CN101302072B - Dye or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material recovery process and apparatus - Google Patents
Dye or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material recovery process and apparatus Download PDFInfo
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- CN101302072B CN101302072B CN2008101227888A CN200810122788A CN101302072B CN 101302072 B CN101302072 B CN 101302072B CN 2008101227888 A CN2008101227888 A CN 2008101227888A CN 200810122788 A CN200810122788 A CN 200810122788A CN 101302072 B CN101302072 B CN 101302072B
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Abstract
The invention relates to a process for recovering the materials separated by a dye and pesticide wastewater reverse-osmosis and nanofiltration combined membrane, comprising the following steps that: the wastewater to be treated in a reservoir enters a medium filter after pressurization; the filtrate of the medium filter enters a microfilter; the filtrate of the microfilter enters a counter-osmosisdevice after the pressurization; a concentrated solution trapped by the counter-osmosis device enters a nanofilter for separation, dyes, pesticides and related intermediates are recovered from the flowed out liquid; and penetrating fluids of the counter-osmosis device and the nanofiler are mixed and collected. The process can be directly amplified in the engineering application; the membrane technology combined process is adopted to test active red printing and dyeing wastewater in a chemical plant, the rejection recovery rate of the dyes is more than 99.0 percent and the water yield flux after continuous operation of the membrane for four hours is more than 25L/ (m<2>.h). The process is adopted to treat the imidacloprid and salicylal wastewater of an insecticide factory, the material recovery rate is more than 70 percent, the salt rejection is more than 90 percent, the removal rate of COD is more than 70 percent and the water productivity is more than 95 percent.
Description
One, technical field
The invention belongs to field of environment engineering technology, the membrane separation material recovery process and the device thereof of particularly a kind of application micro-filtration (Micro filtration:MF), reverse osmosis (Reverse Osmosis:RO) and nanofiltration (Nano filtration:NF) technology.
Two, background technology
At present, the pollutent category is various in the waste water of production dyestuff, agricultural chemicals, comprises the intermediate of production process, reaches several ten thousand kinds.Dyestuff, agricultural chemicals and intermediate molecular structure complexity thereof contain phenyl ring, naphthalene, quinone, sulfonic group, azo-group, hydroxyl, carbonyl, carboxyl, nitro and amido isoreactivity group more.The molecular structure stabilized of dye substance, its product innovation with anti-oxidant, anti-photochemical, antibiosis turns into is product quality indicator; Have poisonous groups such as phosphorous, chlorine, cyanogen, phenol in the Pesticide Molecule structure, these groups have serious lethal effect to microorganism.The dye well agricultural chemicals waste water is the industrial heavily contaminated source of generally acknowledging in the world, and its governing problem is the great environment problem that international academic community is extremely paid close attention to.American-European countries is too high based on the control expense of waste water, the price competitiveness of product is reduced, thereby this class industrial shift is arrived developing country.China is dyestuff, pesticide producing big country, and effectively administering a large amount of poisonous and harmful waste water that produce in the sector has been the instant task of top priority.
Dyestuff, agricultural chemicals waste water have: contain characteristics such as organism amount and saltiness height (COD up to several ten thousand to hundreds of thousands of mg/L, saltiness reaches 10%～30%), toxicity are big, difficult for biological degradation, its treatment process mainly contains biological process and physico-chemical processes two big classes.Biological process is one of the comparatively general method of using at present, and its main advantage is that processing costs is low, can handle to hundreds of times but must dilute tens times, even so, still is difficult to up to standard.Physico-chemical processes mainly contains absorption method, solvent extration, micro-electrolysis method, catalytic oxidation etc., and this class methods cost height, effect are general, difficult enforcement on engineering is used.
