is reduced, and the process has great social and economic benefits.
in the above process, the homogenized development waste liquid is treated by ceramic microfiltration or ultrafiltration membrane, so that large-particle resin, colloid, ink and the like in the waste liquid can be effectively removed, most of COD components can be reduced, and the filter membrane of the ceramic material used herein can show higher filtration flux and contamination resistance to the development waste liquid than the organic membrane. After large suspended matters, resin and colloid in the waste liquid are removed, the prefiltered filtrate is subjected to nanofiltration treatment by a ceramic nanofiltration membrane, so that small molecular impurities in the prefiltered filtrate can be effectively removed, and sodium carbonate can permeate the nanofiltration membrane to be recycled.
In the present invention, the ceramic microfiltration membrane, ultrafiltration membrane or nanofiltration membrane used is made of a ceramic material, and for example, an oxide material such as alumina, zirconia, magnesia, silica, titania, ceria, yttria or barium titanate; composite oxide materials such as cordierite, mullite, forsterite, steatite, sialon, zircon, ferrite and the like; nitride materials such as silicon nitride and aluminum nitride; carbide-based materials such as silicon carbide; hydroxide materials such as hydroxyapatite; elemental materials such as carbon and silicon; or an inorganic composite material containing two or more of them. Natural minerals (clay, clay minerals, liriopitotium, silica sand, pottery stone, feldspar, white sand) or blast furnace slag, fly ash, etc. may also be used. Among these, 1 or 2 or more kinds selected from alumina, zirconia, titania, magnesia and silica are preferable, and ceramic powder mainly composed of alumina, zirconia or titania is more preferable. When the microfiltration, ultrafiltration and nanofiltration membranes made of the ceramic materials are applied to the treatment of the development waste liquid, the microfiltration, ultrafiltration and nanofiltration membranes can show good pollution resistance to impurities such as resin, printing ink and the like in the waste liquid, and the flux in the filtration process is obviously superior to that of the filtration membranes made of organic materials.
The average pore diameter range of the micro-filtration or ultrafiltration membrane is 50-5000 nm.
As the nanofiltration membrane, since the pore diameter is too small to measure the pore diameter on the membrane surface with an electron microscope or the like, a value called a molecular weight cut-off is used as an index of the pore diameter size instead of the average pore diameter. As for the molecular weight cut-off, it is well known to those skilled in the art that "a curve obtained by plotting the data on the horizontal axis and the vertical axis of the solute molecular weight is referred to as a molecular weight cut-off curve". The molecular weight at which the rejection is 90% is also referred to as the molecular weight cut-off of the membrane, which is an index indicating the membrane performance of the nanofiltration membrane and is well known to those skilled in the art. And the intercepted molecular weight of the ceramic nanofiltration membrane in the step 2 is 800-6000 Da. In one embodiment, the operating pressure of the ceramic nanofiltration membrane is 0.1-1.5 MPa, a cross-flow filtration mode is adopted, and the membrane surface flow rate is 2-6 m/s. In one embodiment, the ceramic nanofiltration membrane has a concentration factor of 2 to 10.
in one embodiment, since the concentrated solution of the ceramic microfiltration or ultrafiltration membrane contains high concentration of polymer, ink, etc., the present invention can effectively reduce the COD and colloid content of the concentrated solution by adding a flocculant, such as polyaluminium chloride, polyacrylamide, etc., to the concentrated solution of the ceramic microfiltration or ultrafiltration membrane for flocculation treatment. The COD of the wastewater after flocculation and sedimentation treatment is obviously reduced, and the wastewater can be sent into a biochemical treatment unit for concentration treatment.
in one embodiment, before the step 1, ozone oxidation pretreatment is carried out on the development waste liquid; the addition amount of the ozone is 500-1000 ppm, and the reaction temperature is 40-70 ℃. In the oxidation process, macromolecules and polymers in the development waste liquid can be broken into small molecules, so that the viscosity of the waste liquid is reduced, the pollution on the surface of a ceramic ultrafiltration or microfiltration membrane can be effectively avoided, and the flux of the ceramic ultrafiltration or microfiltration membrane can be effectively improved. In one embodiment, the developing waste liquid after the ozone treatment can be further subjected to a three-phase cyclone separation treatment, the waste liquid contains more surfactants and resins, so that the developing liquid contains certain foams, the viscosity can be effectively reduced after the ozone oxidation treatment, small molecular resins and colloids can be attached to the foams, the printing ink and the small molecular colloids can be separated in an oil phase after the three-phase cyclone separation, in the three-phase cyclone separation, the oil phase at the top mainly contains the small molecular colloids, the foams, the printing ink and the like, a solid phase outlet at the side part separates out large particle suspended matters, a water phase outlet at the bottom mainly contains the separated waste liquid, and after the separation, the small molecular colloids and the resins cannot be attached to other particles in the microfiltration or ultrafiltration process to form a compact filter cake layer. The feeding flow rate is 3-8 m/s, the pressure difference between a solid phase outlet and the feeding is 0.10-0.30 MPa, and the volume ratio of oil-water-solid three-phase discharging is 0.2-0.25: 6.0-10.0: 0.8 to 1.5.
