CN103071392B - Chemical regeneration method for waste paper pulping and papermaking comprehensive waste water polluted ultrafiltration membrane - Google Patents
Chemical regeneration method for waste paper pulping and papermaking comprehensive waste water polluted ultrafiltration membrane Download PDFInfo
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- CN103071392B CN103071392B CN201310006734.6A CN201310006734A CN103071392B CN 103071392 B CN103071392 B CN 103071392B CN 201310006734 A CN201310006734 A CN 201310006734A CN 103071392 B CN103071392 B CN 103071392B
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Abstract
The invention discloses a chemical regeneration method for a waste paper pulping and papermaking comprehensive waste water polluted ultrafiltration membrane. The key point of the adopted method is to carry out initial physical wiping and chemical agent regeneration on the waste paper pulping and papermaking comprehensive waste water polluted ultrafiltration membrane to obtain a chemical regeneration filter membrane which is equivalent to a new membrane in filtering and interception performances. The method is rapid, efficient, environment-friendly and also low in operation cost, and specially aims at the chemical cleaning and regeneration of the waste paper pulping and papermaking comprehensive waste water polluted ultrafiltration membrane. The chemical regeneration method provided by the invention is beneficial for maintaining relatively high waste water flux, relatively few filter membrane replacement, relatively small pollution emission and cheap operation cost in the process of advanced treatment of the waste paper pulping and papermaking comprehensive waste water by a membrane separation technology, so that an important matched technological support is provided for the practical application of the membrane separation technology in the field of advanced treatment of the waste paper pulping and papermaking comprehensive waste water, and therefore, the chemical regeneration method has practical production significance.
Description
Technical field
The present invention relates to a kind of renovation process that pollutes milipore filter, particularly a kind of wastepaper pulping and papermaking comprehensive wastewater pollutes the chemical regeneration method of milipore filter, belongs to Pulp and Paper Engineering field.
Background technology
Pulp and paper industry is to rely on one of traditional manufacturing of water most.Along with the environmental pressure that current countries in the world face is increasing, pulp and paper industry has now trended towards water closed circulation.Thereby membrane separation technique has had wide application prospect in this field.Paper industry water resource circulating and recovering can effectively reduce clear water and chemicals usage, reduces fiber fines loss simultaneously.
From 20 century 70 membrane separation techniques, introduce first pulp and paper industry field, experienced the development of more than 30 year, be mainly used at present the wastewater treatment working section such as bleaching liquor purification, coating recovery and paper production waste water recycling of pulping and papermaking processes.Utilize membrane separation technique advanced treating wastepaper pulping and papermaking comprehensive wastewater, can further improve the purification efficiency of waste water, under the prerequisite of the operation of not impact system and product quality, realize wastepaper pulping and papermaking comprehensive wastewater overwhelming majority circulating and recovering, thereby reduce the consumption of production process clear water, reduce efflux wastewater pollutional load simultaneously, reach country's " new standard " emission request, there is important economic and social benefit.
