CN104971687A - Efficient compound iron-based phosphorous-removing adsorbent as well as preparation method, application method and regeneration method thereof - Google Patents
Efficient compound iron-based phosphorous-removing adsorbent as well as preparation method, application method and regeneration method thereof Download PDFInfo
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Abstract
The invention provides an efficient compound iron-based phosphorous-removing adsorbent as well as a preparation method, an application method and a regeneration method thereof, relates to a solid adsorbent composition, and particularly relates to a solid adsorbent composition for adsorbing phosphorous. The invention aims at providing the efficient compound iron-based phosphorous-removing adsorbent which is simple to prepare, has a good adsorption effect and is convenient to regenerate, as well as the preparation method, the application method and the regeneration method thereof. The efficient compound iron-based phosphorous-removing adsorbent comprises an iron-based oxide and a carrier; the mass ratio of the iron-based oxide to the carrier is (1-10) to 100. The preparation method provided by the invention is simple and easy to operate; the prepared efficient compound iron-based phosphorous-removing adsorbent has good adsorption efficiency on phosphorous in a wide spectrum pH value range; good phosphorous-removing capability can be recovered through simple regeneration operation. The efficient compound iron-based phosphorous-removing adsorbent can be used for the field of materials for removing pollutants including phosphorous in domestic sewage and industrial sewage through an adsorption method.
Description
Technical field
The present invention relates to a kind of solid sorbent compositions, particularly relate to a kind of solid sorbent compositions for Phosphate Sorption.
Background technology
Phosphorus is one of all life entities indispensable element of depending on for existence, and be also a kind of non-renewable resources, the phosphorus ore resource reserves of occurring in nature are limited.The one in 20 kinds of mineral products of national economic development demand can not be met after China's phosphorus ore has been listed in 2010.While phosphor resource faces scarcity, excessive phosphorus discharge causes the crisis of body eutrophication in the world, and the economic loss that annual " wawter bloom " and " red tide " causes is up to more than 10,000,000,000 yuan.Research shows, the governing factor in most eutrophication water is phosphorus, and therefore, waste water dephosphorization is the important means of prevention body eutrophication.
Under the pressure of the severe situation of body eutrophication, national governments and the common people require more to improve to municipal sewage treatment in recent years, index about nutrient salts in sewage drainage standard is also more and more stricter, in order to reach discharge standard, increasing municipal sewage plant all introduces the sewage treatment process with denitrogenation dephosphorizing function, in clarifying urban sewage while organic pollution, significantly cut down the nitrogen and phosphorus content in water outlet.But at present due to a variety of causes, a lot of Sewage Plant biological denitrification phosphorous removal technique effect does not reach expection, and water outlet phosphorus only relies on biological phosphate-eliminating more difficult up to standard.Absorption method dephosphorization utilizes the solid matter of some porous or bigger serface to the affinity of phosphate anion in water, the technology of phosphorus removal from wastewater realized.The physical absorption that phosphorus is shown by adsorbent, ion-exchange or show coprecipitation process, realize phosphorus from the separation sewage, and can reclaim phosphor resource further by desorb process.The key of absorption method dephosphorization is to find efficient adsorbent.
Summary of the invention
The technical problem to be solved in the present invention is to provide that one is prepared simply, advantages of good adsorption effect, regenerate high efficiency composition iron-based dephosphorization adsorbent and preparation method thereof, using method and renovation process easily.
A kind of high efficiency composition iron-based of the present invention dephosphorization adsorbent, comprises iron-based oxide and carrier; The mass ratio of described iron-based oxide and carrier is 1-10:100;
Wherein, described iron-based oxide is the mixture of ferric hydrous oxide (FeOxHy) and hydration lanthanum-oxides (LaOxHy); Described carrier is diatomite.