Based on the above method concept, the adopted device can be as shown in fig. 2:
The method comprises the following steps:
The homogenizing tank 1 is used for carrying out homogenizing treatment on the development waste liquid;
An aeration pipe 2 connected to the homogenizing tank 1 for aerating the homogenizing tank 1;
The ceramic microfiltration membrane or the ceramic ultrafiltration membrane 3 is connected to the homogenizing tank 1 and is used for filtering the homogenized development waste liquid;
the ceramic nanofiltration membrane 4 is connected to the permeation side of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane 3 and is used for performing nanofiltration treatment on the penetrating fluid;
And the nanofiltration penetrating fluid storage tank 8 is connected to the ceramic nanofiltration membrane 4 and is used for storing penetrating fluid containing sodium carbonate.
In one embodiment, the average pore size of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane 3 is in the range of 50 to 500 μm.
In one embodiment, the ceramic nanofiltration membrane in the step 2 has a molecular weight cut-off of 800-6000 Da.
In one embodiment, further comprising: the flocculation tank 5 is connected to the concentrated side of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane 3 and is used for performing flocculation sedimentation treatment on the concentrated solution of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane 3; the flocculation tank 5 is connected with a flocculant adding tank 7 for adding a flocculant into the flocculation tank 5; the water outlet of the flocculation tank 5 is connected with the biochemical reaction unit 6.
In one embodiment, the biochemical reaction unit 6 is an A2O biochemical reaction unit.
in one embodiment, the system further comprises an ozone reactor connected to the wastewater inlet of the ceramic micro-filtration membrane or the ceramic ultra-filtration membrane 3 for performing ozone oxidation treatment on the development wastewater entering the ceramic micro-filtration membrane or the ceramic ultra-filtration membrane 3.
The percentages recited in the present invention are all percentages by mass unless otherwise specified.
Example 1
And treating and recycling the developing and stripping waste liquid in the PCB production. The single batch treatment amount is 2000L of waste liquid, the concentration of sodium carbonate is 0.8 percent, and the COD is 6290 ppm. Homogenizing the waste liquid in a homogenizing tank, carrying out aeration treatment, pretreating the homogenized waste liquid by using a ceramic ultrafiltration membrane with the average pore diameter of 50nm, 200nm, 500nm and 2000nm, wherein the concentration multiple of the ceramic ultrafiltration membrane is 50 times, the ceramic ultrafiltration membrane is used for filtering suspended matters, colloid and the like, then separating small molecular impurities from sodium carbonate by using a ceramic nanofiltration membrane with the cut-off molecular weight of 5000Da, the concentration multiple of the ceramic nanofiltration membrane is 4 times, the operating pressure in the nanofiltration process is 0.1MPa, and the cross-flow filtration mode is adopted, and the membrane surface flow rate is 3 m/s. The clear liquid of the ultrafiltration membrane is 1960L, the clear liquid of the nanofiltration membrane is 1470L, namely the amount of the recovered sodium carbonate is 1470L, and the total recovery rate is 73.5 percent. The concentration of sodium carbonate in the treated filtrate is 0.8 percent, and the COD is 1500 ppm. The sodium carbonate solution can be applied to a developing and demoulding process to realize the recycling of sodium carbonate.
Example 2
And treating and recycling the developing and stripping waste liquid in the PCB production. The single batch treatment amount is 1000L of waste liquid, the concentration of sodium carbonate is 0.2 percent, and the COD is 46200 ppm. Homogenizing the waste liquid in a homogenizing tank, pretreating the homogenized waste liquid by using a 200nm ceramic ultrafiltration membrane, wherein the concentration multiple of the ceramic ultrafiltration membrane is 50 times, the ceramic ultrafiltration membrane is used for filtering suspended matters, then a ceramic nanofiltration membrane with the molecular weight cutoff of 1000, 2000 and 4800Da is used for separating ink and sodium carbonate, the concentration multiple of the ceramic nanofiltration membrane is 6 times, the operating pressure in the nanofiltration process is 0.6MPa, and the flow rate of the membrane surface is 3.5m/s by using a cross-flow filtration mode. The clear liquid of the ultrafiltration membrane is 980L, the clear liquid of the nanofiltration membrane is 815L, namely the amount of the recovered sodium carbonate is 815L, and the total recovery rate is 81.5 percent. The concentration of the sodium carbonate in the treated filtrate is 0.2%, and the sodium carbonate solution can be applied to a developing and demoulding process to realize the recycling of the sodium carbonate.