Membrane separation technique is an emerging wastewater processing technology, comprise MF, ultrafiltration (Ultra filtration, UF), RO, NF, electrodialysis (Electro Dialysis, ED), liquid film (Liquid Membrane, LM) etc., have advantages such as adaptability is strong, processing efficiency is high, simple to operate, no phase transformation, recoverable material, have a extensive future.Size of separation, the process range of various types of films technology have nothing in common with each other, and reasonable combination various types of films technology can be brought into play various types of films technical superiority, efficiency optimization.Research and application that the membrane technique of overseas utilization combination is handled dyestuff, agricultural chemicals waste water have obtained certain progress, but it is still rare that its achievement in research is applied to the report of engineering.
Three, summary of the invention
Technical problem: the technological gap that the present invention is directed to present existence, provide a kind of dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material to reclaim technology and device thereof, this technology and device can be handled dyestuff, agricultural chemicals waste water, can solve dyestuff, agricultural chemicals waste water since concentration height, saltiness greatly, difficult for biological degradation causes the low technical problem of processing efficiency.
Technical scheme: a kind of dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, and processing step is: under 25～35 ℃ water temperature condition, the pH value of pending waste water in the tank is adjusted to 6.5～9.0; Waste water enters medium filter after supercharging, remove the suspended substance of particle diameter＞1mm; Medium filter filtrate enters micro-strainer, removes the colloid of particle diameter at 0.1～1 μ m, and alluvial index SDI＜5 of control water outlet; Micro-strainer filtrate enters counter-osmosis device through pressurization, removes particle diameter 10
-10The inorganic salt of the m order of magnitude and organism, the working pressure of counter-osmosis device are 1.0～2.0MPa; Held back concentrated solution by counter-osmosis device and enter the separation of nanofiltration device, remove particle diameter 10
-9The divalent salts of the m order of magnitude and organism, the working pressure of nanofiltration device are 0.5～0.7MPa, reclaim dyestuff, agricultural chemicals and relevant intermediate in the effluent liquid; The penetrating fluid of counter-osmosis device and nanofiltration device is mixed the back collection.Packing material size in the medium filter is quartz sand or the haydite of 0.5～1.2mm.The microfiltration membrane material is polyvinylidene difluoride (PVDF) or tetrafluoroethylene.The reverse osmosis membrane material is a polymeric amide.The nanofiltration membrane material is a polymeric amide.Be used for the device that dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, it is characterized in that this device comprises tank, medium filter, micro-strainer, counter-osmosis device and nanofiltration device, said apparatus is linked in sequence by inlet and outlet pipe lines, wherein be provided with topping-up pump between tank and the medium filter, be respectively equipped with first tensimeter and second tensimeter on the inlet and outlet pipe lines of micro-strainer two ends, be provided with thief hole successively between second tensimeter on the micro-strainer outlet conduit and the counter-osmosis device, high-pressure pump, check valve, ball valve and first flow meter, be respectively equipped with the 3rd tensimeter on counter-osmosis device inlet channel and the concentrated solution outlet conduit, the 4th tensimeter, be provided with first variable valve between the 4th tensimeter on the counter-osmosis device concentrated solution outlet conduit and the nanofiltration device, first magnetic valve and second under meter, nanofiltration device concentrated solution outlet conduit is provided with the 5th tensimeter, second variable valve, second magnetic valve and the 3rd under meter, wherein first variable valve with contact with second under meter after first magnetic valve is in parallel, second variable valve with contact with the 3rd under meter after second magnetic valve is in parallel, concentrated solution after the nanofiltration device is handled is reclaimed by the concentrated solution vent pipe, penetrating fluid through nanofiltration device and counter-osmosis device processing merges collection by nanofiltration device permeate discharge pipe and counter-osmosis device permeate discharge pipe respectively, enters biochemical treatment afterwards.Be provided with the pH regulator device in the tank.
