CN1817445A - Regeneration of rare-earth adsorbent after sewage denitrifying and dephosphor - Google Patents
Regeneration of rare-earth adsorbent after sewage denitrifying and dephosphor Download PDFInfo
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- CN1817445A CN1817445A CN 200610010634 CN200610010634A CN1817445A CN 1817445 A CN1817445 A CN 1817445A CN 200610010634 CN200610010634 CN 200610010634 CN 200610010634 A CN200610010634 A CN 200610010634A CN 1817445 A CN1817445 A CN 1817445A
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Abstract
A process for regenerating the RE adsorbent after it is used to remove N and P from sewage includes such steps as cyclic desorption with NaCl solution as regenerating solution while regulating pH=8-14, filtering, immersing it in the activating liquid prepared from same Re element for cyclic activating, filtering, drying and calcining.
Description
One, technical field: the present invention relates to contain the renovation process of the saturated rare-earth adsorbent of water contaminated ion, belong to the wastewater treating technology field.
Two, background technology: a kind of chemical reaction process that carries out between the contaminated ion in absorption method dependence adsorbent and the sewage is to reach the purpose of removal.This method is compared with the chemical coacervating precipitation method, produces mud hardly, and treatment facility is simple, and treatment effect is more stable; Compare with biochemical process, simple to operate, be easy to keep efficient and stable removal effect, and be easy to handle the contaminated ion of low concentration; Compare with electroosmose process, hyperfiltration, electrolysis, the way of distillation, method of soil decontamination special process method, have and build and operating cost is low, simple to operate, administer and maintain convenience.Sorbing material commonly used both at home and abroad mainly contains active carbon, activated alumina, silica gel, zeolite and synthetic zeolite etc.; But these sorbing materials have shortcomings such as poor stability, adsorption capacity is low, regeneration is frequent.
At publication number is to disclose a kind of method that makes spent sorbents regeneration among the CN1178135, and this method is: (a) Zn composition of spent sorbents with the presoma that comprises zinc oxide or zinc oxide contacted, thereby form a kind of contact composition; (b), thereby form a kind of contact composition of drying with said contact composition dry about 1 minute-Yue 24 hours time under the about 375 ℃ temperature of about 25-; And (c) with the contact composition of said drying in about 1 minute-Yue 24 hours time of about 400-800 ℃ temperature lower calcination, thereby form said reproducing adsorbent.
At publication number is the method that discloses the regeneration zeolite catalyst among the CN1469776A, this method is: " (1) uses the solvent wash zeolite catalyst; (2) zeolite catalyst after dry washing under-50 ℃ to the 250 ℃ temperature; (3) catalyst behind the heat drying; (4) by the catalyst after the inventive method regeneration heating; (5) catalyst after the regeneration that obtains in the cooling step (4), the catalyst that obtains in (6) regulating step (4) or (5) ".
Rare-earth adsorbent series has overcome the weakness of above sorbing material, but need be to the processing of regenerating of saturated rare-earth adsorbent series, can be recycling.Therefore, the invention solves saturated rare-earth adsorbent series regeneration problem, make that rare-earth adsorbent can be recycling, reduced the environmental improvement cost, the regulation effect of the rare-earth adsorbent after regeneration remains unchanged substantially, for the cost that reduces environmental improvement has great importance.
Three, summary of the invention: the renovation process that the purpose of this invention is to provide a kind of rare-earth adsorbent after sewage denitrifying and dephosphor, saturated rare-earth adsorbent obtains regeneration after desorption, filtration, dipping, filtration, drying and roasting operation, realized the recycling of rare-earth adsorbent, its adsorption capacity reaches more than 90% of former adsorption capacity.