Example 3
And treating and recycling the developing and stripping waste liquid in the PCB production. The single batch treatment amount is 3500L of waste liquid, the concentration of sodium carbonate is 0.35 percent, and the COD is 8200 ppm. Homogenizing the waste liquid in a homogenizing tank, pretreating the homogenized waste liquid by using a 200nm ceramic ultrafiltration membrane, a PVDF ultrafiltration membrane, a PES ultrafiltration membrane and a PS ultrafiltration membrane, wherein the concentration multiple of the ceramic ultrafiltration membrane is 50 times, the ceramic ultrafiltration membrane is used for filtering suspended matters, then, a ceramic nanofiltration membrane with the cut-off molecular weight of 2000Da is used for separating ink from sodium carbonate, the concentration multiple of the ceramic nanofiltration membrane is 12 times, the operating pressure in the nanofiltration process is 0.8MPa, and the membrane surface flow rate is 3m/s by adopting a cross-flow filtration mode. The clear liquid of the ultrafiltration membrane is 3430L, the clear liquid of the nanofiltration membrane is 3145L, namely the amount of the recovered sodium carbonate is 3145L, and the total recovery rate is 89.8%. The average flux of the ultrafiltration membrane is 150LMH, and the average flux of the nanofiltration membrane is 12 LMH. The concentration of sodium carbonate in the treated filtrate is 0.35 percent, and the COD is 850 ppm. The sodium carbonate solution can be applied to a developing and demoulding process to realize the recycling of sodium carbonate.
example 4
And treating and recycling the developing and stripping waste liquid in the PCB production. The single batch treatment amount is 2000L of waste liquid, the concentration of sodium carbonate is 0.8 percent, and the COD is 6290 ppm. Homogenizing the waste liquid in a homogenizing tank, carrying out aeration treatment, carrying out ozone oxidation treatment on the waste liquid, wherein the addition amount of ozone is 800ppm, the reaction temperature is 45 ℃, the COD (chemical oxygen demand) of the treated waste liquid is reduced to 4520ppm, the waste liquid after ozone oxidation is pretreated by a ceramic ultrafiltration membrane with the average pore diameter of 50nm, 200nm, 500nm and 2000nm, the concentration multiple of the ceramic ultrafiltration membrane is 50 times, the ceramic ultrafiltration membrane is used for filtering suspended matters, colloids and the like, then a ceramic nanofiltration membrane with the molecular weight cutoff of 5000Da is used for separating small molecular impurities from sodium carbonate, the concentration multiple of the ceramic nanofiltration membrane is 4 times, the operating pressure of the nanofiltration process is 0.1MPa, a cross-flow filtration mode is adopted, and the membrane surface flow rate is 3 m/. The clear liquid of the ultrafiltration membrane is 1960L, the clear liquid of the nanofiltration membrane is 1470L, namely the amount of the recovered sodium carbonate is 1470L, and the total recovery rate is 73.5 percent. The concentration of sodium carbonate in the treated filtrate is 0.8 percent, and the COD is 1500 ppm. The sodium carbonate solution can be applied to a developing and demoulding process to realize the recycling of sodium carbonate.