Beneficial effect: the present invention has made up membrane techniquies such as MF, RO, NF and has handled dyestuff, agricultural chemicals waste water.Do pre-treatment by media filtration～MF, can hold back the particulate matter greater than 5 μ m such as suspended substance in the waste water and colloidality impurity, RO, NF normally move with protection.Penetrating fluid productive rate＞80% after RO separates, the once concentration liquid of its generation (containing the salinity and material that are trapped) enters NF to be separated.Monovalent salt and small-molecule substance can see through NF, and the penetrating fluid of NF is a total inflow 16%, the total penetrating fluid productive rate of system＞95%.The secondary concentration liquid that NF produces is total inflow 4%, wherein the useful matter rate of recovery＞70%.RO mixes the back water outlet with the penetrating fluid of NF, its COD, salinity satisfy the condition of biochemical treatment, but handles qualified discharge or reuse by routine biochemistry.The present invention can directly be amplified to engineering and use, and adopts this form membrane technique combination process that certain chemical plant reactive brilliant red waste water is tested, and dyestuff is held back the rate of recovery more than 99.0%, and symphysis reforwarding row produced water flux 25L/ (m in 4 hours
2H) more than.To Provado, the salicylic aldehyde wastewater treatment of certain insecticide factory, material recovery rate is greater than 70%, and ratio of desalinization is greater than 80%, and greater than 70%, producing water ratio is greater than 90% to the clearance of COD.In sum, the producing water ratio of conventional membrane separation process processing back infiltration clear liquid is 70-80% only, and material recovery rate is 50-60% in the concentrated solution; Producing water ratio, material recovery rate are increased to 90% respectively, 70-80% and technology of the present invention can make.
Four, description of drawings
Fig. 1 is the device synoptic diagram that is used for dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material recovery technology, pH value adjuster 1 among the figure, tank 2, topping-up pump 3, medium filter 4, the first tensimeter 5a, the second tensimeter 5b, the 3rd tensimeter 5c, the 4th tensimeter 5d, the 5th tensimeter 5e, micro-strainer 6, thief hole 7, high-pressure pump 8, check valve 9, ball valve 10, first flow meter 11a, the second under meter 11b, the 3rd under meter 11c, counter-osmosis device 12, biochemical treatment 13, the first variable valve 14a, the second variable valve 14b, the first magnetic valve 15a, the second magnetic valve 15b, nanofiltration device 16, concentrated solution vent pipe 17, nanofiltration device permeate discharge pipe 18, counter-osmosis device permeate discharge pipe 19.
Five, embodiment
Embodiment 1:
A kind of dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, and processing step is: under 25～35 ℃ water temperature condition, the pH value of pending waste water in the tank is adjusted to 6.5～9.0; Waste water enters medium filter after supercharging, remove the suspended substance of particle diameter＞1mm, and the filler in the medium filter is quartz sand or the haydite of particle diameter 0.5～1.2mm; Medium filter filtrate enters micro-strainer, removes the colloid of particle diameter at 0.1～1 μ m, and alluvial index SDI＜5 of control water outlet, and the filler of micro-strainer is polyvinylidene difluoride (PVDF) or tetrafluoroethylene; Micro-strainer filtrate enters counter-osmosis device through pressurization, removes particle diameter 10
-10The inorganic salt of the m order of magnitude and organism, the working pressure of counter-osmosis device are 1.0～2.0MPa, and the reverse osmosis membrane material is a polymeric amide; Enter the nanofiltration device through the effusive concentrated solution of counter-osmosis device and separate, the working pressure of nanofiltration device is 0.5～0.7MPa, removes particle diameter 10
-9The divalent salts of the m order of magnitude and organism reclaim dyestuff, agricultural chemicals and relevant intermediate in the effluent liquid, and the nanofiltration membrane material is a polymeric amide; The penetrating fluid of counter-osmosis device and nanofiltration device is merged collection, enter biochemical treatment afterwards.When handling certain factory imidacloprid pesticide waste water, 25-30 ℃ of water inlet water temperature regulated the pH value to 6.5-8.0, counter-osmosis device, nanofiltration device working pressure are respectively 1.5MPa, 0.7MPa, and the ratio of desalinization 82% of system is to COD clearance 80.4%, producing water ratio 94.6%, material recovery rate 73.7%.