The preparation method of a kind of high efficiency composition iron-based of the present invention dephosphorization adsorbent, it comprises the following steps:
One, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye is prepared respectively;
Two, under the condition of aeration agitation and 60-90 DEG C of water-bath, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye that step one is obtained fully mix, and continue aeration agitation 2-6h;
Three, add diatomite and shake 2-4h, leaving standstill 2-24h and be used for ageing, abandon supernatant, is 6.8-7.8 with clean water solid to cleaning fluid pH;
Four, by the solid dry 2-12h at 50-75 DEG C after cleaning in step 3, be then warming up to 100-105 DEG C and keep 2-24h, for drying, i.e. obtained high efficiency composition iron-based dephosphorization adsorbent.
Further, the preparation method of high efficiency composition iron-based dephosphorization adsorbent of the present invention, described iron salt solutions is one or more in ferric chloride solution, ferrum sulfuricum oxydatum solutum, iron nitrate solution; Described ferrous salt solution is one or more in solution of ferrous chloride, copperas solution, ferrous nitrate solution; Described lanthanum salting liquid is lanthanum chloride solution; Described alkali lye is one or more in NaOH, potassium hydroxide.
Further, the preparation method of high efficiency composition iron-based dephosphorization adsorbent of the present invention, in described iron salt solutions and ferrous salt solution, ferro element is 1-10 with the ratio (i.e. nFe:nLa) of the molal quantity of lanthanum element in lanthanum salting liquid; Ferro element and ratio (i.e. (nFe+nLa): the nOH of the molal quantity sum of lanthanum element in lanthanum salting liquid with the molal quantity of hydroxide ion in alkali lye in described iron salt solutions and ferrous salt solution
-) be 0.5-2.
Further, the preparation method of high efficiency composition iron-based dephosphorization adsorbent of the present invention, uses air or pure oxygen during described aeration.
The using method of a kind of high efficiency composition iron-based of the present invention dephosphorization adsorbent, comprises the following steps: be filled in fixed bed reactors by high efficiency composition iron-based dephosphorization adsorbent, is filled with at water source to be clean is flowed out by delivery port by the water inlet of fixed bed reactors; The filtering velocity of described water source to be clean in fixed bed reactors is 0.5-5m/h; When high efficiency composition iron-based dephosphorization adsorbent reaches that in the saturated or water outlet of absorption, phosphorus concentration exceedes required standard, stop water inlet, high efficiency composition iron-based dephosphorization adsorbent is regenerated.
The renovation process of a kind of high efficiency composition iron-based of the present invention dephosphorization adsorbent, described renovation process is dystopy renovation process or in situ regeneration method.
Further, the renovation process of high efficiency composition iron-based dephosphorization adsorbent of the present invention, described dystopy renovation process, comprises the following steps:
One, the saturated high efficiency composition iron-based dephosphorization adsorbent of absorption is taken out from fixed bed reactors;
Two, while stirring the high efficiency composition iron-based dephosphorization adsorbent in step one is added in the highly basic of 1mol/L;
Three, continue to stir 0.5-2h, rinsing solid with clear water, is 6.8-7.8 to cleaning fluid pH.
Further, the renovation process of high efficiency composition iron-based dephosphorization adsorbent of the present invention, described in situ regeneration method, comprises the following steps:
One, the highly basic of 1mol/L is pumped in the fixed bed reactors that high efficiency composition iron-based dephosphorization adsorbent is housed, alkali lye is circulated in fixed bed reactors;
Two, after circulation 0.5-2h, alkali lye is emptying;
Three, using clean water fixed bed reactors, is 6.8-7.8 to cleaning fluid pH.
Further, the renovation process of high efficiency composition iron-based dephosphorization adsorbent of the present invention, the mass ratio of described high efficiency composition iron-based dephosphorization adsorbent and highly basic is 1:50-20.
High efficiency composition iron-based dephosphorization adsorbent of the present invention and preparation method thereof, using method and renovation process difference from prior art are:
1, high efficiency composition iron-based dephosphorization adsorbent of the present invention has moderate pore passage structure and abundant activated adoption position, and specific area is at 150-200m
2/ g, average pore size is
average pore volume is 0.2cm
3/ g, thus (4-10) has good adsorbent usefulness to phosphorus within the scope of broad-spectrum pH.
