CN102464308A - Method for preparing and purifying struvite from residual sludge - Google Patents
Method for preparing and purifying struvite from residual sludge Download PDFInfo
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- CN102464308A CN102464308A CN2010105324704A CN201010532470A CN102464308A CN 102464308 A CN102464308 A CN 102464308A CN 2010105324704 A CN2010105324704 A CN 2010105324704A CN 201010532470 A CN201010532470 A CN 201010532470A CN 102464308 A CN102464308 A CN 102464308A
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Abstract
The invention relates to a method for preparing and purifying struvite from residual sludge in an urban sewage treatment factory and is characterized in that the method contains the following steps of: controlling pH within the range of 3-5 for releasing nitrogen and phosphor from the residual sludge; modifying a sodium storng-acid cation exchange resin by using an MgCl2 solution; carrying out ion exchange on a supernatant of the sludge containing rich nitrogen and phosphor by using the modified resin so as to reduce the impact of calcium ion on the formation of the struvite substance; controlling pH within the range of 8.5-9.5, stirring a solution obtained after ion exchange until a lot of off-white precipitates, standing for settling, and recovering the off-white precipitates. By adoption of the acid-base adjustment and ion exchange methods for the preparation and purification of the struvite substance from the residual sludge, the high-purity struvite substance can be obtained, and the impact load of supernatant reflux generated during the sludge treatment process on nitrogen and phosphor during the sewage treatment flow can be mitigated, so as to improve operation of the sewage treatment factory.
Description
Technical field
The present invention relates to a kind of from the excess sludge of municipal sewage plant the preparation and the method for purification struvite, belong to the resource and environment technical field.
Background technology
Along with improving constantly of municipal sewage treatment ability, the mud that sewage work produces the particularly amount of excess sludge is increasing, endangers also serious day by day.Simultaneously, mud also is a kind of available resource, contains nutritive element such as the needed nitrogen of plant-growth, phosphorus, potassium and keeps various trace elements that plant normal growth grows and the organism and the soil ulmin of the structure of improving the soil.Therefore, the minimizing, stabilization, resource utilization and innoxious that how to realize mud become the key subjects that sewage treatment industry needs to be resolved hurrily.In the research of excess sludge resource utilization, consider the sustainable use problem of phosphorus and the recycling problem to phosphorus in the excess sludge of carrying out has become one of focus that industry pays close attention to.At present, struvite and calcium phosphate are considered to the most promising phosphorus and reclaim approach, particularly the struvite precipitator method and enjoy favor owing to reclaiming two kinds of elements of nitrogen phosphorus simultaneously.
The principle that the struvite precipitator method reclaim nitrogen phosphorus is in sewage, to have NH simultaneously
4 +, PO
4 3-And Mg
2+The time, reaction as follows takes place:
Mg
2++PO
4 3-+NH
4 ++6H
2O—→MgNH
4PO
4·6H
2O
Resultant MgNH
4PO
46H
2O, promptly magnesium ammonium phosphate abbreviates MAP as, is commonly called as struvite, and its pure crystal is a white crystal, is a kind of environment-friendly type slow release fertilizer that can realize that the nitrogen phosphor resource effectively utilizes, receives much concern in recent years.
Thereby the struvite precipitator method not only can be removed and reclaim nitrogen, phosphorus simultaneously and reduce and reclaim nitrogen and phosphorus load in the liquid, realize the minimizing of mud and innoxious, and to reclaim the struvite that obtains be a kind of good slow release fertilizer, can in agriculture prodn, utilize once more.Therefore, concerning the such large agricultural country of China, the research and utilization struvite precipitator method reclaim nitrogen and the phosphorus in the sludge treatment structures, have major and immediate significance more undoubtedly.
Research to nitrogen phosphorus method in the struvite precipitator method recovery mud at present focuses mostly in the discussion to formation condition, and the method that from excess sludge, obtains higher degree struvite material is then rarely had report.