The present invention is achieved through the following technical solutions:
1, desorption: the saturated rare-earth adsorbent that will be applied to waste water treatment is put into fixed bed reactors or the fluidized-bed reactor desorption that circulates and is handled, desorption conditions is: actified solution is the NaCl solution of concentration 0.5～3mol/L, the weight ratio of adsorbent and actified solution is 1: 50～70, first spent regeneration solution floods saturated rare-earth adsorbent in fixed bed reactors or fluidized-bed reactor, be that the actified solution of the 2～5m/h desorption that circulates is handled with linear speed again, regulate actified solution pH value between 8～14 with alkali lye in the process, desorption 3～4 hours;
2, filter: adsorbent and actified solution are carried out with distilled water rare-earth adsorbent being washed after the isolated by filtration, and to remove the actified solution of 30%～90% surface attachment, after desorption was handled, the desorption rate of saturated rare-earth adsorbent phosphorus reached more than 95%;
3, flood: the rare-earth adsorbent after desorption is filtered puts into fixed bed reactors or fluidized-bed reactor carries out the cyclic activation processing, treatment conditions are: use the rare earth element identical with rare-earth adsorbent to be mixed with the activating solution that concentration is 0.05～0.1wt%, the weight ratio of adsorbent and cyclic activation liquid is 1: 20～50, in fixed bed reactors or fluidized-bed reactor, flood rare-earth adsorbent with activating solution earlier, be that the activating solution of 2～5m/h carries out cyclic activation to rare-earth adsorbent and handles with linear speed again, regulate activating solution pH value 8～11 with alkali lye in the process, activate 3～4 hours, normal temperature left standstill dipping 4～6 hours then;
4, filter: the rare-earth adsorbent solution after will flooding carries out isolated by filtration, must activate the back rare-earth adsorbent, and filtrate cycle is used;
5, drying and roasting: the rare-earth adsorbent after will activating is put into roaster, is under 100～120 ℃ in temperature, dry half an hour, and then heat up with per minute 10-20 ℃ heating rate, carried out roasting 0.5～2 hour, final calcination temperature is 300～550 ℃, the rare-earth adsorbent that must regenerate.
Major advantage of the present invention has:
(1) the invention solves the recycling problem of saturated rare-earth adsorbent, reduced treatment cost.
(2) can be recycling behind the saturated rare-earth adsorbent process step for regeneration of the present invention, regeneration rare-earth adsorbent adsorption capacity reaches more than 90% of former adsorption capacity.
(3) renovation process of the present invention can reclaim the material of saturated rare-earth adsorbent desorption, realizes the purpose of changing waste into resources and harmless treatment.
Four, description of drawings
Fig. 1 is a process chart of the present invention.
Fig. 2 is rare earth modified front and back and regeneration back spectrogram (IR).
Five, the specific embodiment:
Embodiment 1:
Preparation NaCl concentration is the desorption and regeneration solution of 1mol/L; With particle diameter is that the phosphorous saturated rare-earth adsorbent of 100 orders～180 order appendix lanthanum ions is put into fluidized-bed reactor, with linear speed in the fluidized-bed reactor is that the above-mentioned actified solution of the 4m/h desorption that circulates is handled, the weight ratio of this adsorbent and circular regeneration solution is 1: 60, transferring actified solution pH value with alkali lye is 10.5, desorption 3.5 hours; Through after the desorption, the desorption rate of saturated rare-earth adsorbent phosphorus can reach 96%, then above solid-liquid is carried out isolated by filtration, with distilled water rare-earth adsorbent is washed at last, to remove the actified solution of 90% surface attachment; Rare-earth adsorbent after the desorption filtration is put into fluidized-bed reactor, with linear speed in the fluidized-bed reactor is that 4m/h, lanthanum ion concentration are that the solution of 0.08wt% carries out cyclic activation and handles, the weight ratio of this adsorbent and cyclic activation solution is 1: 50, use the lye pH adjustment value, making the pH value of solution value is 10, soak time is 2 hours, and normal temperature left standstill dipping 4 hours then; Rare-earth adsorbent solution behind the dipping is carried out isolated by filtration, and filtrate cycle is used; Rare-earth adsorbent after filtering is put into vertical tubular type roaster, and temperature is 100 ℃, dry half an hour, and then heat up with the heating rate of 15 ℃ of per minutes, final calcination temperature is 500 ℃, roasting 1 hour; After the cooling, again through screening, the rare-earth adsorbent that obtains regenerating.
Handle with the rare-earth adsorbent of this regeneration and to contain the phosphorous chemical industry waste water that phosphorus concentration is 200mg/L, as above behind the circular regeneration 20 times, then the adsorption capacity to phosphorus still can reach more than the 20mg/g.Adsorbent after the regeneration and fresh adsorbent, raw material zeolite adsorbents contrast situation are seen Fig. 2.