Wastepaper pulping and papermaking comprehensive wastewater is mainly derived from the workshop sections such as slurrying, deinking, bleaching, making beating, purification screening and wet end of machine of waste paper, has discharge capacity large, containing the suspensions such as ink, fiber, filler and auxiliary agent, SS, COD
cr, BOD
5high etc. pollution index, color is darker, containing features such as toxicity chlorides.Adopt such waste water of membrane separation technique advanced treating, organic and inorganic pollution wherein easily deposits and is attached in filter membrane surface and hole, cause filter membrane to pollute, waste water flux declines, thereby causing membrane separation process to consume energy increases, filter membrane replacing is frequent, film separation process production cost rises, and then has hindered the practical application of membrane separation technique in wastepaper pulping and papermaking comprehensive wastewater advanced treating field.Therefore, urgently research and development fast, efficient, environmental protection, cheap pollution filter membrane cleaning program, for wastepaper pulping and papermaking comprehensive wastewater, pollute filter membrane specially and clean and regenerate.Polluting filter membrane cleaning and regeneration field, Chinese patent (ZL 95194986.1) " cleaning of hollow fiber film " utilizes the mode of back scrubbing that hollow fiber film is periodically cleaned, during back scrubbing, housing is sealed, before housing is opened to atmosphere or afterwards, at inner chamber effect one pressure fluid source, make to produce on fibre wall abrupt pressure reduction, thereby pressure fluid is through wall portion, makes most of Impurity removal in wall; Chinese patent (ZL 98125099.8) " a kind of cleaning method of external pressure hollow-fibre membrane and corresponding membrane assembly " adopts corresponding membrane module, backwash liquor is entered in inverted U external pressure hollow-fibre membrane and is carried out inverse osmosis cleaning by the mouth of pipe of membrane module lower end, another mouth of pipe in membrane module lower end injects in the lacuna of anti-compressed air outside inverted U external pressure hollow-fibre membrane and between membrane module housing, so that air oscillation cleaning is carried out in inverted U external pressure doughnut outside, inside and outside complete pair of films, carry out backwash and shake and wash simultaneously; Chinese patent (ZL 200710046708.0) " a kind of cleaning agent of cleaning hollow fiber ultrafiltration membrane and preparation method thereof that is applicable to " discloses a kind of cleaning agent and preparation method thereof, and this cleaning agent is applicable to the cleaning of ultrafiltration oily waste water, organic wastewater and protein-based milipore filter; United States Patent (USP) (US 20100018921A1) " Reverse osmosis water recover method " adopts and adds sulfurous acid as cleaning agent, then removes by filter continuously acidifying water, obtains clean reverse osmosis membrane; Japan Patent (WO 2005042133) " Hollow fiber membrane module; hollow fiber membrane module unit; and water treatment method " discloses a kind of hollow fiber film assembly and a kind of method for treating water that utilizes this membrane module, the method under pressure, make microorganism efficiently with hollow-fibre membrane Surface Contact, reach the object of cleaning filter membranes.The pollution filter membrane cleaning program that the patent that can find and document are mentioned, substantially all relate to and use strong acid or highly basic reagent cleaning filter membranes, clean the outer row of waste water and easily cause secondary environmental pollution problem, and easily filter membrane skin-material is caused to damage, and then affect the repetition strainability of filter membrane.Therefore, a kind of wastepaper pulping and papermaking comprehensive wastewater that this case proposes pollutes the chemical regeneration method of milipore filter, inapplicable strong acid or highly basic reagent, fast, efficient, environmental protection and low operation cost, Chemical cleaning and the regeneration of for wastepaper pulping and papermaking comprehensive wastewater, polluting specially milipore filter.So far, yet there are no the related process technology of utilizing chemical method recycled waste paper pulping and papermaking effluent to pollute milipore filter occurs.
Therefore, sternness increasingly in view of paper industry Environmental Protection Situation, for accelerating membrane separation technique in the application process in wastepaper pulping and papermaking comprehensive wastewater advanced treating field, and then realize reduction water outlet and pollute to reach country's " new standard " emission request, increase the target that circulating and recovering consumes to reduce clear water, exploitation is suitable for Chemical cleaning and the renovation process that wastepaper pulping and papermaking comprehensive wastewater pollutes milipore filter, has important practical significance.
Summary of the invention
For overcoming, utilize at present in membrane separation technique advanced treating wastepaper pulping and papermaking comprehensive wastewater process, because film pollutes the waste water flux causing, decline too fast, filter membrane replacing frequency is too high, and then cause the practical problems such as operating cost rising of film separation process, to improve cleaning efficiency, reduce secondary pollution, reduce running cost, the object of this invention is to provide a kind of chemical regeneration method that wastepaper pulping and papermaking comprehensive wastewater pollutes milipore filter.
