CN102774929A - Method for recovering phosphor from eutrophic water - Google Patents
Method for recovering phosphor from eutrophic water Download PDFInfo
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- CN102774929A CN102774929A CN2012102314841A CN201210231484A CN102774929A CN 102774929 A CN102774929 A CN 102774929A CN 2012102314841 A CN2012102314841 A CN 2012102314841A CN 201210231484 A CN201210231484 A CN 201210231484A CN 102774929 A CN102774929 A CN 102774929A
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Abstract
The invention discloses a method for recovering phosphor from eutrophic water. The method comprises the following steps of: (1) pretreating resin to enable the resin to be positioned in a known OH<-> type ionic form; (2) feeding the pretreated resin into a container to form a resin bed layer, introducing the eutrophic water and intercepting the phosphor in the water to the resin by carrying out ion exchange on an anionic group in the resin and a phosphor-containing group in the water; (3) desorbing the resin adsorbing the phosphor to obtain a phosphor-enriched solution; and (4) regenerating the desorbed resin. According to the method disclosed by the invention, the eutrophic water quality is used as a phosphor source, an anionic exchange group is endowed for the resin by pretreating the resin, the resin is used for treating the eutrophic water quality, the phosphor is adsorbed from the water, and thus the eutrophic water quality is purified and the improvement on an ecological environment is promoted. According to the method, the phosphor is thoroughly separated from the water and recovered; and a high-concentration and phosphor-enriched desorption solution can be used as a raw material of phosphor fertilizer, and thus the recycling and sustainable production of the phosphor are realized, finally the resin can be regenerated and further the effect of recycling is achieved.
Description
Technical field
The present invention relates to a kind of method that from eutrophic water, reclaims phosphorus.
Background technology
Phosphorus is common elements, is about 0.118% at the weight percentage of the earth's crust.Phosphorus all occurs with various phosphatic forms at nature.Being present in cell, bone and the tooth, is the important composition composition of plant-animal and needed by human, in the vital movement of cell, plays keying action, and just often the people need replenish 1.4g phosphorus every day from water and food.Simultaneously, phosphorus still is a kind of indispensable valuable source in industrial and agricultural production and the development, is widely used in smelting, synthetic detergent, agricultural chemicals, chemical fertilizer, the agrochemical industrial production.Yet phosphorus excessive uses and discharges the frequent generation that causes body eutrophication, red tide.According to 25 investigation that carry out in big-and-middle-sized lake in the whole nation, the lake of the eutrophication that become reaches 92%, wherein, accounts for more than 56% of lake of statistics because of nitrogen, phosphorus pollute the lake that causes eutrophication, especially with Taihu Lake, Dian Chi for.Body eutrophication all causes tens yuan loss every year to China's fishery, the taking place frequently of " wawter bloom ", " red tide ", and serious threat is to the supply and the fish production of tap water; Aggravated the situation of China's water quality property lack of water; Seriously restrict economic construction and social development, therefore, removed the nutritive salt in the water body; Phosphoric acid salt particularly becomes the key of effective control body eutrophication.
Meanwhile, phosphorus ore is again tellurian limited resources, and deficient day by day and the enrichment of phosphorus in water surrounding of land phosphate rock resource have formed a pair of contradiction.In order to address this problem, from eutrophication water, to remove phosphorus and reclaim phosphorus and seem particularly necessary.The present invention just is being based on this thinking; Eutrophic water as a kind of new phosphor resource that contains; Through ion exchange resin phosphorus in the water is adsorbed, removes and reclaims, not only can solve water pollution, make water quality be purified the ecological functions of recovering water body; And isolated phosphorus can be used as the phosphate fertilizer raw material, carries out the recycle of phosphorus.
A lot of countries are studied the problem that water body produces eutrophication to phosphorus, and have proposed the control corresponding method.Ion exchange method receives extensive attention as a kind of less energy-consumption, resource utilization wastewater processing technology, both at home and abroad for the research of sorbent material, mainly concentrates on three directions of natural materials and waste residue, activated alumina and modifier thereof and synthetic sorbent material at present.
(1) natural materials and waste residue.Many clay minerals (like zeolite, wilkinite, polynite and vermiculite) and industrial residue (like blast-furnace slag, flyash and the red stone mine tailing) phosphate anion in can planar water.
People such as Hengpeng Ye have reported that modified paligorskite is used for removing the phosphatic experimental study of solution.Result of study shows, the polygorskite after the modification because the change of surface mass structure, thereby has had the phosphorus loading capacity of phosphorus adsorptive power and Geng Gao more fast; Absorption to phosphorus simultaneously has high selectivity, yet for adsorbed phosphorus, its desorption has only 10-13%, comparatively difficulty; Adsorption process meets Freundlish adsorption isotherm and Elovich kinetics of adsorption equation more.
