CN1803274A - Preparation method of adsorption agent for sewage denitrification and dephosphorization - Google Patents
Preparation method of adsorption agent for sewage denitrification and dephosphorization Download PDFInfo
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- CN1803274A CN1803274A CN200510048671.6A CN200510048671A CN1803274A CN 1803274 A CN1803274 A CN 1803274A CN 200510048671 A CN200510048671 A CN 200510048671A CN 1803274 A CN1803274 A CN 1803274A
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- 239000010865 sewage Substances 0.000 title claims abstract description 18
- 238000001179 sorption measurement Methods 0.000 title claims description 22
- 238000002360 preparation method Methods 0.000 title claims description 10
- 239000003463 adsorbent Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- -1 rare-earth hydroxide Chemical class 0.000 claims abstract description 17
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 16
- 239000012065 filter cake Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 11
- 239000010457 zeolite Substances 0.000 claims abstract description 11
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 238000007598 dipping method Methods 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 claims description 4
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 3
- YXEUGTSPQFTXTR-UHFFFAOYSA-K lanthanum(3+);trihydroxide Chemical compound [OH-].[OH-].[OH-].[La+3] YXEUGTSPQFTXTR-UHFFFAOYSA-K 0.000 claims description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 2
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 26
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 13
- 229920006395 saturated elastomer Polymers 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract 2
- 239000000463 material Substances 0.000 abstract 2
- 230000000274 adsorptive effect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 150000002910 rare earth metals Chemical class 0.000 abstract 1
- 238000005245 sintering Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 16
- 239000011574 phosphorus Substances 0.000 description 16
- 229910052698 phosphorus Inorganic materials 0.000 description 16
- 239000002351 wastewater Substances 0.000 description 12
- 239000002352 surface water Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 6
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012851 eutrophication Methods 0.000 description 3
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000011953 bioanalysis Methods 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000033444 hydroxylation Effects 0.000 description 2
- 238000005805 hydroxylation reaction Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- DJFBJKSMACBYBD-UHFFFAOYSA-N phosphane;hydrate Chemical compound O.P DJFBJKSMACBYBD-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910001387 inorganic aluminate Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a making method of denitrifying dephosphorizing rare-earth adsorbent for sewage, which comprises the following steps: soak 60-100-order powdery zeolite, diatomite or aluminum oxide in the distilled water for 15-30 min; drying the material at 100-430 deg C for 1-2 hours after filtering; adding the material in the prepared rare-earth hydroxide at 1: 40-60 solid-liquid weight ratio; stirring for 45-60 min at atmosphere temperature; stewing immersion for 15-20 h; filtering the solution to obtain filter cake and filtrate; sintering the filter cake at 300-600 deg C for 0.5-2 h; sifting to obtain 0.3-0.5 nm aperture of adsorbent. The invention can remove nitrogen by 15-20mg/g and squama by 22-25mg/g, which regenerates the saturated adsorptive adsorbent through alkaline.
Description
One, technical field: the present invention relates to a kind of preparation method of adsorption agent for sewage denitrification and dephosphorization, belong to the purification of waste water processing technology field.
Two, background technology: studying for a long period of time shows, the nitrogen in the sanitary sewage, phosphorus are to cause the particularly main cause of lake eutrophication of surface water body.The national requirements sanitary sewage must be through handling before entering surface water body, but what the sanitary sewage that enters surface water body after sewage treatment plant handles was carried out is GB8978-1996 " integrated wastewater discharge standard ", and the surface water execution is GB3838-2002 " ground water environment quality standard ", concentration of nitrogen and phosphorus between two standards differs tens times, therefore, although sanitary sewage has passed through processing, but because the difference of final concentration of treatment, the sanitary sewage that makes sewage treatment plant discharge still is the primary pollution source of surface water body eutrophication.
Simultaneously, limitation in view of existing sewage treatment plant two stage treatment technology level, it is very difficult significantly to improve nitrogen, tp removal rate, therefore, for being the sewage treatment plant of final receiving water body with surface water body, should take efficient advanced nitrogen dephosphorization process, strengthen removal, sewage disposal be met the water quality requirement of the surface water body of receiving to water outlet nutrients nitrogen, phosphorus.