For achieving the above object, technical scheme of the present invention is to adopt following steps:
1) milipore filter that wastepaper pulping and papermaking comprehensive wastewater pollutes adopts wetting its face of rayon balls wiping of running water, will be deposited on the soil release of polluting filter membrane surface, obtains the pollution milipore filter of physical cleaning;
2) by step 1) in the pollution milipore filter of the physical cleaning that obtains under the mechanical agitation of 200~300rpm, in the running water of 20~40 ℃, cross film pressure 0.1~0.2MPa ultrafiltration 5~10 minutes, obtain the pollution milipore filter that clear water cleans;
3) by step 2) in the pollution milipore filter that cleans of the clear water that obtains under the mechanical agitation of 200~300rpm, in the combined type cleaning flow process forming at the regeneration chemical reagent that are 0.1~0.4% by mass fraction of 20~40 ℃, cross film pressure 0.1~0.2MPa ultrafiltration 15~30 minutes, adopt running water to clean the regeneration chemical reagent that remains in above-mentioned milipore filter surface, finally obtain the milipore filter through chemical regeneration, regeneration chemical reagent is wherein selected from clorox, lauryl sodium sulfate, diethyl pentetic acid, polyethylene glycol is to two kinds in iso-octyl phenyl ether or two or more.
The combined type cleaning flow process that described regeneration chemical reagent forms is first in 0.4% liquor natrii hypochloritis of 20 ℃, crosses film pressure 0.1MPa ultrafiltration 30 minutes, adopts running water to clean 0.4% liquor natrii hypochloritis who remains in above-mentioned milipore filter surface; Then in the 0.1% diethyl pentetic acid solution of 20 ℃, cross film pressure 0.1MPa ultrafiltration 30 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned milipore filter surface; Last in 0.1% sodium dodecyl sulfate solution of 20 ℃, cross film pressure 0.1MPa ultrafiltration 30 minutes, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned milipore filter surface, finally obtain the milipore filter through chemical regeneration.
The combined type cleaning flow process that described regeneration chemical reagent forms is first in the 0.1% diethyl pentetic acid solution of 30 ℃, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned milipore filter surface; Then in 0.1% sodium dodecyl sulfate solution of 30 ℃, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned milipore filter surface; Finally 0.2% polyethylene glycol of 30 ℃ to iso-octyl phenyl ether solution in, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt clean 0.2% polyethylene glycol that remains in above-mentioned milipore filter surface of running water to iso-octyl phenyl ether solution, finally obtain the milipore filter through chemical regeneration.
The combined type cleaning flow process that described regeneration chemical reagent forms is first in 0.4% liquor natrii hypochloritis of 40 ℃, crosses film pressure 0.2MPa ultrafiltration 15 minutes, adopts running water to clean 0.4% liquor natrii hypochloritis who remains in above-mentioned milipore filter surface; Then in the 0.1% diethyl pentetic acid solution of 40 ℃, cross film pressure 0.2MPa ultrafiltration 15 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned milipore filter surface; In 0.1% sodium dodecyl sulfate solution of 40 ℃, cross film pressure 0.2MPa ultrafiltration 15 minutes afterwards, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned milipore filter surface; Finally 0.2% polyethylene glycol of 40 ℃ to iso-octyl phenyl ether in, cross film pressure 0.2MPa ultrafiltration 15 minutes, adopt the clean polyethylene glycol that remains in above-mentioned milipore filter surface of running water to iso-octyl phenyl ether solution, finally obtain the milipore filter through chemical regeneration.
Described milipore filter is a kind of in poly (ether sulfone) film, PVDF membrane, regenerated cellulose film, and its molecular cut off is 50~100kDa.