Le Zeng etc. has studied the adsorption and dephosphorization performance of red stone mine tailing, and the result shows, when adsorption temp is 35 ℃, when pH is 6.6-6.8, can obtain 71% dephosphorizing rate.
People such as Liu Lina studied three kinds common in, the phosphorus characterization of adsorption of low calcium fly ash.Research shows: the equal accords with Langmuir equation of absorption reaction, loading capacity reaches 20.49,23.15 and 6.54 mg/g respectively.All can reach the phosphorus adsorption equilibrium within the 30min, cement-water ratio has considerable influence to the phosphorus adsorption effect.Three kinds of flyash are relatively poor to the direct removal effect of lightly eutrophicated city appearance water body; Wherein two kinds of flyash demonstrate good direct removal effect to phosphorus in the severe eutrophication city landscape water body, have future in engineering applications.Flyash contains CaO, Na
2O, K
2Alkaline matters such as O cause after treatment the pH value to surpass emission standard, need take to reduce the countermeasure of pH value in the practical engineering application.
(2) activated alumina and modifier thereof.Activated alumina is the material of a kind of porous, high degree of dispersion, and very big specific surface area is arranged, and its micropore surface has strong adsorptive power, be a kind of research relatively thoroughly and obtain the dephosphorization adsorbent of practical application.
Arne Genz etc. study the bio-chemical effluent of activated alumina and the low phosphorus concentration of ironic hydroxide associating adsorption treatment.The result shows, reaches 8000 when handling bed volume with ironic hydroxide, handles bed volume with activated alumina and reaches at 4000 o'clock, and water outlet residual phosphorus amount can drop to 50 μ g/L.
Donnert uses activated alumina to build a day processing 500m for certain fish pond water
3Adsorption bed, make phosphorus content drop to 0.05mg/L by 0.5mg/L, filtration velocity is 1-2m/h.Device moves 900d continuously and sorbent material is not regenerated, and still can reach the water outlet requirement of design.They also plan the processing and amplifying device, are a volume 116000m
3The phosphorus content of lake water, be reduced in the 0.03mg/L from 0.16mg/L.
(3) synthetic sorbent material.Because traditional adsorbents adsorb capacity is little, have in addition have a toxic action, so, limited their application in the sewage phosphorus hydrochlorate reclaims. be to obtain higher loading capacity, the researchist has developed various synthetic sorbent materials.The synthetic range of choice that has enlarged sorbing material of dephosphorization adsorbent, the sorbing material of now studying comprises the oxide compound and its esters of multiple metals such as Al, Mg, Fe, Ca, Ti, Zr and La.
J.Das etc. have reported that the double-metal hydroxide LDHs (Layered Double Hydroxides) of Mg-Al mol ratio 2:1 has higher phosphorus loading capacity; For the 50mg/L aqueous phosphate solution, dosage is 0.4g/L, reaction times 4h, and under the pH=6.0 condition, clearance can reach more than 94%.This sorbent material has the ability of better antagonism interfering ion, adsorption process accords with Langmuir adsorption isotherm.
Cheng etc. have developed Zn-Al-LDHs; The adsorptive power of every gram LDHs can reach 40. 77mg/g. strongly-acids and strong basicity has considerable influence to its adsorptive power; Be adsorbed as thermo-negative reaction to phosphatic; Adsorption isothermal line meets Langmuir's adsorption isotherm, and can be used massfraction by the phosphoric acid salt after the LDHs absorption is 5% sodium hydroxide solution desorb.
Dublin, Ireland university utilizes artificial swamp to handle plant's waste water, adopts alum sludge, and the dewatered sludge that promptly coagulate sludge dehydration back forms in the water supply plant reclaims the phosphorus in the sewage as sorbent material.Its adsorption mechanism is the OH that relies on wherein
-, Cl
-, SO
4 2-With humic acid isoreactivity group and phosphate anion generation chemical precipitation reaction; Remove the phosphorus in the sewage; After acid or alkaline purification and reclaim phosphorus wherein. this alum sludge can be removed more than 90% of total phosphorus in the sewage, adsorbs the rich phosphorus alum sludge phosphorus content in saturated back and reaches 14.3 mg/g.This method not only can solve the alum sludge handling problems, and can reclaim the phosphorus in the sewage.