The method of known denitrogenation of waste water dephosphorization mainly contains neutralization precipitation method, bioanalysis and absorption method.Neutralisation need add a large amount of lime and coagulant, produce and to be difficult to the mud handled in a large number, cause secondary pollution easily, and be difficult to thoroughly eliminate pollution [the Design Manual:Phosphorus Removal.EPA TechnologyTranster of phosphorus-containing wastewater to environment, EPA/625/1-87/001,1987].Bioanalysis dephosphorization process flow process complexity, operation stability is relatively poor, the operation strictness, be subjected to the temperature, acid-base value etc. of waste water to influence big, to organic concentration in the waste water (BOD) dependence very strong [Gu Xiasheng, biological wastewater treatment mathematic(al) mode. Beijing: publishing house of Tsing-Hua University, 1993].Absorption method has overcome these shortcomings, can remove nitrogen and phosphorus simultaneously again, is one of the most promising denitrogenation of waste water phosphorus removing method at present.
Known traditional denitrogenation dephosphorizing adsorbent mainly contains activated alumina, active carbon, zeolite etc.Ning Ping has carried out the comparative study of inorganic phosphorated pollutant adsorption capacity to active carbon, activated alumina, find that activated alumina is 10mg/g to phosphatic adsorption capacity in the water, and active carbon only is the peaceful equality of 2mg/g[, non-ferrous metal, 54 (1), 2002,3].Yuan Junsheng [Yuan Junsheng etc., Techniques and Equipment for Environmental Pollution Control, (12), 2002,3] has studied the method for removing ammonia nitrogen in the trade effluent with zeolite.The result shows that the zeolite adsorption capacity to ammonia nitrogen under acid condition after the salt activation is 12.96mg/g to the maximum.Zhang Lanquan [Zhang Lanquan etc., Lanzhou Railway College's journal, 18 (2), 1999,6] carries out modification with inorganic aluminate, magnesium salts to zeolite and is prepared into the zeolite compound adsorbent, and the dephosphorization adsorption capacity is 15mg/g.These adsorbents all exist can only remove ammonia nitrogen or phosphorus separately, can not remove ammonia nitrogen and phosphorus in the water simultaneously, and in addition, the adsorption capacity of adsorbent is also lower.For these reasons, seek a kind of adsorbent and carry out denitrogenation dephosphorizing to substitute traditional adsorbents such as activated alumina, active carbon, significant to the eutrophication of control surface water body.
Three, summary of the invention: the objective of the invention is at the nitrogen in the waste water, phosphorus, a kind of preparation method of adsorption agent for sewage denitrification and dephosphorization is provided, a kind of with in raw material zeolite, diatomite, the aluminium oxide, obtain the adsorbent of aperture 0.3nm～0.5nm after activated, dipping, the calcination process, this adsorbent can remove nitrogen and the phosphorus in the decontaminated water simultaneously, adsorption capacity to ammonia reaches 15-20mg/g, and the adsorption capacity of phosphorus is reached 22-25mg/g.
The present invention is achieved through the following technical solutions:
(1) preparation of rare-earth hydroxide solution:
With a kind of being dissolved in the water in lanthanum nitrate, cerous nitrate, lanthanum chloride, the cerium chloride, be made into the rare-earth ion solution that concentration expressed in percentage by weight is 0.25～0.5wt%, regulate the pH value with alkali lye in the solution that preparation is finished, making the pH value of solution value is 8～11, generates rare-earth hydroxide solution;
(2) activation of raw material:
Raw material is a kind of in granularity 60-100 purpose powdery zeolite, diatomite, the aluminium oxide, and raw material was soaked in distilled water 15～30 minutes, filter the back and under 100 ℃～130 ℃ temperature, dried 1～2 hour, to water content less than 5%;
(3) dipping of adsorbent:
Raw material behind overactivation adds in the rare-earth hydroxide solution for preparing according to 1: 40～60 solid-liquid weight ratio, normal temperature stirred 45～60 minutes down, left standstill dipping 15～20 hours, and solution is filtered, obtain filter cake and filtrate, filtrate is returned in the rare-earth hydroxide solution and is re-used;
(4) roasting of adsorbent:
Place metallurgical furnace to carry out roasting filter cake, temperature is 300 ℃～600 ℃, and the time is 0.5～2 hour, and roasting is after screening obtains the adsorbent of aperture 0.3nm～0.5nm.
