CN1748857A - Process for preparing phosphate radical adsorber - Google Patents
Process for preparing phosphate radical adsorber Download PDFInfo
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- CN1748857A CN1748857A CN 200510014769 CN200510014769A CN1748857A CN 1748857 A CN1748857 A CN 1748857A CN 200510014769 CN200510014769 CN 200510014769 CN 200510014769 A CN200510014769 A CN 200510014769A CN 1748857 A CN1748857 A CN 1748857A
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- described preparation
- phosphate radical
- adsorber
- oxychloride
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Abstract
The preparation process of phosphate radical adsorber features that powdered inorganic mineral soil containing silica, magnesia, alumina and ferric oxide is made to mix with water solution of oxychloride capable of hydrolyzing to obtain white or brown precipitate, and the precipitate is further high temperature treated to obtain the porous granular adsorber. The porous granular adsorber has great amount of hydroxyl radicals in the surface and can produce exchange reaction with phosphate radical in water to eliminate phosphate radical, so that it may be used in the purification of phosphate containing water and the treatment of phosphate containing sewage. The adsorber has low cost, easy-to-obtain material, great adsorption capacity, high selectivity, simple operation acid and alkali resistance, radiation resistance and simple regeneration, and the concentrated phosphate radical may be used in producing fertilizer or for agricultural production directly.
Description
[technical field]
The present invention relates to the water body purification field, particularly a kind of preparation method who passes through the phosphate radical adsorber of absorption method dephosphorization.
[background technology]
The eutrophication of water body has become the problem of worldwide attention, and phosphorus is the one of the chief elements that causes the eutrophication of water body, phosphorus in water generally with PO
4 3-, HPO
4 2-, H
2PO
4 -Form exist, be the essential thing of algae in the water body, floating material growth, the excessive a large amount of breedings and death of aquatic organism that makes in the water of phosphorus causes water quality deterioration, even causes " red tide ", and the water system ecological balance is destroyed.In the prior art, people adopt the phosphorus in chemical method or the biochemical process removal water usually.It is higher that the former removes the efficient of phosphorus, but the mud that produces is many, the post processing trouble.Latter's operating condition is relatively harsher, complicated, and dephosphorization rate is lower.Given this, many researchers focus on notice with the method for absorption phosphorus-containing wastewater are handled.Yet with adsorbent the phosphate radical in the water body is adsorbed, especially need to solve selectivity, adsorption capacity and the regeneration problem of adsorbent.
[summary of the invention]
Purpose of the present invention is intended to solve prior art problems, and a kind of cost is low, adsorption capacity is big, selectivity is high and provide, and is easy to the preparation method of the phosphate radical adsorber of regeneration.
Technical scheme of the present invention is the preparation method of a kind of phosphate radical adsorber of design.It is characterized in that it is mixed with the oxychloride aqueous solution that can be hydrolyzed by the inorganic ore deposit soil of the powdery that contains silica, magnesia, aluminium oxide and iron oxide, obtain the sediment of white or brown, carry out the granular adsorption agent that high-temperature process obtains porous again.
The adsorbent of the inventive method preparation is the particulate material of porous, has a large amount of hydroxyls on its surface, can exchange take place to remove the phosphate radical in the water with the phosphate radical in the water body, can be used for containing the purification of phosphorus water and the processing of phosphorus-containing wastewater.This adsorbent is cheap, raw material is easy to get, adsorption capacity is big, selectivity is high, practical operation is simple, acid and alkali-resistance, radiation hardness, and regeneration is easily simple, can use repeatedly.The phosphate radical that concentrates back (regenerated liquid) can also be made fertilizer or be directly used in agricultural production.
[specific embodiment]
Phosphate radical preparation of adsorbent method of the present invention, inorganic ore deposit soil by the mixture that contains silica, magnesia, aluminium oxide and iron oxide mixes with the oxychloride that can be hydrolyzed, regulate the pH value of mixture with alkaline matter, obtain the sediment of white, carry out the granular adsorption agent that high-temperature process obtains porous again.Wherein: the inorganic ore deposit soil that contains the mixture of silica, magnesia, aluminium oxide, iron oxide is: the mixture of one or both in attapulgite, natural zeolite, wollastonite and the diatomite etc.; The oxychloride that can be hydrolyzed is: the mixture of one or both in ferric trichloride, magnesium chloride, zirconium oxychloride and the alchlor etc., the concentration of this oxychloride aqueous solution is 40～55%.When inorganic ore deposit soil mixed with the oxychloride aqueous solution that can be hydrolyzed, the pH value of regulating mixture with alkaline matter was 9～12, and this alkaline matter is a sodium hydrate aqueous solution, and its concentration is 0.5～1.5mol/L.Carry out calcination in the last muffle furnace that changes automatic temperature-control behind the sediment that obtains white or brown over to, its calcination temperature is 200 ℃～300 ℃, and the time is 1.5～3.0 hours; Or under 120-150 ℃, 1.2-1.4atm, carry out hydrothermal treatment consists 30～90min, the back 80 ℃ dry down, steam moisture wherein, put into 8～20kw micro-wave oven again and dry by the fire and burn 8～15min, can obtain the adsorbent of different-grain diameter.
