CN100577578C - Method of processing semi-conductor industrial waste water - Google Patents
Method of processing semi-conductor industrial waste water Download PDFInfo
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- CN100577578C CN100577578C CN200710134796A CN200710134796A CN100577578C CN 100577578 C CN100577578 C CN 100577578C CN 200710134796 A CN200710134796 A CN 200710134796A CN 200710134796 A CN200710134796 A CN 200710134796A CN 100577578 C CN100577578 C CN 100577578C
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Abstract
The invention relates to a process method for semiconductor industry wastewater. The invention is principally used for treating and reusing of the waste water generated in the reducing process of the semiconductor production enterprises. The invention is characterized in that the following steps are included in the process: (1) the electroplating water and the grinding water generated in the production process of the semiconductor elements are mixed together for forming a mixed waste water; (2) the mixed waste water in step (1) is pumped into a submerged membrane filtering device for filtering; (3) the filtered water in step (3) is pumped into a nanofiltration membrane filtering device for filtering and the filtered water filtered through the nanofiltration membrane filtering device can be directly reused. In the invention, filtering treatment is carried out for the mixed waste water generated in a semiconductor process through the submerged membrane filtering device and the nanofiltration membrane filtering device, the recycled water source rate is bigger than 85 percent. The recycled water has a stable quality which completely arrives or is better than the national standard. The whole treatment process has no chemical medicine; therefore, no detrimental sludge is produced. The processing method for semiconductor industry wastewater has the advantages of low operation cost and non-detrimental compressed sludge as well as easy treatment.
Description
Technical field
The present invention relates to water treatment method, especially relate to the treatment process of semi-conductor industrial waste water, more precisely, relate to silicon wafer cutting that in the semiconducter device production process, produces and the waste water and the component method of electroplating wastewater treatment of grinding.
Background technology
Semi-conductor industry is the industry that an extremely relies on water resources, also is the industry of high water consumption, especially under the limited situation of water resources, restricts water supply, lack of water produces immense pressure to the operation of semi-conductor manufacturing enterprise.Therefore,, help to promote the water benefit, reduce the water cost water-saving research of semi-conductor manufacturing enterprise and practice.At present; water saving, middle water reuse, recovery of Waste Water have become the important measures that the semi-conductor dealer tackles the lack of water crisis, particularly recovery of Waste Water, can reduce the demand to water resources; can reduce production costs again, also reduce pollution simultaneously environment.
Semi-conductor industrial waste water mainly comprises two portions: silicon wafer cutting and the waste water that grinds and the electroplating wastewater of semiconductor packages shell.Wherein the electroplating wastewater of semiconductor packages shell mainly is meant the electroplating wastewater of semiconductor device package casing and the electroplating wastewater of semi-conductor discrete device package casing, the i.e. waste water that when the metallic element higher slice of described package casing has been electroplated the conduction and the metal level of preservative activity, has produced, pollutent wherein mainly is metal ions such as bronsted lowry acids and bases bronsted lowry and tin, lead, copper, nickel, and organism and organic complex etc.; Silicon wafer cutting wherein and the waste water that grinds result from the cutting and grinding operation of silicon wafer, wherein contain a large amount of submicron order silicon grains, following silicon carbide abrasive particle and the clean-out system of tens nanometer.Above-mentioned waste water quality sees table 1 for details:
Table 1: waste water quality
| The index project | Electroplating wastewater | Project | Abrasive waste water |
| The pH value | ≤3 | The |
7～8 |
| SS(mg/L) | ≤250 | SS(mg/L) | 150～2000 |
| Pb 2+(mg/L) | ≤15 | COD Cr(mg/L) | 10～1500 |
| Sn 2+(mg/L) | ≤14 | Turbidity (NTU) | 50～80 |
| Cu 2+(mg/L) | ≤10 | Suspended particle particle diameter (μ m) | ＜1 |
| Ni 2+(mg/L) | ≤15 | ||
| COD Cr(mg/L) | ≤150 |
In the table 1, SS is the suspended solid concentration value, COD
CrBe chemical oxygen demand (COD), it is for weighing the parameter of organic pollutant in the waste water.As seen from Table 1, two portions waste water quality is very complicated, and pollutant kind is various, and the superfine suspended particle of high density especially wherein and organic pollutant are difficult to remove.