Compare with background technology, the beneficial effect that the present invention has is:
The milipore filter that the present invention pollutes for wastepaper pulping and papermaking comprehensive wastewater specially, a kind of brand-new Chemical cleaning and renovation process have been proposed, be conducive in utilizing membrane separation technique advanced treating wastepaper pulping and papermaking comprehensive wastewater process, maintain higher waste water flux, less filter membrane replacing, less disposal of pollutants and cheap operating cost, and then provide important supporting technology support for the practical application of membrane separation technique in wastepaper pulping and papermaking comprehensive wastewater advanced treating field.
Accompanying drawing explanation
Fig. 1 is new 50kDa regenerated cellulose milipore filter cross section field emission scanning electron microscope photo;
Fig. 2 is the field emission scanning electron microscope photo in the 50kDa regenerated cellulose milipore filter cross section of wastepaper pulping and papermaking comprehensive wastewater pollution;
Fig. 3 is the field emission scanning electron microscope photo through the 50kDa regenerated cellulose milipore filter cross section of chemical regeneration.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
1) the 100kDa polyvinylidene fluoride ultrafiltration film that wastepaper pulping and papermaking comprehensive wastewater pollutes adopts wetting its face of rayon balls wiping of running water, to be deposited on the soil release of polluting filter membrane surface, obtain the pollution 100kDa polyvinylidene fluoride ultrafiltration film of physical cleaning;
2) by step 1) in the pollution 100kDa polyvinylidene fluoride ultrafiltration film of the physical cleaning that obtains under the mechanical agitation of 300rpm, in the running water of 20 ℃, cross film pressure 0.1MPa ultrafiltration 10 minutes, obtain the pollution 100kDa polyvinylidene fluoride ultrafiltration film that clear water cleans;
3) by step 2) in the pollution 100kDa polyvinylidene fluoride ultrafiltration film that cleans of the clear water that obtains under the mechanical agitation of 300rpm, first in 0.4% liquor natrii hypochloritis of 20 ℃, cross film pressure 0.1MPa ultrafiltration 30 minutes, adopt running water to clean 0.4% liquor natrii hypochloritis who remains in above-mentioned 100kDa polyvinylidene fluoride ultrafiltration film surface; Then in the 0.1% diethyl pentetic acid solution of 20 ℃, cross film pressure 0.1MPa ultrafiltration 30 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned 100kDa polyvinylidene fluoride ultrafiltration film surface; Last in 0.1% sodium dodecyl sulfate solution of 20 ℃, cross film pressure 0.1MPa ultrafiltration 30 minutes, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned 100kDa polyvinylidene fluoride ultrafiltration film surface, finally obtain the 100kDa polyvinylidene fluoride ultrafiltration film through chemical regeneration.
Embodiment 2:
1) the 100kDa poly (ether-sulfone) ultrafiltration membrane that wastepaper pulping and papermaking comprehensive wastewater pollutes adopts wetting its face of rayon balls wiping of running water, will be deposited on the soil release of polluting filter membrane surface, obtains the pollution 100kDa poly (ether-sulfone) ultrafiltration membrane of physical cleaning;
2) by step 1) in the pollution 100kDa poly (ether-sulfone) ultrafiltration membrane of the physical cleaning that obtains under the mechanical agitation of 200rpm, in the running water of 30 ℃, cross film pressure 0.15MPa ultrafiltration 10 minutes, obtain the pollution 100kDa poly (ether-sulfone) ultrafiltration membrane that clear water cleans;
3) by step 2) in the pollution 100kDa poly (ether-sulfone) ultrafiltration membrane that cleans of the clear water that obtains under the mechanical agitation of 200rpm, first in the 0.1% diethyl pentetic acid solution of 30 ℃, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned 100kDa poly (ether-sulfone) ultrafiltration membrane surface; Then in 0.1% sodium dodecyl sulfate solution of 30 ℃, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned 100kDa poly (ether-sulfone) ultrafiltration membrane surface; Finally 0.2% polyethylene glycol of 30 ℃ to iso-octyl phenyl ether solution in, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt clean 0.2% polyethylene glycol that remains in above-mentioned 100kDa poly (ether-sulfone) ultrafiltration membrane surface of running water to iso-octyl phenyl ether solution, finally obtain the 100kDa poly (ether-sulfone) ultrafiltration membrane through chemical regeneration.