Example 1. is selected the attapulgite that produced from Jiangsu for use, and (main component is SiO
255%, AL
2O
310%, etc.) 20g, putting into 25ml concentration is 45% zirconyl chloride solution, is 1molL with content
-1NaOH solution regulate its pH to 10.5, obtain sediment, leach sediment, steam moisture wherein, change in the muffle furnace in 280 ℃ of following calcinations 2 hours, can obtain granular adsorbent.
It is 150mgL that the adsorbent of above-mentioned 0.2g is put into 30ml concentration
-1Phosphorous Simulated Water, the pH value in the water equals 5.6.Absorption is 8 hours under room temperature, and maximum adsorption capacity is 34.5mgg
-1
Example 2. is selected powdery wollastonite 25g for use, joins 20ml concentration and is in 50% the magnesium chloride and the alchlor aqueous solution, uses 1.2molL
-1NaOH solution regulate about its pH to 11.Obtain the sediment of white, leach sediment and change in the muffle furnace that moves temperature adjustment, be 200 ℃～300 ℃ calcinations 2.0～3.0 hours.Can obtain the adsorbent of different-grain diameter.
It is 10～15mol/L that the adsorbent of above-mentioned 0.1g is put into 50ml concentration
-1City domestic sewage in adsorb, after 8 hours in the water content of phosphorus drop to 1～2mgL
-1
Example 3. is selected the attapulgite that produced from Jiangsu for use, and (main component is SiO
255%, AL
2O
310%, etc.) 20g, putting into 25ml concentration is 45% zirconyl chloride solution, is 1molL with content
-1NaOH solution regulate its pH to 10.5, obtain sediment, after the pressure cooker of again sediment being put into family expenses carries out hydrothermal treatment consists 60min, 80 ℃ dry down, after change in the micro-wave oven under power 10kw baking over to and burn 10min.Can obtain the adsorbent of different-grain diameter.
It is 150mgL that the adsorbent of above-mentioned 0.2g is put into 50ml concentration
-1Phosphorous Simulated Water, the pH value in the water equals 5.6.Absorption is 8 hours under room temperature, and maximum adsorption capacity is 33.5mgg
-1
Example 4. is selected powdery wollastonite 25g for use, joins 20ml concentration and is in 50% the zirconia aqueous solution, uses 1.2molL
-1NaOH solution regulate about its pH to 11.Obtain the sediment of white, the pressure cooker that puts it into family expenses carries out hydrothermal treatment consists 50min, and is dry down at 80 ℃.Steam moisture wherein, after change in the micro-wave oven under power 8kw baking over to and burn 10min.Can obtain the adsorbent of different-grain diameter.
It is 10～15mgL that the adsorbent of above-mentioned 0.1g is put into 50ml concentration
-1City domestic sewage in adsorb, after 3 hours in the water content of phosphorus drop to 1～2mgL
-1.
It is in 45%Mgcl, Alcl3 (Mg: Al is 1: the 0.5) mixed solution that example 5. joins 25ml concentration with the attapulgite of 25g, with content is that the NaOH solution of 1molL-1 is regulated its pH to 9.5, obtain sediment, after the pressure cooker of again sediment being put into family expenses carries out hydrothermal treatment consists 40min.80 ℃ down dry, after change in the micro-wave oven under power 10kw baking over to and burn 10min, can obtain the adsorbent that adsorption capacity is 14.5mg/g.
Example 6. evenly mixes the wollastonite of 20g with the natural zeolite of 10g, joins 60% the Fecl3 aqueous solution, with the pH value to 10.6 of the NaOH regulator solution of 0.5mol.Obtain the sediment of brown, leach sediment and change in the muffle furnace that moves temperature adjustment, be 200 ℃～250 ℃ calcinations 2.0～3.0 hours.Can obtain the adsorbent that adsorption capacity 15.3mg/g is.
Example 7. mixes the attapulgite of 20g with the diatomite of 8g, joining 30ml concentration is in 45%Mgcl, Alcl3 (Mg: Al is 1: the 1) mixed solution, with content is that the NaOH solution of 1.2molL-1 is regulated its pH to 11.5, obtain sediment, leach sediment and change in the muffle furnace that moves temperature adjustment, be 250 ℃～300 ℃ calcinations 2.0～3.0 hours.Can obtain the adsorbent that adsorption capacity 23.3mg/g is.