Know-why of the present invention:
Rare earth oxide is having under the situation of water, and surface metal ion at first tends to the water of coordination molecule, and the disassociation chemisorption of hydrone causes surface hydroxylation.But this surface hydroxylation makes the rare earth oxide positively charged in the aqueous solution, also can be electronegative, charged character be decided by the pH value of place solution.Hydroxylated oxide surface is positive electricity or negative electricity state because of protonated or non-protonization, with electrostatic attraction absorption yin, yang ion, generates complex compound.Be attended by ion exchange simultaneously.One pH value is arranged between the positive and negative electric charge of particle band, under this pH value, the particle neutral, this state is called the isoelectric point state, and this pH value is called the isoelectric point of oxide.The isoelectric point of rare earth oxide is generally 9～10, and positively charged in sour environment with phosphate anion electrically absorption takes place, and generates the rare-earth phosphorate complex compound, and hydroxyl is replaced simultaneously, and the pH value of solution value is raise.
Raw material is in the oven dry of adsorbent preparation, roasting process, and the aperture increases, and adsorbent is when removing ammonia nitrogen, and the cation in the structure and ammonia nitrogen generation ion-exchange are with removal nitrogen.
The present invention has the following advantages:
1, carrier in the adsorbent and active material obtain utilizing simultaneously, both can remove cation, can remove anion again.
2, the adsorbent of absorption after saturated can desorb by dipping by lye, makes the adsorbent recycling use.
3, the pH value of waste water was 4～6 o'clock adsorbent denitrogenation dephosphorizing best results, and this is acidity with the phosphate fertilizer industrial wastewater and conforms to, and waste water reaches emission request through pH value after the sorbent treatment between 8～9.This makes the import waste water and the pH value of outlet waste water all need not add acid or add the alkali adjusting.
4, adsorbent is to the adsorption capacity height of nitrogen, phosphorus, can reach 20mg/g to the adsorption capacity maximum of nitrogen, can reach 25mg/g to the adsorption capacity maximum of phosphorus.
5, the adsorbent of absorption after saturated is behind alkali liquid regeneration, and adsorption capacity only reduces by 6%～7%.
Four, the specific embodiment:
Example one: lanthanum nitrate is dissolved in the water, is made into the rare-earth ion solution that concentration expressed in percentage by weight is 0.3wt%, regulate the pH value with alkali lye in this solution, making the pH value of solution value is 9, has this moment lanthanum hydroxide to generate in the solution; Raw material is a granularity 60-100 purpose powdery zeolite, soaks in distilled water 20 minutes, filters back oven dry 1-2 hour under 100 ℃～130 ℃ temperature, to water content less than 5%; Raw material behind overactivation adds in the lanthanum hydroxide solution for preparing according to 1: 50 solid-liquid weight ratio, and normal temperature stirred 45 minutes down, left standstill dipping 17 hours, and solution is filtered, and obtained filter cake and filtrate; Place Muffle furnace to carry out roasting filter cake, temperature is 550 ℃, and the time is 1 hour, and roasting is after screening obtains the adsorbent of aperture 0.3nm～0.5nm.
Be used to handle the solution that total phosphorus concentration is 40mg/L, the adsorption capacity of phosphorus is reached 22～25mg/g.Adsorb the most desorption of adsorbent phosphorus behind dipping by lye after saturated, be used further in the adsorption treatment water phosphorus adsorption capacity 6-7% that only descends.
Example two: cerous nitrate is dissolved in the water, is made into the rare-earth ion solution that concentration expressed in percentage by weight is 0.4wt%, regulate the pH value with alkali lye in this solution, making the pH value of solution value is 10, has this moment cerium hydroxide to generate in the solution; Raw material is a granularity 60-100 purpose konilite, soaks in distilled water 30 minutes, filters back oven dry 1-2 hour under 100 ℃～130 ℃ temperature, to water content less than 5%; Raw material behind overactivation adds in the cerium hydroxide solution for preparing according to 1: 60 solid-liquid weight ratio, and normal temperature stirred 45 minutes down, left standstill dipping 20 hours, and solution is filtered, and obtained filter cake and filtrate; Place Muffle furnace to carry out roasting filter cake, temperature is 500 ℃, and the time is 1 hour, and roasting is after screening obtains the adsorbent of aperture 0.3nm～0.5nm.