Summary of the invention
The initial characteristic and the existing method gained struvite purity that the present invention is directed to excess sludge are difficult to gratifying deficiency; A kind of method that from excess sludge, prepares high purity struvite material is provided; This method not only can obtain highly purified struvite material; And can alleviate in the sludge handling process the supernatant that produces reflux to the nitrogen phosphorus impact load of WWT flow process, thereby improve the operation of sewage work.
Technical scheme provided by the invention is a kind of method that from excess sludge, prepares high purity struvite material, it is characterized in that method carries out as follows:
1) excess sludge is placed in the sbr reactor device; The control stirring velocity is (excess sludge can stir but be unlikely to produce whirlpool at this moment) in proper range; Use certain density HCl and NaOH solution to regulate pH in 3～5 scopes; Under room temperature environment, react, so that the nitrogen phosphorus in the excess sludge is released in the supernatant.After 2～4h is carried out in reaction, obtain being rich in the mud supernatant of ammonia nitrogen, orthophosphoric acid salt and calcium ions and magnesium ions.
2) use certain density MgCl
2Solution is modified as magnesium type strongly acidic cationic exchange resin with sodium type strongly acidic cationic exchange resin.
3) with gained mud supernatant in the step 1) with certain flow rate through the ion exchange column of the magnesium type strongly acidic cationic exchange resin behind the remodeling is housed; Carry out the removal of calcium ion; With the ratio (brief note is Mg/Ca) that changes the calcium magnesium amount of substance in the mud supernatant, with Mg/Ca less than 5 as the resin leakage point.
4) mud supernatant after the IX of gained in the step 3) is placed struvite preparation feedback device; With the pH of certain density HCl and NaOH solution regulator solution 8.5～9.5; Under the speed of 100～200r/min, be stirred to a large amount of pale precipitation things of appearance, staticly settle the back and reclaim the pale precipitation thing that is rich in struvite.
The invention has the beneficial effects as follows:
1) realized within a short period of time the nitrogen phosphorus in the excess sludge transferred to the liquid phase from solid phase and gone, thus the quick acquisition that has realized being rich in the nitrogen phosphorus solution.
2) through the IX of magnesium type strongly acidic cationic exchange resin, improved the Mg/Ca that is rich in the nitrogen phosphorus solution, thereby eliminated calcium ion to greatest extent forming the influence of struvite material.
3) obtained struvite purity at the deposition product more than 95%.
Description of drawings
Accompanying drawing of the present invention is the process flow sheet of embodiment.
Label among the figure: 1. electric mixer, 2. peristaltic pump, 3. the magnesium type strongly acidic cationic exchange resin behind the remodeling, 4. magnetic stirring apparatus.
Embodiment
Get certain sewage work and (adopt A
2/ O technology) excess sludge of returned sluge pump house; Place in the excess sludge nitrogen phosphorus tripping gear; The control stirring velocity is (excess sludge can stir but be unlikely to produce whirlpool at this moment) in the scope of 70～90r/min; Using HCl and the NaOH solution adjusting pH of 2mol/L is in 3 ± 0.2 scopes; Under room temperature environment, react, after 4h is carried out in reaction, obtain containing the mud supernatant that ammonia nitrogen, orthophosphoric acid salt and calcium, magnesium ion concentration are respectively 239.2mg/L, 128mg/L, 399.7mg/L and 196.2mg/L.When nitrogen phosphorus discharged in excess sludge, use concentration was 3% MgCl
2Solution changes purchase 001 * 7 strongly acidic cationic exchange resin into the magnesium type by the sodium type.Then; Get the magnesium type strongly acidic cationic exchange resin after 40ml remodeling is accomplished; Pack in the exchange column, desire is handled the mud supernatant with the flow velocity of the 2cm/min exchange column of flowing through, the Mg/Ca in the mud supernatant before and after the IX is brought up to 9.8 by 0.4 with peristaltic pump.Next; Gained solution after the IX is placed the struvite preparation facilities; The pH that adds certain density HCl and NaOH solution regulator solution is 9.5; Under the speed of 100r/min, stir 10 backs and a large amount of pale precipitation things occur, staticly settle the back and reclaim that to obtain struvite purity be 96.85% pale precipitation thing.