The adsorbent that the present invention reaches capacity absorption is placed in the alkaline solution of 0.5mol/L, and at room temperature, through 2～3 hours, dephosphorization rate can reach more than 98%.
Can be used for absorption once more and use for taking off adsorbent after the suction.As getting the adsorbent after the suction of taking off of 0.1g, to put into 20ml concentration be 50mgL
-1Adsorb in the phosphorous Simulated Water, adsorption capacity can reach 8.7mgg after 5 hours
-1Adsorption capacity 9.0mgg with fresh adsorbent under the same terms
-1Very nearly the same.To put into 20ml concentration respectively be 50mgL with take off adsorbent after the suction and the fresh adsorbent of 0.2g
-1Adsorb in the phosphorous Simulated Water, adsorption capacity is respectively 14.9mgg after 10 hours
-1With 9.0mgg
-1
Claims (9)
- The preparation method of 1 one kinds of phosphate radical adsorbers, it is characterized in that it is mixed with the oxychloride aqueous solution that can be hydrolyzed by the inorganic ore deposit soil of the powdery that contains silica, magnesia, aluminium oxide and iron oxide, and regulate mixture with alkaline matter, obtain the sediment of white or brown, carry out the granular adsorption agent that high-temperature process obtains porous again.
- 2 according to the described preparation method of claim 1, it is characterized in that the said inorganic ore deposit soil that contains the mixture of silica, magnesia, aluminium oxide and iron oxide is: the mixture of one or both in attapulgite, natural zeolite, wollastonite and the diatomite.
- 3 according to claim 1 or 2 described preparation methods, it is characterized in that the said oxychloride that can be hydrolyzed is: the mixture of one or both in ferric trichloride, magnesium chloride, zirconium oxychloride and the alchlor, the concentration of the oxychloride aqueous solution are 40～55%.
- 4 according to the described preparation method of claim 1, and when it is characterized in that said inorganic ore deposit soil mixes with the oxychloride aqueous solution that can be hydrolyzed, the pH value of regulating mixture with alkaline matter is 9～12.
- 5 according to the described preparation method of claim 4, it is characterized in that said alkaline matter is a sodium hydrate aqueous solution, and its concentration is 0.5～1.5mol/L.
- 6 according to claim 1 or 2,4,5 described preparation methods, it is characterized in that said high-temperature process is to carry out in the muffle furnace of automatic temperature-control, and its calcination temperature is 200 ℃～300 ℃, and calcination time is 1.5～2.5 hours.
- 7 according to the described preparation method of claim 3, it is characterized in that said high-temperature process is to carry out in the muffle furnace of automatic temperature-control, and its calcination temperature is 200 ℃～300 ℃, and calcination time is 1.5～2.5 hours.
- 8 according to claim 1 or 2,4,5 described preparation methods, it is characterized in that said high-temperature process is that sediment is carried out hydrothermal treatment consists 30～90min under 120-150 ℃, 1.2-1.4atm, the back is dry down at 80 ℃, steam moisture wherein, put into 8～20kw micro-wave oven again and dry by the fire burning 8～15min.
- 9 according to the described preparation method of claim 3, it is characterized in that said high-temperature process is that sediment is carried out hydrothermal treatment consists 30～90min under 120-150 ℃, 1.2-1.4atm, the back is dry under 80 ℃, steams moisture wherein, puts into 8～20kw micro-wave oven again and dries by the fire burning 8～15min.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791534A (en) * | 2010-04-14 | 2010-08-04 | 西南大学 | Phosphorus-removing adsorbent and preparation method thereof |
| CN101249417B (en) * | 2008-03-28 | 2010-12-08 | 合肥工业大学 | Concave-convex bar stone clay-trihydrate alumina/iron nano composite adsorbing agent, preparation and applications |
| CN101966444A (en) * | 2010-11-15 | 2011-02-09 | 西北农林科技大学 | Preparation method of dephosphorisation absorptive material and application thereof |
| CN102350297A (en) * | 2011-09-14 | 2012-02-15 | 安徽师范大学 | Novel adsorbent, preparation method and application thereof |
| CN102515830A (en) * | 2012-01-05 | 2012-06-27 | 武汉科技大学 | Reproducible phosphorus-uptake ceramsite and preparation method thereof |