Embodiment 2:
A kind of device that is used for dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material recovery technology, this device comprises tank 2, medium filter 4, micro-strainer 6, counter-osmosis device 12 and nanofiltration device 16, said apparatus is linked in sequence by inlet and outlet pipe lines, be provided with pH regulator device 1 in the tank, wherein be provided with topping-up pump 3 between tank and the medium filter, be respectively equipped with the first tensimeter 5a and the second tensimeter 5b on the inlet and outlet pipe lines of micro-strainer two ends, be provided with thief hole 7 successively between second tensimeter 5b on the micro-strainer outlet conduit and the counter-osmosis device, high-pressure pump 8, check valve 9, ball valve 10 and first flow meter 11a, be respectively equipped with the 3rd tensimeter 5c on counter-osmosis device inlet channel and the concentrated solution outlet conduit, the 4th tensimeter 5d, be provided with the first variable valve 14a between the 4th tensimeter 5d on the counter-osmosis device concentrated solution outlet conduit and the nanofiltration device 16, the first magnetic valve 15a and the second under meter 11b, nanofiltration device concentrated solution outlet pipeline is provided with the 5th tensimeter 5e, the second variable valve 14b, the second magnetic valve 15b and the 3rd under meter 11c, wherein the first variable valve 14a with contact with the second under meter 11b after the first magnetic valve 15a is in parallel, the second variable valve 14b with after the second magnetic valve 15b is in parallel with the 3rd under meter polyphone 11c, concentrated solution after the nanofiltration device is handled is reclaimed by concentrated solution vent pipe 17, collects laggard biochemical treatment 13 by nanofiltration device permeate discharge pipe 18 and 19 merging of counter-osmosis device permeate discharge pipe respectively through the penetrating fluid of nanofiltration device and counter-osmosis device processing.Working pressure, once concentration flow quantity, the reverse osmosis membrane of controlling counter-osmosis device by the adjusting of the first variable valve 14a, the first magnetic valve 15a and the second under meter 11b clean.The working pressure of the control nanofiltration device by the second variable valve 14b, the second magnetic valve 15b and the 3rd under meter 11c, secondary concentration flow quantity, nanofiltration membrane are cleaned.
Embodiment 3:
The correlation parameter of media filtration, MF, RO, NF such as following table:
| Parameter | Media filtration | Micro-filtration (MF) | Reverse osmosis (RO) | Nanofiltration (NF) |
| Material | Particle diameter such as quartz sand, haydite 0.5～1.2mm | Polyvinylidene difluoride (PVDF), tetrafluoroethylene | Polymeric amide | Polymeric amide |
| Parameter | Media filtration | Micro-filtration (MF) | Reverse osmosis (RO) | Nanofiltration (NF) |
| Remove material and size thereof | Suspended substance,＞1mm | Colloid, 0.1～1 μ m | Inorganic salt, organism, 10 -10M (Ethylmercurichlorendimide) | Divalent salts, organism, 10 -9M (nanometer) |
| Water inlet | Waste water | Medium filtrate | MF filtrate | The RO concentrated solution |
| Processing rate (%) | 100 | 100 | 70～80 | 70～80 |
| COD clearance (%) | 20～30 | 20～30 | 80～85 | 70～80 |
Embodiment 4:
SDI alluvial index measurement instrument comprises: 47mm diameter test bellows, 47mm test diaphragm (aperture 0.45 μ m), 1～5bar (10～70psi) tensimeters, pressure regulation needle type valve.Measuring process is as follows: (come from 2006 editions Tao Shi film products and technical manual-Di 4 portion water chemistry and pre-treatment P
140)
1. will test diaphragm (diameter 47mm, aperture 0.45 μ m) and carefully be placed in the test bellows,, tighten " O " shape sealing-ring, bellows will vertically be placed, should also be noted that diaphragm has the difference of pros and cons with the wetting diaphragm of little water.
2. regulate intake pressure begins to filter the 500mL water sample to 2.1bar (30psi) and metering immediately time t
0(by continuously regulating, it is constant that intake pressure is remained).
3. be the following continuous filtration of 2.1bar (30psi) 15 minutes at intake pressure.