Bastin etc. have reported that a kind of gypsum shape iron-calcium oxide (iron oxide-gypsum) of synthetic is used for the removal research of phosphorus.The result points out that this dephosphorizing agent can be removed phosphorus in the waste water that concentration is 0.001-10mgP/L.When the pH value was higher, loading capacity was bigger.This dephosphorizing agent has the calcium ion stripping when phosphorus concentration is low.
Rarmesh Chitrakar etc. has reported the dephosphorization research of adopting a kind of unbodied zirconium nitrate that seawater and waste water are carried out.PH influence test is illustrated in pH and is higher than at 6 o'clock, and for seawater, the ability of this adsorbents adsorb phosphorus increases with the increase of pH value.When the sorbent material dosage is 0.05g/L, be respectively 10 and 17mg/g for the phosphorus loading capacity of the seawater of rich phosphorus and simulated wastewater.
Ion exchange method as a kind of classics efficiently the ion remaval technology have a large amount of industrial applications instances with research the degree of depth.But also fewer for the research that utilizes ion exchange method treatment of high concentration phosphorus-containing wastewater both at home and abroad at present, gush low-concentration phosphorus-containing sewage such as sewage and utilize ion exchange method directly to handle the river, also do not see relevant report.Ion exchange technique is applied to the processing that sewage is gushed in the eutrophication river; Thoroughly separate from river except making phosphorus; Effectively the control water eutrophication is outside the pale of civilization, can with the phosphorus enrichment in regenerated liquid, make it obtain to reclaim through resin regeneration; Realize the sustainable recycle of phosphor resource, meet the requirement of friendly type of current China built environment and conservation-minded society.
Summary of the invention
The purpose of this invention is to provide a kind of method that from eutrophic water, reclaims phosphorus.
The technical scheme that the present invention taked is:
A kind of method that from eutrophic water, reclaims phosphorus may further comprise the steps:
1) with the resin pre-treatment so that resin is in known OH-type ionic forms;
2) the pretreated resin container of packing into is formed resin bed, feed eutrophic water, carry out IX through anionic group in the resin and the phosphorus-containing groups in the water, the phosphorus in the water is trapped within on the resin;
3) resin to above-mentioned absorption phosphorus carries out desorption, obtains the phosphorus pregnant solution;
4) resin behind the desorption is regenerated.
In the step 1), pretreatment process is: to there not being muddy look, the sodium hydroxide solution with resin quality 3-4 5-10wt% doubly soaks resin 9-10h again, pours out alkali lye with water washing resin, and water washing resin is to neutral subsequent use.
Step 2) in, the height of resin bed is the 1/3-1/2 of container height.
In the step 3), the method for desorption is: the NaCl solution with 8wt% carries out wash-out.
In the step 4), described renovation process is: it is 9-10h in resin 3-4 5% the NaClO solution doubly that resin is immersed in quality, pours out NaClO solution; Water washing is to neutral; Use quality as resin 3-4 5% NaOH solution soaking 9-10h doubly again, pour out alkali lye, water washing is to neutral subsequent use.
The invention has the beneficial effects as follows: be used as the phosphorus source to eutrophication water quality,, give the resin anion exchange groups through pre-treatment to resin; And be used for this resin the processing of eutrophication water quality; From water, adsorb phosphorus, make eutrophication water quality obtain to purify, promote the improvement of ecotope.Method of the present invention makes phosphorus from water, thoroughly separate and obtain to reclaim, and the rich phosphorus stripping liquid of high density can be used as the phosphate fertilizer raw material, thereby realizes the recycle and the Sustainable Production of phosphorus, and last resin is renewable, thereby reaches the effect of recycle.
Description of drawings
Fig. 1 is dynamic confluent and accumulation phosphorus adsorptive capacity graph of relation.
Embodiment
A kind of method that from eutrophic water, reclaims phosphorus is characterized in that: may further comprise the steps:
1) with the pre-treatment of DS401 macroporous adsorbent resin so that resin is in known OH-type ionic forms; Described pretreatment process is: with water washing resin to there not being muddy look; Sodium hydroxide solution with resin quality 3-4 5-10wt% doubly soaks resin 9-10h again; Pour out alkali lye, water washing resin is to neutral, and is subsequent use.
2) the pretreated resin diameter of packing into is 4.5-80cm, highly forms resin bed for the ion exchange column of 0.5-2m; Feeding total phosphorus concentration with feedwater flow velocity 100-120mL/min is the eutrophic water of 1-3 mg/l; Carry out IX through anionic group in the resin and the phosphorus-containing groups in the water, the phosphorus in the water is trapped within on the resin; Wherein, the height of resin bed is the 1/3-1/2 of container height.