| CN102527328A (en) * | 2012-02-16 | 2012-07-04 | 北京科技大学 | Method for preparing adsorbing material for removing phosphate from sewage |
| CN106811200A (en) * | 2017-01-13 | 2017-06-09 | 环保桥（湖南）生态环境修复有限公司 | A kind of complex repairation agent for reducing arsenic content in the crops of arsenic pollution area and preparation method thereof |
| CN107265548A (en) * | 2017-07-05 | 2017-10-20 | 盛隆资源再生（无锡）有限公司 | A kind of method using the attapulgite depth adsorption and dephosphorization for loading hydrated ferric oxide |
| US10246346B2 (en) | 2012-08-30 | 2019-04-02 | Nclear Inc. | Compositions and methods for the removal of phosphates and other contaminants from aqueous solutions |
| CN110433782A (en) * | 2019-07-18 | 2019-11-12 | 北京科技大学 | A kind of calcium sulfate crystal whiskers support the preparation method of porous oxide defluorination material |
| CN111871365A (en) * | 2020-07-22 | 2020-11-03 | 中国电建集团华东勘测设计研究院有限公司 | Aluminum-zirconium modified zeolite, preparation method and method for controlling release of nitrogen and phosphorus in polluted bottom mud |
| CN113000015A (en) * | 2021-03-10 | 2021-06-22 | 南方科技大学 | Preparation method and dephosphorization application of attapulgite-periclase-based hydrotalcite |
| CN113083219A (en) * | 2021-05-12 | 2021-07-09 | 昆明理工大学 | Method for preparing denitrification and dephosphorization adsorbent from yellow phosphorus slag and application |
-
2005
- 2005-08-19 CN CN 200510014769 patent/CN1748857A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101249417B (en) * | 2008-03-28 | 2010-12-08 | 合肥工业大学 | Concave-convex bar stone clay-trihydrate alumina/iron nano composite adsorbing agent, preparation and applications |
| CN101791534A (en) * | 2010-04-14 | 2010-08-04 | 西南大学 | Phosphorus-removing adsorbent and preparation method thereof |
| CN101966444A (en) * | 2010-11-15 | 2011-02-09 | 西北农林科技大学 | Preparation method of dephosphorisation absorptive material and application thereof |
| CN101966444B (en) * | 2010-11-15 | 2012-11-14 | 西北农林科技大学 | Preparation method of dephosphorisation absorptive material and application thereof |
| CN102350297A (en) * | 2011-09-14 | 2012-02-15 | 安徽师范大学 | Novel adsorbent, preparation method and application thereof |
| CN102350297B (en) * | 2011-09-14 | 2013-06-12 | 安徽师范大学 | Adsorbent, preparation method and application thereof |
| CN102515830A (en) * | 2012-01-05 | 2012-06-27 | 武汉科技大学 | Reproducible phosphorus-uptake ceramsite and preparation method thereof |
| CN102527328A (en) * | 2012-02-16 | 2012-07-04 | 北京科技大学 | Method for preparing adsorbing material for removing phosphate from sewage |
| US10246346B2 (en) | 2012-08-30 | 2019-04-02 | Nclear Inc. | Compositions and methods for the removal of phosphates and other contaminants from aqueous solutions |
| CN106811200A (en) * | 2017-01-13 | 2017-06-09 | 环保桥（湖南）生态环境修复有限公司 | A kind of complex repairation agent for reducing arsenic content in the crops of arsenic pollution area and preparation method thereof |
| CN106811200B (en) * | 2017-01-13 | 2020-04-24 | 环保桥（湖南）生态环境修复有限公司 | Composite repairing agent for reducing arsenic content in crops in arsenic-polluted area and preparation method thereof |
| CN107265548A (en) * | 2017-07-05 | 2017-10-20 | 盛隆资源再生（无锡）有限公司 | A kind of method using the attapulgite depth adsorption and dephosphorization for loading hydrated ferric oxide |
| CN110433782A (en) * | 2019-07-18 | 2019-11-12 | 北京科技大学 | A kind of calcium sulfate crystal whiskers support the preparation method of porous oxide defluorination material |
| CN110433782B (en) * | 2019-07-18 | 2020-10-02 | 北京科技大学 | Preparation method of calcium sulfate whisker supported porous oxide fluorine removal material |
| CN111871365A (en) * | 2020-07-22 | 2020-11-03 | 中国电建集团华东勘测设计研究院有限公司 | Aluminum-zirconium modified zeolite, preparation method and method for controlling release of nitrogen and phosphorus in polluted bottom mud |
| CN111871365B (en) * | 2020-07-22 | 2023-04-07 | 中国电建集团华东勘测设计研究院有限公司 | Aluminum-zirconium modified zeolite, preparation method and method for controlling release of nitrogen and phosphorus in polluted bottom mud |
| CN113000015A (en) * | 2021-03-10 | 2021-06-22 | 南方科技大学 | Preparation method and dephosphorization application of attapulgite-periclase-based hydrotalcite |
| CN113083219A (en) * | 2021-05-12 | 2021-07-09 | 昆明理工大学 | Method for preparing denitrification and dephosphorization adsorbent from yellow phosphorus slag and application |
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