In the prior art, above-mentioned electroplating wastewater and abrasive waste water adopt the method that shunting is handled usually.Wherein electroplating wastewater processing adopts methods such as chemical reduction, precipitation, absorption, little electrolysis, evaporation and ion-exchange at present mostly, in these method of wastewater treatment, (1) needs to use heavy dose of sodium hydroxide, flocculation agent etc., produce a large amount of harmful heavy metal mud in the treating processes; (2) the treatment system floor space is big, and flow process is loaded down with trivial details; (3) complicated operation is because this part factory effluent water quality instability causes the effluent quality instability, thereby can't directly recycle water resources.In the prior art, also have to relate to the patent that membrane filter method is handled electroplating wastewater, its name is called " membrane separating method of electroplating wastewater processing zero release ", application number is the ZL03157655 patent, and its publication number is CN1590322A, and open day is on March 9th, 2005.The electroplating effluent treatment method of this patent disclosure adopts the one-level nanofiltration membrane to filter, secondary brackish water reverse osmosis membrane filtration, and three grades of seawater reverse osmosis membranes filter, and flow process is loaded down with trivial details, and operation energy consumption is very high, and the reclamation rate of water is lower, only is about 70%.Wherein abrasive waste water is handled the method processing of adopting chemical flocculation-precipitation-ultrafiltration-reverse osmosis to combine at present mostly.Be called " colorful glass bulb abrasive water is through the dehydration treatment method of the inorganic mud of processed formation " in name, application number is ZL200610013764, publication number is CN/101007697, the dehydration treatment method of a kind of colorful glass bulb abrasive waste water through the inorganic mud of processed formation disclosed in the patent application that open day is on August 1st, 2007, it at first utilizes polyacrylamide to the mud concentration of flocculating, mud enters the press filtration of pocket type pressure filter again, but need to add chemical agent in its treating processes, cause secondary pollution to seeing through liquid, running cost is higher.Be called " a kind of fiber super-filtering method and equipment " in name, application number is ZL200510041374, publication number is CN1743055, a kind of method that adopts fiber pre-filtration step and ultra-filtration to handle abrasive waste water is disclosed in the patent application that open day is on March 8th, 2006, it is at first with the fiber micro-filtration part macrobead suspended substance of abrasive waste water through 1～10 micron, utilizing pressuring method to enter to hold back the aperture again is 0.01～0.03 micron rolling ultrafiltration membrance filter, because filtering structures, these twice easily pollute, so need frequent back flushing, whole flow process producing water ratio is less than 85%.
Above-mentioned water treatment method exists that treatment facility structure bulky complex, floor space are big, investment and the very expensive problem of working cost, and treating processes need be added various chemical medicaments usually, to realize precipitation by metallic ion and solid particulate flocculation sediment, thereby in treating processes, produce a large amount of harmful mud, and organic pollutant is by the mode of osmosis filtration, exist complicated operation, effluent characteristics instability, water outlet can't reuse, weak point such as operation energy consumption height.
Summary of the invention
The applicant is at above-mentioned problem, having carried out research improves, a kind of treatment process with semi-conductor industry electroplating wastewater and abrasive waste water mixing and employing combined filtration method is provided, the entire treatment process need not add any chemical agent, just can effectively remove various impurity, real realization waste water reclaiming, and treatment system is taken up an area of little, safe, reliable.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of treatment process of semi-conductor industrial waste water, its treatment step is as follows:
((1) mixes electroplating wastewater and the abrasive waste water that produces in the semiconducter device manufacturing, forms composite waste;
(2) composite waste with step (1) pumps into the filtration of submerged membrane filtration unit;
(3) will pump into the nanofiltration membrane filtration unit through the filtering water of step (2) and filter, get final product direct reuse through the filtering water of nanofiltration membrane filtration unit.
Above-mentioned nanofiltration membrane filtration unit adopts surperficial positively charged aromatic polyamides composite nanometer filtering film or surperficial positively charged polyacrylonitrile nanofiltration membrane to filter.
The treatment process of above-mentioned semi-conductor industrial waste water is to comprise the submerged membrane filtration unit to filter (MF) and the filtering composite membrane filtration treatment method of nanofiltration membrane filtration (NF) device.Mix with electroplating wastewater with the abrasive waste water that produces in semiconductor integrated circuit and the discrete device production, obtain composite waste, composite waste is handled, finally obtain the middle water of resistivity more than 0.1M Ω cm through above-mentioned steps.