Embodiment 2:
Preparation NaCl concentration is the desorption and regeneration solution of 2mol/L; The saturated rare-earth adsorbent of nitrogenous phosphorus of diameter 2.5-10mm, height 3-20mm cylinder appendix cerium ion is put into fixed bed reactors, with linear speed in the fixed bed reactors is that the above-mentioned actified solution of the 3m/h desorption that circulates is handled, the weight ratio of this adsorbent and circular regeneration solution is 1: 60, use the lye pH adjustment value, making actified solution pH value is 12; Desorption 4 hours; Through after the desorption, the desorption rate of saturated rare-earth adsorbent nitrogen can reach 92%, and the desorption rate of phosphorus can reach 95%, then above solid-liquid is carried out isolated by filtration, with distilled water rare-earth adsorbent is washed at last, to remove the actified solution of 80% surface attachment; Rare-earth adsorbent after the desorption filtration is put into fixed bed reactors, with linear speed in the fixed bed reactors is that 4m/h, cerium ion concentration are that the activating solution of 0.06wt% carries out cyclic activation and handles, the weight ratio of this adsorbent and cyclic activation solution is 1: 50, use the lye pH adjustment value, making activating solution pH value is 11, soak time is 3 hours, and normal temperature left standstill dipping 5 hours then; Appendix cerium ion rare-earth adsorbent solution behind the dipping is carried out isolated by filtration, and filtrate cycle is used; Rare-earth adsorbent after filtering is put into the van-type roaster, carry out drying earlier and handle, baking temperature is 110 ℃, dry half an hour, and then heat up with the heating rate of 20 ℃ of per minutes, final calcination temperature is 500 ℃, roasting 1 hour after the cooling, obtains required rare-earth adsorbent.
Rare-earth adsorbent with this regeneration carries out the dephosphorization of city domestic sewage advanced nitrogen, and as above behind the circular regeneration 20 times, then the adsorption capacity to nitrogen still can reach more than the 5mg/g, still can reach more than the 15mg/g the adsorption capacity of phosphorus.
Embodiment 3:
Preparation NaCl concentration is the desorption and regeneration solution of 3mol/L; The saturated rare-earth adsorbent of chromium (VI) that contains of diameter 2.5-8mm spheroid appendix lanthanum ion is put into fixed bed reactors, with linear speed in the fixed bed reactors is that the above-mentioned actified solution of the 2.5m/h desorption that circulates is handled, the weight ratio of this adsorbent and circular regeneration solution is 1: 55, use the lye pH adjustment value, making actified solution pH value is 11, desorption 4 hours; Through after the desorption, the desorption rate of saturated rare-earth adsorbent chromium can reach 98%, then above solid-liquid is carried out isolated by filtration, with an amount of distilled water solid is washed at last, to remove the actified solution of surface attachment; Rare-earth adsorbent after the desorption filtration is put into fixed bed reactors, with linear speed in the fixed bed reactors is that 3m/h, lanthanum ion concentration are that the activating solution of 0.1wt% carries out cyclic activation and handles, the weight ratio of this adsorbent and cyclic activation liquid is 1: 30, use the lye pH adjustment value, making activated solution pH value is 11, soak time is 2.5 hours, and normal temperature left standstill dipping 6 hours then; Appendix lanthanum ion rare-earth adsorbent solution behind the dipping is carried out isolated by filtration, and filtrate cycle is used; Rare-earth adsorbent after filtering is put into the swinging roaster, carry out drying earlier and handle, baking temperature is 120 ℃, dry half an hour, and then heat up with the heating rate of 20 ℃ of per minutes, final calcination temperature is 550 ℃, roasting 1.5 hours after the cooling, obtains required original rare-earth adsorbent.
Handle with the rare-earth adsorbent of this regeneration that to contain chromium (VI) concentration be the electroplating wastewater of 250mg/L, as above behind the circular regeneration 20 times, then the adsorption capacity to chromium still can reach more than the 5mg/g.