3) resin to above-mentioned absorption phosphorus carries out desorption, obtains the phosphorus pregnant solution; The method of described desorption is: the molar weight of carrying out the total phosphorus in wash-out (elution speed is 3ml/min) to the elutriant with the NaCl solution of 8wt% is stable;
4) resin behind the desorption is regenerated; Described renovation process is: it is 9-10h in resin 3-4 5% the NaClO solution doubly that resin is immersed in quality; Pour out NaClO solution, water washing is to neutral, uses quality to be resin 3-4 5% NaOH solution soaking 9-10h doubly again; Pour out alkali lye, water washing is to neutral subsequent use.
Below in conjunction with specific embodiment the present invention is done further explanation:
Embodiment 1:
Resin is before using; Through pre-treatment, pretreatment process is: to there not being muddy look, the sodium hydroxide solution with resin quality 3-4 5-10wt% doubly soaks resin 9-10h again with water washing DS401 macroporous adsorbent resin; Pour out alkali lye, water washing resin is to neutral subsequent use.
With the resin internal diameter of packing into is 4.5cm, and height is in the ion exchange column of 50cm, and the resin floor height is 19.0cm; The resin volume is 302ml, and the feeding total phosphorus concentration is 2.6mg/l, and phosphate concentration is the eutrophication river water burst of 1.5mg/l; The feedwater flow velocity is 100mL/min, and every separated 5min takes effusive water sample, the content of phosphorus in total phosphorus and the solubility orthophosphoric acid salt in the mensuration outflow water sample; When eutrophic water when feeding ion exchange column, the resin in the post can be divided into saturated section, fractional saturation section and adsorption stage not from top to bottom successively, when the each several part resin has all adsorbed saturated; Promptly no longer have adsorptive power, at this moment resin needs desorb and regeneration.
Record the DS resin s-adsorption of solubility orthophosphoric acid salt and total phosphorus is respectively 1.3 and 1.8 mg P g
-1Confluent is seen Fig. 1 with accumulation phosphorus adsorptive capacity relation curve.
Embodiment 2:
Resin is before using; Through pre-treatment, pretreatment process is: to there not being muddy look, the sodium hydroxide solution with resin quality 3-4 5-10wt% doubly soaks resin 9-10h again with water washing DS401 macroporous adsorbent resin; Pour out alkali lye, water washing resin is to neutral subsequent use.
Press the method system post of embodiment 1; With total phosphorus concentration is 1.86mg/l; Phosphate concentration is the eutrophication river water burst of 1.03mg/l, feeds in the resin-column, and the feedwater flow velocity is 100mL/min; The content of phosphorus in every total phosphorus and solubility orthophosphoric acid salt at a distance from 5min sampling and measuring effluent obtains resin according to experimental result the dynamic s-adsorption of solubility orthophosphoric acid salt and total phosphorus is respectively 1.3 and 1.85 mg P g
-1
Resin reaches capacity after the absorption; With stripping liquid (the NaCl solution of 8wt%) resin is carried out wash-out (elution speed is 3ml/min); Get off the phosphorus-containing groups desorb that is adsorbed on the resin; When efflux volume was 700ml, desorption efficiency reached 93.4%, and phosphorus content is 699 mg/L in the solution that desorb is got off.
After the desorb resin is regenerated; The regenerated method is: it is 9-10h in resin 3-4 5% the NaClO solution doubly that resin is immersed in quality; Pour out NaClO solution, water washing is to neutral, uses quality to be resin 3-4 5% NaOH solution soaking 9-10h doubly again; Pour out alkali lye, water washing is to neutral subsequent use.
Regenerating resin is used to handle phosphorous eutrophic water (be eutrophic water same above the present embodiment, promptly total phosphorus concentration is 1.86mg/l, and phosphate concentration is the eutrophication river water burst of 1.03mg/l) again; Through 6 absorption-desorb-reprocessing cycle (absorption; Resolve, renovation process is taked method same above the present embodiment), resin all has close treatment effect to the eutrophication actual sewage; Through test, the resin after 6 times of regenerating still reaches 92.5% to the adsorption rate of phosphorus in the waste water.
Claims (5)
1. method that from eutrophic water, reclaims phosphorus is characterized in that: may further comprise the steps:
1) with the resin pre-treatment so that resin is in known OH-type ionic forms;
2) the pretreated resin container of packing into is formed resin bed, feed eutrophic water, carry out IX through anionic group in the resin and the phosphorus-containing groups in the water, the phosphorus in the water is trapped within on the resin;
3) resin to above-mentioned absorption phosphorus carries out desorption, obtains the phosphorus pregnant solution;
4) resin behind the desorption is regenerated.