Organic pollutant in the electroplating wastewater belongs to the tensio-active agent of high molecular functional, and the organic pollutant in the abrasive waste water (for example clean-out system wherein) belongs to macroion type tensio-active agent.After electroplating wastewater and abrasive waste water mix, above-mentioned surfactant molecule can spontaneously reach in solution and directionally be adsorbed on the solid-liquid two-phase interface, thereby reduced the interfacial tension between solution and silicon carbide and the silicon solid particulate, made these solid particulates be suspended in the aqueous solution; Secondly, because the concentration of above-mentioned surfactant molecule in waste water is far above its micelle-forming concentration, add the enhancement of a large amount of inorganic electrolytes (for example metal ion, acid group etc.), cause many surfactant molecules to associate into the state of aggregation micelle, these micelle surfaces contact, adhere to silicon carbide and silicon solid particulate in water, make micelle become big, make it to be easier to be filtered away.By as seen above-mentioned, after electroplating wastewater and abrasive waste water mix, organic dirt wherein and mineral contaminants produce synergy, the above-mentioned micelle that is suspended in the solid particulate in the aqueous solution and adheres to solid particulate matter, cross after the unit filters through submerged membrane of the present invention, can be filtered removing, make delivery turbidity drop to below the 0.1NTU COD
CrDrop to below the 80mg/L, SS drops to 0mg/L.And filter in the residual concentrated solution in back, discharge by residual sea water pump during in SS concentration up to the 10000mg/L left and right sides, do not need to add chemical agent, directly press filtration or the mode taking to dry are handled.Like this, the organism and the solid particulate of intractable are easy to be removed under above-mentioned synergy originally.And the ratio of above-mentioned two kinds of waste water can not limited, can produce above-mentioned synergy, although synergistic varying in size.
The nanofiltration membrane filtration unit is to be motivating force with pressure, nanofiltration membrane is filtered has following distinguishing feature in application: sieve effect is held back or held back to (1) physics, the nanofiltration membrane aperture is minimum, about its mean pore size 1nm, can hold back minimum dissolved constituent or solid particulate effectively; (2) charge, promptly selectivity is held back, and is then higher to the rejection of divalence and polyvalent ion to the rejection lower (40%～80%) of univalent ion, for example, can filter the most of metal ion in the above-mentioned waste water, both economical; (3) to compare working pressure low with reverse osmosis, and it is big to see through flow rate.(4) compare with the treatment process that method of evaporation or other have " mutually " to become, the nanofiltration membrane filtration method do not have " phase " to become, thereby energy consumption is low to the treating processes of electroplating wastewater; (5) nano filtering process treatment facility floor space is little, facility compact, easily automatic control, but operate continuously.
And, through the above-mentioned semiconductor machining composite waste of submerged membrane filter plant processing, owing to most suspended particulates, organism are removed, so can avoid fouling in nanofiltration system.Water is held back by the selectivity of its charge after handling through nanofiltration system, and the above heavy metal ion rejection of divalence is higher than 99.5%, and the rejection of monovalent ion can reach 80%, sees through Pb in the liquid
2+, Sn
2+, Cu
2+Concentration to drop to national miscellaneous water below the mark, specific conductivity drops to below the 10 μ S/cm, resistance reaches more than the 0.1M Ω cm.Because the physics crown_interception of nanofiltration is further removed organism and suspended particle in the water, makes water outlet COD
CrDrop to below the 50mg/L.Concentrated solution through nanofiltration membrane filtration unit filtration residue mixes with the concentrated solution of submerged membrane filtration unit filtration residue, and press filtration is handled.Because the entire treatment process is not added any chemical agent, only comprises silicon grain and particles of silicon carbide mud and tensio-active agent in the concentrated solution, it is nontoxic and dense, and viscosity is bigger, easily by the filter-pressing device press filtration.
Above-mentioned semiconductor machining composite waste is after filtering filtration of (MF) device and nanofiltration membrane filtration (NF) device filtration treatment through submerged membrane, recyclable greater than 85% water resources, recovery water quality reaches fully and is better than country about " urban sewage reutilization process water water quality " (GB T19923-2005), " urban sewage reutilization city miscellaneous water water quality " is standard (GB/T18920-2002), reach more than the 0.1M Ω cm, but direct reuse makes to produce bath water, plant area's greening, fire-fighting replenishes water, cooling tower replenishes uses water of condensation, the reverse osmosis manufacturing production source water of ultrapure water etc.; The entire treatment process is not added any chemical agent, and the mud after concentrating is nontoxic, harmless, easily handles; And the treatment system flow process is short, occupation of land is little, energy consumption is low, easily is automated control, and system's operation is more reliable, and working cost is lower, really realizes sewage, waste water reclaiming, increases available water resources, helps realizing that waste water is innoxious, the anti-pollution of harnessing the river.
Description of drawings
Fig. 1 is a schema of the present invention.
Fig. 2 is a water treatment system schematic diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail.