Claims (3)
1, a kind of renovation process of rare-earth adsorbent after sewage denitrifying and dephosphor is characterized in that: invention is finished according to the following steps,
1), desorption: the saturated rare-earth adsorbent that will be applied to waste water treatment is gone into the reactor desorption that circulates and is handled, desorption conditions is: actified solution is the NaCl solution of concentration 0.5～3mol/L, the weight ratio of adsorbent and actified solution is 1: 50～70, first spent regeneration solution floods saturated rare-earth adsorbent in reactor, be that the actified solution of the 2～5m/h desorption that circulates is handled with linear speed again, regulate actified solution pH value between 8～14 with alkali lye in the process, desorption 3～4 hours;
2), filter: adsorbent and actified solution are carried out with distilled water rare-earth adsorbent being washed after the isolated by filtration;
3), dipping: the rare-earth adsorbent after the desorption filtration is gone into to carry out in the reactor cyclic activation handle, treatment conditions are: use the rare earth element identical with saturated rare-earth adsorbent to be mixed with the activating solution that concentration is 0.05～0.1wt%, the weight ratio of rare-earth adsorbent and activating solution is 1: 20～50, in reactor, flood rare-earth adsorbent with activating solution earlier, be that the activating solution of 2～5m/h carries out cyclic activation to rare-earth adsorbent and handles with linear speed again, regulate activating solution pH value 8～11 with alkali lye in the process, activate 3～4 hours, normal temperature left standstill dipping 4～6 hours then;
4), filter: the rare-earth adsorbent solution after will flooding carries out isolated by filtration, must activate the back rare-earth adsorbent, and filtrate cycle is used;
5), drying and roasting: the rare-earth adsorbent after will activating is put into roaster, is under 100～120 ℃ in temperature, dry half an hour, and then heat up with per minute 10-20 ℃ heating rate, carried out roasting 0.5～2 hour, final calcination temperature is 300～550 ℃, the rare-earth adsorbent that must regenerate.
2, the renovation process of rare-earth adsorbent after sewage denitrifying and dephosphor according to claim 1 is characterized in that: described saturated rare-earth adsorbent be the saturated rare-earth adsorbent of nitrogenous phosphorus of the phosphorous saturated rare-earth adsorbent of particle diameter 100 orders～180 order appendix lanthanum ions or diameter 2.5-10mm, height 3-20mm cylinder appendix cerium ion or diameter 2.5-8mm spheroid appendix lanthanum ion contain the saturated rare-earth adsorbent of chromium.
3, the renovation process of rare-earth adsorbent after sewage denitrifying and dephosphor according to claim 1 is characterized in that: described reactor is fixed bed reactors or fluidized-bed reactor.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103418359A (en) * | 2013-07-11 | 2013-12-04 | 江苏华杉环保科技有限公司 | Regeneration method for denitrification filter material adsorbing ammonia nitrogen |
| CN104710081A (en) * | 2015-03-18 | 2015-06-17 | 河海大学 | Sewage nitrogen and phosphorus removal method and device |
| CN104971687A (en) * | 2015-07-20 | 2015-10-14 | 北京宝鸿锐科环境科技有限公司 | Efficient compound iron-based phosphorous-removing adsorbent as well as preparation method, application method and regeneration method thereof |
| CN110152638A (en) * | 2018-02-26 | 2019-08-23 | 彭万喜 | A kind of regeneration method of high-efficiency adsorbent |
| CN111432911A (en) * | 2017-10-01 | 2020-07-17 | 艾博森有限公司 | Method of recycling saturated active sorbent of a filter module |
-
2006
- 2006-01-17 CN CN 200610010634 patent/CN100525899C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103418359A (en) * | 2013-07-11 | 2013-12-04 | 江苏华杉环保科技有限公司 | Regeneration method for denitrification filter material adsorbing ammonia nitrogen |
| CN104710081A (en) * | 2015-03-18 | 2015-06-17 | 河海大学 | Sewage nitrogen and phosphorus removal method and device |
| CN104971687A (en) * | 2015-07-20 | 2015-10-14 | 北京宝鸿锐科环境科技有限公司 | Efficient compound iron-based phosphorous-removing adsorbent as well as preparation method, application method and regeneration method thereof |
| CN111432911A (en) * | 2017-10-01 | 2020-07-17 | 艾博森有限公司 | Method of recycling saturated active sorbent of a filter module |
| CN110152638A (en) * | 2018-02-26 | 2019-08-23 | 彭万喜 | A kind of regeneration method of high-efficiency adsorbent |
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