Be used to handle the solution that total nitrogen concentration is 20mg/L, adsorption capacity is for can reach 15～18mg/g.
Claims (3)
1, a kind of preparation method of adsorption agent for sewage denitrification and dephosphorization, it is characterized in that: method is finished according to the following steps,
(1) with a kind of being dissolved in the water in lanthanum nitrate, cerous nitrate, lanthanum chloride, the cerium chloride, be made into the rare-earth ion solution that concentration expressed in percentage by weight is 0.25～0.5wt%, regulating pH with alkali lye in this solution is 8～11, generates rare-earth hydroxide solution;
(2) activation of raw material is to be a kind of in 60-100 purpose powdery zeolite, diatomite, the aluminium oxide with granularity, soaks in distilled water 15～30 minutes, filter the back and under 100 ℃～130 ℃ temperature, dried 1～2 hour, to water content less than 5%;
(3) raw material behind overactivation adds in the rare-earth hydroxide solution for preparing according to 1: 40～60 solid-liquid weight ratio, normal temperature stirred 45～60 minutes down, left standstill dipping 15～20 hours, and solution is filtered, obtain filter cake and filtrate, filtrate is returned in the rare-earth hydroxide solution and is re-used;
(4) filter cake is placed metallurgical furnace carry out roasting, temperature is 300～600 ℃, and the time is 0.5～2 hour, and roasting is after screening obtains the adsorbent of aperture 0.3nm～0.5nm.
2, the preparation method of adsorption agent for sewage denitrification and dephosphorization according to claim 1, it is characterized in that: lanthanum nitrate is dissolved in the water, be made into the rare-earth ion solution that concentration expressed in percentage by weight is 0.3wt%, regulate the pH value with alkali lye in this solution, making the pH value of solution value is 9; Raw material is a granularity 60-100 purpose powdery zeolite, soaks in distilled water 20 minutes, filters back oven dry 1-2 hour under 100～130 ℃ of temperature, to water content less than 5%; Raw material behind overactivation adds in the lanthanum hydroxide solution for preparing according to 1: 50 solid-liquid weight ratio, and normal temperature stirred 45 minutes down, left standstill dipping 17 hours, and solution is filtered, and obtained filter cake and filtrate; Place Muffle furnace to carry out roasting filter cake, temperature is 550 ℃, and the time is 1 hour, and roasting is after screening obtains the adsorbent of aperture 0.3nm～0.5nm.
3, the preparation method of adsorption agent for sewage denitrification and dephosphorization according to claim 1, it is characterized in that: cerous nitrate is dissolved in the water, be made into the rare-earth ion solution that concentration expressed in percentage by weight is 0.4wt%, in this solution, regulate the pH value with alkali lye, making the pH value of solution value is 10, has this moment cerium hydroxide to generate in the solution; Raw material is a granularity 60-100 purpose konilite, soaks in distilled water 30 minutes, filters back oven dry 1-2 hour under 100～130 ℃ of temperature, to water content less than 5%; Raw material behind overactivation adds in the cerium hydroxide solution for preparing according to 1: 60 solid-liquid weight ratio, and normal temperature stirred 45 minutes down, left standstill dipping 20 hours, and solution is filtered, and obtained filter cake and filtrate; Place Muffle furnace to carry out roasting filter cake, temperature is 500 ℃, and the time is 1 hour, and roasting is after screening obtains the adsorbent of aperture 0.3nm～0.5nm.
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| CN101306850B (en) * | 2008-07-09 | 2010-09-29 | 昆明铜龙科技开发有限公司 | Composite high-efficiency diatomaceous earth purifier and preparation method |
| CN102173496A (en) * | 2011-03-25 | 2011-09-07 | 中国科学院南京土壤研究所 | Phosphorous removing agent for wastewater produced during producing organophosphorus pesticides and preparation method thereof |
| CN102180535A (en) * | 2011-03-25 | 2011-09-14 | 中国科学院南京土壤研究所 | Method for removing phosphorus in organophosphorus pesticide waste water by using metal compound complex mineral material |
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2005
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