Technical process as shown in Figure 1 adopts the silicon wafer electroplating wastewater of certain Microtronic A/S's unicircuit production generation and the abrasive waste water of package casing to enter in the mixing pit, becomes composite waste, and its water quality sees Table 2.The immersion flat sheet membrane filtration unit that adopts Wuxi Ningyang Environmental Science ﹠ Technology Co., Ltd. to manufacture and design, its Chinese number of patent application is 200720035758.4, its structural representation is seen Fig. 2.The used filtering membrane of this equipment is a dull and stereotyped immersion organic polymer material microfiltration membrane (MF), its filter opening is between 0.04～0.5 μ m, working pressure is less than 20KPa, can effectively remove suspended substance, micelle, particle and most organic impurity in the above-mentioned semiconductor machining composite waste, above-mentioned semiconductor machining composite waste is listed in the table 2 in the water quality of filtering the back water outlet through the submerged membrane filtration unit.
See Fig. 1, the liquid that sees through through submerged membrane filtration unit filtration treatment pumps into the nanofiltration membrane filtration unit and handles.The nanofiltration membrane filtration unit can use the commercially available prod, selects the aromatic polyamides composite nanometer filtering film of surperficial lotus positive electricity for use, and mean pore size is 1nm, and below the molecular weight cut-off 200Da (dalton), its working pressure is about 0.5～1.5MPa.Can remove in the water remaining larger molecular organics, 99.5% heavy metal ion and 80% monovalent salt ion, handle the back effluent quality and list in the table 2 ("-" expression detects to go out in the table, and its value is similar to zero).Reach fully and be better than country through the water quality that sees through liquid of submerged membrane filtration unit and nanofiltration membrane filtration unit, but direct reuse is made to produce bath water, plant area's greening water, fire-fighting and replenished water, cooling tower and replenish with water of condensation etc. about (GB/T18920-2002) standard of " urban sewage reutilization process water water quality " (GB T19923-2005), " urban sewage reutilization city miscellaneous water water quality ".
As shown in Figure 2, above-mentioned semiconductor machining composite waste pending in the mixing pit is pumped in the treating pond 1 of immersion flat sheet membrane filtration unit, its filter element is the membrane filtration module 3 that is immersed in the waste water.The flat film filter 8 of device series of parallel in the membrane filtration module 3, each flat filter 8 outer is with a sealed framework, the flat filtering membrane of framework face upper sealing device, there is water outlet the upper end of framework, among Fig. 27 is total water outlet of membrane filtration module 3, and the water outlet of itself and each flat film filter 8 is connected by pipeline.During filtration, the outside of the flat filtering membrane of waste water from each flat film filter 8 enters the inside of each flat film filter 8, becomes the filtration water outlet, is discharged by the water outlet of strainer 8.
A plug-in mounting frame that has slot is arranged at the bottom of membrane filtration module 3, and in the slot of each flat film filter 8 vertical insertion plug-in mounting frame, this plug-in mounting structure can make the displacement of flat film filter 8 become very convenient.
The water quality of table 2 semiconductor machining composite waste and water outlet
| The index project | The pH value | SS (mg/L) | Pb 2+ (mg/L) | Sn 2+ (mg/L) | Cu 2+ (mg/L) | COD Cr (mg/L) | Turbidity (NTU) |
| Above-mentioned semiconductor machining composite waste | 6 | 600 | 12 | 10 | 5 | 1000 | 80 |
| The submerged membrane filtration unit filters the back water outlet | 6 | - | 12 | 10 | 5 | 80 | 0.1 |
| Nanofiltration device is filtered the back water outlet | 6.1 | - | 0.01 | 0.02 | 0.05 | 45 | 0.018 |
| " urban sewage reutilization process water water quality " (GB T19923-2005) | 6～ 9 | 30 | No requirement (NR) | No requirement (NR) | No requirement (NR) | 60 | ≤3 |
The aerated conduit 9 that has solarization air cap is installed below membrane filtration module 3, and aerated conduit 9 is connected with the pressure gas of gas blower 10 output terminals, constitutes aerating apparatus.The a large amount of bubbles 2 that utilize aerating apparatus to produce cause the swirling flow that air water stream rises in treatment tank 1, utilize its shearing force to wash away filtration dirt on the filter membrane surface, to keep the flux of filtering membrane, because it adopts flat sheet membrane to filter, the obstruction possibility of film is low, so do not need back flushing.