2. a kind of method that from eutrophic water, reclaims phosphorus according to claim 1; It is characterized in that: in the step 1); Pretreatment process is: with water washing resin to there not being muddy look; Sodium hydroxide solution with resin quality 3-4 5-10wt% doubly soaks resin 9-10h again, pours out alkali lye, and water washing resin is to neutral subsequent use.
3. a kind of method that from eutrophic water, reclaims phosphorus according to claim 1 is characterized in that: step 2) in, the height of resin bed is the 1/3-1/2 of container height.
4. a kind of method that from eutrophic water, reclaims phosphorus according to claim 1, it is characterized in that: in the step 3), the method for desorption is: the NaCl solution with 8wt% carries out wash-out.
5. a kind of method that from eutrophic water, reclaims phosphorus according to claim 1; It is characterized in that: in the step 4), described renovation process is: it is 9-10h in resin 3-4 5% the NaClO solution doubly that resin is immersed in quality, pours out NaClO solution; Water washing is to neutral; Use quality as resin 3-4 5% NaOH solution soaking 9-10h doubly again, pour out alkali lye, water washing is to neutral subsequent use.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103217388A (en) * | 2013-04-01 | 2013-07-24 | 浙江大学 | Method for carrying out water quality monitoring by utilizing waste ion exchange resin ball |
| CN104628086A (en) * | 2015-01-06 | 2015-05-20 | 大连东泰资源再生有限公司 | Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium |
| CN105289555A (en) * | 2015-12-11 | 2016-02-03 | 华颐药业有限公司 | Regeneration method of macroporous adsorption resin |
| CN111732148A (en) * | 2020-06-29 | 2020-10-02 | 河海大学 | System for retrieve phosphate in follow surface eutrophic water |
| CN113004054A (en) * | 2021-04-13 | 2021-06-22 | 广西博世科环保科技股份有限公司 | Enhanced efficient phosphorus removal constructed wetland substrate and preparation method thereof |
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| JP2002361247A (en) * | 2001-06-11 | 2002-12-17 | Kurita Water Ind Ltd | Method for manufacturing pure water |
| CN101254966A (en) * | 2008-04-14 | 2008-09-03 | 北京特斯顿新材料技术发展有限公司 | Recovery method of phosphate discharge liquid |
| CN101343093A (en) * | 2008-09-03 | 2009-01-14 | 南京大学 | Method for deeply purifying minim phosphor in water with composite resin |
| CN101618904A (en) * | 2009-07-29 | 2010-01-06 | 河南理工大学 | Method of catalyzing hydrogen peroxide with molybdate-carried ion exchange resin to degrade trichlorophenol |
-
2012
- 2012-07-06 CN CN201210231484.1A patent/CN102774929B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002361247A (en) * | 2001-06-11 | 2002-12-17 | Kurita Water Ind Ltd | Method for manufacturing pure water |
| CN101254966A (en) * | 2008-04-14 | 2008-09-03 | 北京特斯顿新材料技术发展有限公司 | Recovery method of phosphate discharge liquid |
| CN101343093A (en) * | 2008-09-03 | 2009-01-14 | 南京大学 | Method for deeply purifying minim phosphor in water with composite resin |
| CN101618904A (en) * | 2009-07-29 | 2010-01-06 | 河南理工大学 | Method of catalyzing hydrogen peroxide with molybdate-carried ion exchange resin to degrade trichlorophenol |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103217388A (en) * | 2013-04-01 | 2013-07-24 | 浙江大学 | Method for carrying out water quality monitoring by utilizing waste ion exchange resin ball |
| CN103217388B (en) * | 2013-04-01 | 2015-04-29 | 浙江大学 | Method for carrying out water quality monitoring by utilizing waste ion exchange resin ball |
| CN104628086A (en) * | 2015-01-06 | 2015-05-20 | 大连东泰资源再生有限公司 | Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium |
| CN105289555A (en) * | 2015-12-11 | 2016-02-03 | 华颐药业有限公司 | Regeneration method of macroporous adsorption resin |
| CN111732148A (en) * | 2020-06-29 | 2020-10-02 | 河海大学 | System for retrieve phosphate in follow surface eutrophic water |
| CN113004054A (en) * | 2021-04-13 | 2021-06-22 | 广西博世科环保科技股份有限公司 | Enhanced efficient phosphorus removal constructed wetland substrate and preparation method thereof |
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