Embodiment 3:
1) the 50kDa regenerated cellulose milipore filter that wastepaper pulping and papermaking comprehensive wastewater pollutes adopts wetting its face of rayon balls wiping of running water, will be deposited on the soil release of polluting filter membrane surface, obtains the pollution 50kDa regenerated cellulose milipore filter of physical cleaning;
2) by step 1) in the pollution 50kDa regenerated cellulose milipore filter of the preliminary physical cleaning that obtains under the mechanical agitation of 250rpm, in the running water of 40 ℃, cross film pressure 0.2MPa ultrafiltration 5 minutes, obtain the pollution 50kDa regenerated cellulose milipore filter that clear water cleans;
3) by step 2) in the pollution 50kDa regenerated cellulose milipore filter that cleans of the clear water that obtains under the mechanical agitation of 250rpm, first in 0.4% liquor natrii hypochloritis of 40 ℃, cross film pressure 0.2MPa ultrafiltration 15 minutes, adopt running water to clean 0.4% liquor natrii hypochloritis who remains in above-mentioned 50kDa regenerated cellulose milipore filter surface; Then in the 0.1% diethyl pentetic acid solution of 40 ℃, cross film pressure 0.2MPa ultrafiltration 15 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned 50kDa regenerated cellulose milipore filter surface; In 0.1% sodium dodecyl sulfate solution of 40 ℃, cross film pressure 0.2MPa ultrafiltration 15 minutes afterwards, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned 50kDa regenerated cellulose milipore filter surface; Finally 0.2% polyethylene glycol of 40 ℃ to iso-octyl phenyl ether in, cross film pressure 0.2MPa ultrafiltration 15 minutes, adopt the clean polyethylene glycol that remains in above-mentioned 50kDa regenerated cellulose milipore filter surface of running water to iso-octyl phenyl ether solution, finally obtain through the 50kDa of chemical regeneration regenerated cellulose milipore filter.
Measure embodiment 1,2,3 and through the wastepaper pulping and papermaking comprehensive wastewater of chemical regeneration, pollute the pure water flux recovery rate of pure water flux the calculating regeneration filter membrane of milipore filter.Table 1 is by the wastepaper pulping and papermaking comprehensive wastewater of embodiment 1,2,3 chemical regenerations, to be polluted pure water flux measurement result and the corresponding pure water flux recovery rate of milipore filter.Known by data in table 1, adopt chemical regeneration method of the present invention, the pure water flux that can make wastepaper pulping and papermaking comprehensive wastewater pollute milipore filter returns to 86.4~98.5% of new film, cleaning performance is all better, and the conventional cleaning method that can be used as wastepaper pulping and papermaking comprehensive wastewater pollution milipore filter is used.
From embodiment 3, the field emission scanning electron microscope photo in the 50kDa regenerated cellulose milipore filter cross section of 3 chemical regenerations can be found out, through the present invention relates to chemical regeneration method, the regenerated cellulose milipore filter surface that wastepaper pulping and papermaking comprehensive wastewater can be polluted and inner void thereof clean comparatively clean, can be close to new regenerated cellulose milipore filter level.