4.15 continue the required time t of the same 500mL of record filtering after minute
15, keep the diaphragm on the filter and further analyze so that do.
5. calculate: work as t
15Be t
04 times the time, SDI
15Value is 5.When if water sample stops up diaphragm live fully, SDI
15Value is 6.7.The design guide rule requires to keep SDI
15Smaller or equal to 5.Actual proof reduces SDI
15Some preconditioning techniques comprise medium filter (as quartz sand and hard coal), ultrafiltration and micro-filtration.
Embodiment 5:
Waste water at first enters tank, and water temperature 25-35 ℃, pH=2-11.Different dyes, agricultural chemicals waste water are adjusted the pH value, and control waste water from dyestuff pH=7.0-9.0, agricultural chemicals waste water pH=6.5-8.0 change the state of material in water and the minimizing absorption at face thus.Waste water enters medium filter, MF successively after the topping-up pump supercharging, alluvial index (Silt Density Index, the SDI of control water outlet
15＜5), to prevent that RO film, NF membrane-coating granules material from stopping up.Water outlet is pressurizeed through high-pressure pump, enters RO film (working pressure 1.0-2.0MPa), and once concentration liquid enters NF to be separated, and (working pressure 0.5～0.7MPa) reclaims dyestuff, agricultural chemicals and relevant intermediate.The penetrating fluid of RO and NF is mixed, and its water outlet COD and salinity are all lower, but handle qualified discharge or reuse by routine biochemistry.Because the adsorption of material, RO device, NF device run to certain period and need clean, water for cleaning adopts the penetrating fluid (and adjust pH) of system, and rinse water is got back to wastewater disposal basin, cleans to get final product in 15-30 minute.For guarantee steady running, prevent concentration polarization, gelatin phenomenon, whole process adopts PLC system full automatic control.Can be by regulating the flooding quantity of ball valve controlling diaphragm, the water production rate of variable valve controlling diaphragm, solenoid control flushing.RO film and NF film can be chosen flexibly according to the feature of handling waste water, but array configuration remains unchanged, i.e. media filtration-MF-RO-NF (wherein the main manufacturer of RO and NF has the Osmincs company of FilmTec, the GE of U.S. DOW).Core technology is the different size of separations according to media filtration, MF, RO, NF, and traditional filtering and membrane technique combination are realized removing step by step pollutent, separates concentrating useful material.Utilize RO that the high rejection of lower-molecular substance and NF are held back the part of divalent salts and pressure-driven is lower, to realize high efficiency separation.
Claims (7)
1. dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, it is characterized in that processing step is:
A. under 25～35 ℃ water temperature condition, the pH value of dyestuff pending in the tank or agricultural chemicals waste water is adjusted to 6.5～9.0;
B. waste water enters medium filter after supercharging, removes the suspended substance of particle diameter＞1mm;
C. medium filter filtrate enters micro-strainer, removes the colloid of particle diameter at 0.1～1 μ m, and alluvial index SDI＜5 of control water outlet;
D. micro-strainer filtrate enters counter-osmosis device through pressurization, removes the inorganic salt and the organism of particle diameter at the 10-10m order of magnitude, and the working pressure of counter-osmosis device is 1.0～2.0MPa;
E. the concentrated solution of being held back by counter-osmosis device enters the separation of nanofiltration device, and the working pressure of nanofiltration device is 0.5～0.7MPa, removes the divalent salts and the organism of particle diameter at the 10-9m order of magnitude, reclaims dyestuff, agricultural chemicals and relevant intermediate in the concentrated solution;
F. enter biochemical treatment after the penetrating fluid mixing back of counter-osmosis device and nanofiltration device being collected.
2. dyestuff according to claim 1 or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, it is characterized in that the filler in the described medium filter is quartz sand or the haydite of particle diameter 0.5～1.2mm.
3. dyestuff according to claim 1 or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, it is characterized in that the microfiltration membrane material is polyvinylidene difluoride (PVDF) or tetrafluoroethylene in the described micro-strainer.