2, high efficiency composition iron-based dephosphorization adsorbent of the present invention can show good removal effect to phosphorus.
3, high efficiency composition iron-based dephosphorization adsorbent of the present invention has fast, the capacious feature of adsorption rate, has excellent purification of water quality usefulness.
4, the preparation method of high efficiency composition iron-based dephosphorization adsorbent of the present invention is simple, with low cost.
5, the renovation process of high efficiency composition iron-based dephosphorization adsorbent of the present invention comprises in-situ regeneration and dystopy regeneration, and method is simple, and regeneration effect is good; Only need simple regenerative operation can recover excellent dephosphorization ability.
Detailed description of the invention
Embodiment 1
The preparation method of the present embodiment high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye is prepared respectively;
Two, under the condition of aeration agitation and 60 DEG C of water-baths, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye that step one is obtained fully mix, and continue aeration agitation 4h;
Three, add diatomite and shake 4h, leaving standstill 12h and be used for ageing, abandon supernatant, is 7.3 with clean water solid to cleaning fluid pH;
Four, by the solid dry 2h at 62 DEG C after cleaning in step 3, be then warming up to 102 DEG C and keep 14h, for drying, i.e. obtained high efficiency composition iron-based dephosphorization adsorbent.
Embodiment 2
The preparation method of the present embodiment high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye is prepared respectively;
Two, under the condition of aeration agitation and 90 DEG C of water-baths, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye that step one is obtained fully mix, and continue aeration agitation 2h;
Three, add diatomite and shake 3h, leaving standstill 24h and be used for ageing, abandon supernatant, is 7.8 with clean water solid to cleaning fluid pH;
Four, by the solid dry 7h at 75 DEG C after cleaning in step 3, be then warming up to 100 DEG C and keep 24h, for drying, i.e. obtained high efficiency composition iron-based dephosphorization adsorbent.
Embodiment 3
The preparation method of the present embodiment high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye is prepared respectively;
Two, under the condition of aeration agitation and 75 DEG C of water-baths, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye that step one is obtained fully mix, and continue aeration agitation 6h;
Three, add diatomite and shake 2h, leaving standstill 2h and be used for ageing, abandon supernatant, is 6.8 with clean water solid to cleaning fluid pH;
Four, by the solid dry 12h at 50 DEG C after cleaning in step 3, be then warming up to 105 DEG C and keep 2h, for drying, i.e. obtained high efficiency composition iron-based dephosphorization adsorbent.
The concentration of iron salt solutions, ferrous salt solution, lanthanum salting liquid, alkali lye in step one in above embodiment, and diatomaceous weight in step 3 is as shown in table 1.
The kind of each raw material and amount in table 1 embodiment 1-3
The each 500mL of above-mentioned solution is prepared according to the concentration of iron salt solutions, ferrous salt solution, lanthanum salting liquid, alkali lye in table 1.The product obtained to sequence number 1-6 in embodiment 1-3 detects, and uses specific area detector measurement the specific area; Average pore size analyzer is used to measure aperture; Pore volume detector is used to measure product pore volume.After measured, the high efficiency composition iron-based dephosphorization adsorbent that above embodiment obtains has moderate pore passage structure and abundant activated adoption position, and specific area is at 150-200m
2/ g, average pore size is
average pore volume is 0.2cm
3/ g.
Embodiment 4
The present embodiment uses the method for high efficiency composition iron-based dephosphorization adsorbent adsorption and dephosphorization, carries out according to the following steps:
To the obtained high efficiency composition iron-based dephosphorization adsorbent of sequence number 1,2 raw material in embodiment 1, be used to be filled in fixed bed reactors, wherein reactor height about 1.2m, diameter 10cm, packing volume 6000cm
3; To be 4.5mg/L, pH by phosphorus concentration be 6.7 water source to be clean, be filled with by the water inlet of fixed bed reactors and flowed out by delivery port; Filtering velocity is 1m/h; The real time measure water outlet phosphorus concentration, after flowing through 95 times of packing volumes, in water outlet, phosphorus concentration is just higher than 0.5mg/L.