Example 5
and treating and recycling the developing and stripping waste liquid in the PCB production. The single batch treatment amount is 2000L of waste liquid, the concentration of sodium carbonate is 0.8 percent, and the COD is 6290 ppm. Homogenizing the waste liquid in a homogenizing tank, carrying out aeration treatment, sending the waste liquid into a three-phase cyclone separator for separation, feeding the waste liquid from the side part, discharging an oil phase from the top part, separating out large-particle suspended matters from a solid phase outlet at the side part, mainly discharging the separated waste liquid from a water phase outlet at the bottom part, wherein the feeding flow rate is 4m/s, the pressure difference between the solid phase outlet and the feeding is 0.20MPa, and the volume ratio of oil, water and solid three-phase discharging is 0.22: 8.0: 1.5, pretreating the separated bottom waste liquid by using a ceramic ultrafiltration membrane with the average pore diameter of 50nm, 200nm, 500nm and 2000nm, wherein the concentration multiple of the ceramic ultrafiltration membrane is 50 times, the ceramic ultrafiltration membrane is used for filtering suspended matters, colloid and the like, then, a ceramic nanofiltration membrane with the cut-off molecular weight of 5000Da is used for separating small molecular impurities from sodium carbonate, the concentration multiple of the ceramic nanofiltration membrane is 4 times, the operating pressure in the nanofiltration process is 0.1MPa, and the cross-flow filtration mode is adopted, and the membrane surface flow rate is 3 m/s. The clear liquid of the ultrafiltration membrane is 1960L, the clear liquid of the nanofiltration membrane is 1470L, namely the amount of the recovered sodium carbonate is 1470L, and the total recovery rate is 73.5 percent. The concentration of sodium carbonate in the treated filtrate is 0.8 percent, and the COD is 1500 ppm. The sodium carbonate solution can be applied to a developing and demoulding process to realize the recycling of sodium carbonate.
The above description of embodiments does not constitute a limitation of the invention.
Claims (10)
1. A method for recycling development waste liquid is characterized by comprising the following steps:
Step 1, carrying out pre-filtration treatment on the development waste liquid;
And 2, filtering the filtrate obtained by pre-filtering by adopting a ceramic nanofiltration membrane, and obtaining a penetrating fluid containing sodium carbonate at the penetrating side of the ceramic nanofiltration membrane.
2. The method for recycling a development waste liquid according to claim 1, wherein the development waste liquid contains 0.1 to 1wt% of sodium carbonate, and 1000 to 50000ppm of COD; the pre-filtration in the step 1 is carried out by adopting a ceramic ultrafiltration or microfiltration membrane; the average pore diameter range of the ceramic ultrafiltration or microfiltration membrane is 50-500 mu m.
3. The method for recycling a waste developing solution according to claim 1, wherein the waste developing solution is subjected to a homogenization treatment before the step 1; and the intercepted molecular weight of the ceramic nanofiltration membrane in the step 2 is 800-6000 Da.
4. The method for recycling the development waste liquid according to claim 1, wherein the operating pressure of the ceramic nanofiltration membrane is 0.1 to 1.5MPa, a cross-flow filtration mode is adopted, and the membrane surface flow rate is 2 to 6 m/s.
5. The method for recycling the development waste liquid according to claim 1, wherein the concentration multiple of the ceramic nanofiltration membrane is 2 to 10 times.
6. The method for recycling a waste developing solution according to claim 1, wherein before the step 1, an ozone oxidation pretreatment is performed on the waste developing solution; the addition amount of the ozone is 500-1000 ppm, and the reaction temperature is 40-70 ℃.
7. The utility model provides a recycle device of development waste liquid which characterized in that includes:
A homogenizing tank (1) for homogenizing the development waste liquid;
The aeration pipe (2) is connected with the homogenizing tank (1) and is used for aerating the homogenizing tank (1);
The ceramic microfiltration membrane or ceramic ultrafiltration membrane (3) is connected with the homogenizing tank (1) and is used for filtering the homogenized development waste liquid;
The ceramic nanofiltration membrane (4) is connected to the permeation side of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane (3) and is used for performing nanofiltration treatment on the permeation liquid;
And the nanofiltration penetrating fluid storage tank (8) is connected to the ceramic nanofiltration membrane (4) and is used for storing penetrating fluid containing sodium carbonate.
8. The apparatus for recycling a development waste liquid according to claim 7, wherein the average pore diameter of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane (3) is within a range of 50 to 500 μm; and the intercepted molecular weight of the ceramic nanofiltration membrane in the step 2 is 800-6000 Da.
9. The apparatus for recycling a development waste liquid according to claim 7, further comprising: the flocculation tank (5) is connected to the concentrated side of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane (3) and is used for performing flocculation sedimentation treatment on the concentrated solution of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane (3); the flocculation tank (5) is connected with a flocculant adding tank (7) for adding a flocculant into the flocculation tank (5); the water outlet of the flocculation tank (5) is connected with the biochemical reaction unit (6).
10. The apparatus for recycling development waste liquid according to claim 7, wherein said biochemical reaction unit (6) is an A2O biochemical reaction unit; the device also comprises an ozone reactor which is connected with a wastewater inlet of the ceramic microfiltration membrane or the ceramic ultrafiltration membrane (3) and is used for carrying out ozone oxidation treatment on the development wastewater entering the ceramic microfiltration membrane or the ceramic ultrafiltration membrane (3).
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