4. dyestuff according to claim 1 or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, it is characterized in that the reverse osmosis membrane material is a polymeric amide in the described counter-osmosis device.
5. dyestuff according to claim 1 or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, it is characterized in that the nanofiltration membrane material is a polymeric amide in the described nanofiltration device.
6. one kind is used for the device that dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material reclaim technology, it is characterized in that this device comprises tank (2), medium filter (4), micro-strainer (6), counter-osmosis device (12) and nanofiltration device (16), said apparatus is linked in sequence by inlet and outlet pipe lines, wherein be provided with topping-up pump (3) between tank and the medium filter, be respectively equipped with first tensimeter (5a) and second tensimeter (5b) on the inlet and outlet pipe lines of micro-strainer two ends, be provided with thief hole (7) successively between second tensimeter (5b) on the micro-strainer outlet conduit and the counter-osmosis device, high-pressure pump (8), check valve (9), ball valve (10) and first flow meter (11a), be respectively equipped with the 3rd tensimeter (5c) on counter-osmosis device inlet channel and the concentrated solution outlet conduit, the 4th tensimeter (5d), be provided with first variable valve (14a) between the 4th tensimeter (5d) on the counter-osmosis device concentrated solution outlet conduit and the nanofiltration device (16), first magnetic valve (15a) and second under meter (11b), on nanofiltration device concentrated solution outlet pipeline, be provided with the 5th tensimeter (5e), second variable valve (14b), second magnetic valve (15b) and the 3rd under meter (11c), wherein contact with second under meter (11b) in first variable valve (14a) back in parallel with first magnetic valve (15a), contact through (11c) with the 3rd under meter in second variable valve (14b) back in parallel with second magnetic valve (15b), concentrated solution after the nanofiltration device is handled is reclaimed by concentrated solution vent pipe (17), and the penetrating fluid that nanofiltration device and counter-osmosis device are handled enters biochemical treatment (13) after merging collection by nanofiltration device permeate discharge pipe (18) and counter-osmosis device permeate discharge pipe (19) respectively.
7. the device that is used for dyestuff or pesticide waste water reverse osmosis-nanofiltration combined membrane separation material recovery technology according to claim 6 is characterized in that being provided with in the described tank pH regulator device (1).
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| WO2011146936A2 (en) | 2010-05-21 | 2011-11-24 | Adrian Brozell | Self-assembled surfactant structures |
| CN101935111B (en) * | 2010-08-26 | 2012-12-19 | 宝钢工程技术集团有限公司 | Wastewater recycling preparation system with low energy consumption |
| CN102408171A (en) * | 2010-09-25 | 2012-04-11 | 中国石油化工股份有限公司 | Method for treating reverse osmosis concentrated water |
| CN101979345B (en) * | 2010-10-29 | 2012-05-23 | 沈斌 | Mobile combined catalytic wastewater recycling water resource device |
| WO2013078464A1 (en) | 2011-11-22 | 2013-05-30 | Znano Llc | Self-assembled surfactant structures |
| CN103449571B (en) * | 2013-08-22 | 2015-09-30 | 煤炭科学研究总院杭州环保研究院 | Treating mine drainage method and device |
| CN104229941A (en) * | 2014-09-28 | 2014-12-24 | 王建军 | Device and method for recycling treatment of amino containing waste water |
| CN110606587B (en) * | 2019-08-09 | 2023-03-10 | 浙江丝绸科技有限公司 | Full-flow circulating dyeing system and process and application thereof |
| CN111116402A (en) * | 2019-11-26 | 2020-05-08 | 江苏瑞祥化工有限公司 | Imidacloprid byproduct salt treatment method |
| CN111672321B (en) * | 2020-05-22 | 2022-04-19 | 杭州娃哈哈科技有限公司 | Membrane equipment with adjustable desalination rate |
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| CN1868925A (en) * | 2005-05-26 | 2006-11-29 | 王俊川 | Circulation utilization technology and equipment for electroplating waste water separated by integrated membrane |
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