As shown in Figure 2,4 blow-off lines for the remaining sewage after filtering are connected with residual sea water pump by valve.The filtration effluent adopting suction filtration of each membrane filtration module 3 is connected with the water outlet 7 of membrane filtration module 3 by header 5 by suction filtration pump 6, and the filtered water of extraction enters to be proceeded in the nanofiltration membrane filtration unit 11 to filter.The process nanofiltration membrane filtration unit 11 filtering liquid that see through are discharged through rising pipe 12, but direct reuse, its concentrated solution is discharged through blow-off line 13, and the remaining sewage concentrated solution of discharging with blow-off line 4 carries out the press filtration processing.
Certain electronics scientific technology co, specialty development, production semi-conductor discrete device.Abrasive waste water and the water quality of discrete device electroplating wastewater after entering mixing pit that its semi-conductor manufacturing produces are listed in table 3, and wherein the package casing of semi-conductor discrete device is that first electro-coppering, re-plating nickel are handled.Above-mentioned semiconductor machining composite waste in the mixing pit is pumped into the submerged membrane filtration unit handle, filter back water quality and see Table 3 ("-" expression can not detect in the table, and its value is similar to zero).See through liquid and enter nanofiltration filtration unit continuation filtration treatment again, but the water quality direct reuse after final the filtration, and its water quality sees table 3 for details.
The water quality of above-mentioned semiconductor machining composite waste of table 3 and water outlet
| The index project | The pH value | SS (mg/L) | Cu 2+ (mg/L) | Ni 2+ (mg/L) | COD Cr/ (mg/L) | Turbidity (NTU) |
| Above-mentioned semiconductor machining composite waste | 6 | 400 | 7 | 10 | 800 | 70 |
| The submerged membrane filtration unit filters the back water outlet | 6 | - | 7 | 10 | 75 | 0.1 |
| Nanofiltration device is filtered the back water outlet | 6.1 | - | 0.05 | 0.01 | 40 | ≤0.018 |
| " urban sewage reutilization process water water quality " (GB T19923-2005) | 6～9 | 30 | No requirement (NR) | No requirement (NR) | No requirement (NR) | 60 |
Claims (2)
1. the treatment process of semi-conductor industrial waste water is characterized in that treatment step is as follows:
(1) electroplating wastewater and the abrasive waste water that produces in the semiconducter device manufacturing mixed, form composite waste;
(2) composite waste with step (1) pumps into the filtration of submerged membrane filtration unit, and the filtering membrane of described submerged membrane filtration unit is dull and stereotyped immersion organic polymer material microfiltration membrane, and its filter opening aperture is between 0.04～0.5 μ m;
(3) will pump into the nanofiltration membrane filtration unit through the filtering water of step (2) and filter, get final product direct reuse through the filtering water of nanofiltration membrane filtration unit.
2. the treatment process of semi-conductor industrial waste water according to claim 1 is characterized in that: described nanofiltration membrane filtration unit adopts surperficial positively charged aromatic polyamides composite nanometer filtering film or surperficial positively charged polyacrylonitrile nanofiltration membrane to filter.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101549913B (en) * | 2008-10-30 | 2011-08-17 | 浙江东洋环境工程有限公司 | Process and system for recovering reduction scribing waste water |
| CN104150624A (en) * | 2014-07-01 | 2014-11-19 | 霖创环保科技(上海)有限公司 | Treatment method for recycling silicon wafer grinding wastewater in semiconductor industry |
| US9828263B2 (en) * | 2014-08-28 | 2017-11-28 | Infineon Technologies Ag | Method of removing particulate silicon from an effluent water |
| CN110143646A (en) * | 2019-06-27 | 2019-08-20 | 埃姆媞（无锡）分离技术有限公司 | The method for concentration of printed circuit board production process copper-containing wastewater |
| CN112624428A (en) * | 2020-12-29 | 2021-04-09 | 上海丰信环保科技有限公司 | Three-stage filtration reuse water process for grinding wastewater in integrated circuit industry |
| CN115583751A (en) * | 2022-10-12 | 2023-01-10 | 天津中环领先材料技术有限公司 | Epitaxial wafer washing water treatment device and treatment method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1590322A (en) * | 2003-09-05 | 2005-03-09 | 国家海洋局杭州水处理技术研究开发中心 | Membrane separation method of zero discharge of electroplating waste water treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1590322A (en) * | 2003-09-05 | 2005-03-09 | 国家海洋局杭州水处理技术研究开发中心 | Membrane separation method of zero discharge of electroplating waste water treatment |
Non-Patent Citations (2)
| Title |
|---|
| 我国液体分离膜技术现状及展望. 王晓琳，杨健，徐南平，高从堦.南京工业大学学报，第27卷第5期. 2005 |
| 我国液体分离膜技术现状及展望. 王晓琳，杨健，徐南平，高从堦.南京工业大学学报，第27卷第5期. 2005 * |
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