Claims (5)
1. method that from excess sludge, prepares high purity struvite material is characterized in that method carries out as follows:
1) control pH carries out the release of nitrogen phosphorus in the excess sludge in 3～5 scope;
2) use MgCl
2Solution carries out the remodeling of sodium type strongly acidic cationic exchange resin;
3) resin behind the usefulness remodeling carries out IX to the nitrogen phosphorus sludge supernatant that is rich in of gained, reduces the influence that calcium ion forms the struvite material;
4) control pH is stirred to a large amount of pale precipitations of appearance to gained solution after the IX in 8.5～9.5 scopes, staticly settles the back and reclaims the pale precipitation thing that is rich in struvite.
2. require the described method that from excess sludge, prepares high purity struvite material according to right 1, it is characterized in that: in the excess sludge in the nitrogen phosphorus dispose procedure pH be controlled in 3～5 scopes.
3. require the described method that from excess sludge, prepares high purity struvite material according to right 1; It is characterized in that: the magnesium type strongly acidic cationic exchange resin behind the employing remodeling carries out IX to the mud supernatant body refuse that is rich in ammonia nitrogen, orthophosphoric acid salt and calcium ions and magnesium ions of gained; Change the ratio (brief note is Mg/Ca) of the calcium magnesium amount of substance in the mud supernatant, and with Mg/Ca less than 5 as the resin leakage point.
4. require the described method that from excess sludge, prepares high purity struvite material according to right 1, it is characterized in that: the mud supernatant after the use IX carries out struvite and prepares in the process, and pH is controlled in 8.5～9.5 scopes.
5. require the described method that from excess sludge, prepares high purity struvite material according to right 1, it is characterized in that: gained deposition product gets struvite purity more than 95%.
Priority Applications (1)
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|---|---|---|---|
| CN2010105324704A CN102464308A (en) | 2010-11-05 | 2010-11-05 | Method for preparing and purifying struvite from residual sludge |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105324704A CN102464308A (en) | 2010-11-05 | 2010-11-05 | Method for preparing and purifying struvite from residual sludge |
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| CN102464308A true CN102464308A (en) | 2012-05-23 |
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ID=46068479
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| CN2010105324704A Pending CN102464308A (en) | 2010-11-05 | 2010-11-05 | Method for preparing and purifying struvite from residual sludge |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641283A (en) * | 2013-11-26 | 2014-03-19 | 华南理工大学 | Method of economically recycling phosphor from excess sludge |
| CN103663403A (en) * | 2013-11-28 | 2014-03-26 | 中国农业大学 | Circulating fluidized crystallization control reaction device for wastewater phosphorus synergy crystallization and dynamic monitoring and regulating method thereof |
| CN104692837A (en) * | 2015-02-13 | 2015-06-10 | 重庆工商大学 | Method of comprehensively utilizing sludge |
| CN105524952A (en) * | 2016-02-04 | 2016-04-27 | 同济大学 | Method for producing acid by fermenting excess sludge and synthesizing microbial oil |
| CN106753320A (en) * | 2016-12-30 | 2017-05-31 | 中国地质大学（武汉） | Modified super-low-density proppant of a kind of ionomer and preparation method thereof |
| CN107675003A (en) * | 2017-10-10 | 2018-02-09 | 江西理工大学 | A kind of method of the Enrichment purification rare earth from southern ion type rareearth ore leachate |
| CN110950314A (en) * | 2019-11-25 | 2020-04-03 | 中南民族大学 | Artificial struvite, preparation method thereof and citrate soluble fertilizer |