Table 1
What more than enumerate is only specific embodiments of the invention.Obviously, the invention is not restricted to above embodiment, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (3)
1. wastepaper pulping and papermaking comprehensive wastewater pollutes a chemical regeneration method for milipore filter, it is characterized in that comprising the following steps:
1) milipore filter that wastepaper pulping and papermaking comprehensive wastewater pollutes adopts wetting its face of rayon balls wiping of running water, will be deposited on the soil release of polluting filter membrane surface, obtains the pollution milipore filter of physical cleaning;
2) by step 1) in the pollution milipore filter of the physical cleaning that obtains under the mechanical agitation of 200~300rpm, in the running water of 20~40 ℃, cross film pressure 0.1~0.2MPa ultrafiltration 5~10 minutes, obtain the pollution milipore filter that clear water cleans;
3) by step 2) in the pollution milipore filter that cleans of the clear water that obtains under the mechanical agitation of 200~300rpm, in the combined type cleaning flow process forming at the regeneration chemical reagent that are 0.1~0.4% by mass fraction of 20~40 ℃, cross film pressure 0.1~0.2MPa ultrafiltration 15~30 minutes, adopt running water to clean the regeneration chemical reagent that remains in above-mentioned milipore filter surface, finally obtain the milipore filter through chemical regeneration, regeneration chemical reagent is wherein selected from clorox, lauryl sodium sulfate, diethyl pentetic acid, polyethylene glycol is to two kinds in iso-octyl phenyl ether or two or more,
The combined type cleaning flow process that regeneration chemical reagent wherein forms is: first, in 0.4% liquor natrii hypochloritis of 20 ℃, cross film pressure 0.1MPa ultrafiltration 30 minutes, adopt running water to clean 0.4% liquor natrii hypochloritis who remains in above-mentioned milipore filter surface; Then in the 0.1% diethyl pentetic acid solution of 20 ℃, cross film pressure 0.1MPa ultrafiltration 30 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned milipore filter surface; Last in 0.1% sodium dodecyl sulfate solution of 20 ℃, cross film pressure 0.1MPa ultrafiltration 30 minutes, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned milipore filter surface, finally obtain the milipore filter through chemical regeneration;
Or be first in the 0.1% diethyl pentetic acid solution of 30 ℃, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned milipore filter surface; Then in 0.1% sodium dodecyl sulfate solution of 30 ℃, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned milipore filter surface; Finally 0.2% polyethylene glycol of 30 ℃ to iso-octyl phenyl ether solution in, cross film pressure 0.15MPa ultrafiltration 20 minutes, adopt clean 0.2% polyethylene glycol that remains in above-mentioned milipore filter surface of running water to iso-octyl phenyl ether solution, finally obtain the milipore filter through chemical regeneration.
Or be first in 0.4% liquor natrii hypochloritis of 40 ℃, cross film pressure 0.2MPa ultrafiltration 15 minutes, adopt running water to clean 0.4% liquor natrii hypochloritis who remains in above-mentioned milipore filter surface; Then in the 0.1% diethyl pentetic acid solution of 40 ℃, cross film pressure 0.2MPa ultrafiltration 15 minutes, adopt running water to clean the 0.1% diethyl pentetic acid solution that remains in above-mentioned milipore filter surface; In 0.1% sodium dodecyl sulfate solution of 40 ℃, cross film pressure 0.2MPa ultrafiltration 15 minutes afterwards, adopt running water to clean 0.1% sodium dodecyl sulfate solution that remains in above-mentioned milipore filter surface; Finally 0.2% polyethylene glycol of 40 ℃ to iso-octyl phenyl ether in, cross film pressure 0.2MPa ultrafiltration 15 minutes, adopt the clean polyethylene glycol that remains in above-mentioned milipore filter surface of running water to iso-octyl phenyl ether solution, finally obtain the milipore filter through chemical regeneration.
2. a kind of wastepaper pulping and papermaking comprehensive wastewater according to claim 1 pollutes the chemical regeneration method of milipore filter, it is characterized in that: described milipore filter is a kind of in poly (ether sulfone) film, PVDF membrane, regenerated cellulose film, and its molecular cut off is 50~100kDa.
3. a kind of wastepaper pulping and papermaking comprehensive wastewater according to claim 1 pollutes the chemical regeneration method of milipore filter, it is characterized in that: described milipore filter is a kind of in poly (ether sulfone) film, PVDF membrane, regenerated cellulose film, its molecular cut off 50kDa.
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