| CN112079543A (en) * | 2020-09-07 | 2020-12-15 | 天津壹新环保工程有限公司 | Novel anaerobic sludge modified ammonia nitrogen removal treatment system and method |
| CN112125483A (en) * | 2020-08-31 | 2020-12-25 | 同济大学 | Synchronous recovery processing method for nitrogen and phosphorus in high-solid anaerobic digestion sludge |
| CN112225192A (en) * | 2020-10-19 | 2021-01-15 | 南京融众环境工程研究院有限公司 | Method for preparing struvite by reinforcing residual sludge to release nitrogen and phosphorus and inducing biochar |
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| CN101654238A (en) * | 2009-09-11 | 2010-02-24 | 华东理工大学 | Method for recovering phosphonium compound from phosphorous excess sludge of urban sewage treatment plant |
| CN101695999A (en) * | 2009-10-23 | 2010-04-21 | 宁波工程学院 | Method for recovering nutritive materials of phosphorus and nitrogen from sewage and sludge |
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2010
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| CN101654238A (en) * | 2009-09-11 | 2010-02-24 | 华东理工大学 | Method for recovering phosphonium compound from phosphorous excess sludge of urban sewage treatment plant |
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Non-Patent Citations (1)
| Title |
|---|
| 陈轶等: "酸碱环境对剩余污泥水解酸化过程中NH4+-N、PO43--P释放的影响", 《2008年全国给水排水技术交流会暨全国水网理事会换届大会论文集》 * |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641283A (en) * | 2013-11-26 | 2014-03-19 | 华南理工大学 | Method of economically recycling phosphor from excess sludge |
| CN103641283B (en) * | 2013-11-26 | 2016-01-06 | 华南理工大学 | A kind of method reclaiming phosphorus from excess sludge of economy |
| CN103663403A (en) * | 2013-11-28 | 2014-03-26 | 中国农业大学 | Circulating fluidized crystallization control reaction device for wastewater phosphorus synergy crystallization and dynamic monitoring and regulating method thereof |
| CN103663403B (en) * | 2013-11-28 | 2015-04-08 | 中国农业大学 | Circulating fluidized crystallization control reaction device for wastewater phosphorus synergy crystallization and dynamic monitoring and regulating method thereof |
| CN104692837A (en) * | 2015-02-13 | 2015-06-10 | 重庆工商大学 | Method of comprehensively utilizing sludge |
| CN105524952B (en) * | 2016-02-04 | 2019-10-01 | 同济大学 | A method of utilizing excess sludge fermentation and acid and synthesized micro-organism grease |
| CN105524952A (en) * | 2016-02-04 | 2016-04-27 | 同济大学 | Method for producing acid by fermenting excess sludge and synthesizing microbial oil |
| CN106753320A (en) * | 2016-12-30 | 2017-05-31 | 中国地质大学（武汉） | Modified super-low-density proppant of a kind of ionomer and preparation method thereof |
| CN106753320B (en) * | 2016-12-30 | 2020-05-15 | 中国地质大学（武汉） | Ionic crosslinking modified ultralow-density proppant and preparation method thereof |
| CN107675003A (en) * | 2017-10-10 | 2018-02-09 | 江西理工大学 | A kind of method of the Enrichment purification rare earth from southern ion type rareearth ore leachate |
| CN107675003B (en) * | 2017-10-10 | 2019-10-08 | 江西理工大学 | A method of the Enrichment purification rare earth from southern ion type rareearth ore leachate |
| CN110950314A (en) * | 2019-11-25 | 2020-04-03 | 中南民族大学 | Artificial struvite, preparation method thereof and citrate soluble fertilizer |
| CN112125483A (en) * | 2020-08-31 | 2020-12-25 | 同济大学 | Synchronous recovery processing method for nitrogen and phosphorus in high-solid anaerobic digestion sludge |
| CN112079543A (en) * | 2020-09-07 | 2020-12-15 | 天津壹新环保工程有限公司 | Novel anaerobic sludge modified ammonia nitrogen removal treatment system and method |
| CN112079543B (en) * | 2020-09-07 | 2023-10-20 | 天津壹新环保工程有限公司 | Novel anaerobic sludge modified ammonia nitrogen removal treatment system and method |
| CN112225192A (en) * | 2020-10-19 | 2021-01-15 | 南京融众环境工程研究院有限公司 | Method for preparing struvite by reinforcing residual sludge to release nitrogen and phosphorus and inducing biochar |
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Application publication date: 20120523 |