Embodiment 5
The present embodiment uses the method for high efficiency composition iron-based dephosphorization adsorbent adsorption and dephosphorization, and difference from Example 4 is: the high efficiency composition iron-based dephosphorization adsorbent of use obtains for using sequence number 3,4 raw material in embodiment 2; Water source phosphorus concentration to be clean is 5mg/L, pH is 4; Filtering velocity is 0.5m/h; The real time measure water outlet phosphorus concentration, after flowing through 125 times of packing volumes, in water outlet, phosphorus concentration is just higher than 0.5mg/L.
Embodiment 6
The present embodiment uses the method for high efficiency composition iron-based dephosphorization adsorbent adsorption and dephosphorization, and difference from Example 4 is: the high efficiency composition iron-based dephosphorization adsorbent of use obtains for using sequence number 5,6 raw material in embodiment 2; Water source phosphorus concentration to be clean is 3mg/L, pH is 10; Filtering velocity is 5m/h; The real time measure water outlet phosphorus concentration, after flowing through 70 times of packing volumes, in water outlet, phosphorus concentration is just higher than 0.5mg/L.
Embodiment 7
The renovation process of the present embodiment to high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, high efficiency composition iron-based dephosphorization adsorbent (the high efficiency composition iron-based dephosphorization adsorbent that in embodiment 1, sequence number 1 is obtained) saturated for absorption is taken out from fixed bed reactors;
Two, add in the highly basic of 1mol/L by the high efficiency composition iron-based dephosphorization adsorbent in step one while stirring, wherein the mass ratio of high efficiency composition iron-based dephosphorization adsorbent and highly basic is 1:5;
Three, continue to stir 1h, rinsing solid with clear water, is 7.3 to cleaning fluid pH.
Embodiment 8
The renovation process of the present embodiment to high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, high efficiency composition iron-based dephosphorization adsorbent (the high efficiency composition iron-based dephosphorization adsorbent that in embodiment 1, sequence number 1 is obtained) saturated for absorption is taken out from fixed bed reactors;
Two, add in the highly basic of 1mol/L by the high efficiency composition iron-based dephosphorization adsorbent in step one while stirring, wherein the mass ratio of high efficiency composition iron-based dephosphorization adsorbent and highly basic is 1:20;
Three, continue to stir 0.5h, rinsing solid with clear water, is 6.8 to cleaning fluid pH.
Embodiment 9
The renovation process of the present embodiment to high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, high efficiency composition iron-based dephosphorization adsorbent (the high efficiency composition iron-based dephosphorization adsorbent that in embodiment 1, sequence number 1 is obtained) saturated for absorption is taken out from fixed bed reactors;
Two, add in the highly basic of 1mol/L by the high efficiency composition iron-based dephosphorization adsorbent in step one while stirring, wherein the mass ratio of high efficiency composition iron-based dephosphorization adsorbent and highly basic is 1:15;
Three, continue to stir 2h, rinsing solid with clear water, is 7.8 to cleaning fluid pH.
Embodiment 10
The renovation process of the present embodiment to high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, the highly basic of 1mol/L is pumped in the fixed bed reactors that the saturated high efficiency composition iron-based dephosphorization adsorbent of absorption (the high efficiency composition iron-based dephosphorization adsorbent that in embodiment 1, sequence number 1 is obtained) is housed, alkali lye is circulated in fixed bed reactors; Wherein the mass ratio of high efficiency composition iron-based dephosphorization adsorbent and highly basic is 1:5;
Two, after circulation 0.5h, alkali lye is emptying;
Three, using clean water fixed bed reactors, is 7.8 to cleaning fluid pH.
Embodiment 11
The renovation process of the present embodiment to high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, the highly basic of 1mol/L is pumped in the fixed bed reactors that the saturated high efficiency composition iron-based dephosphorization adsorbent of absorption (the high efficiency composition iron-based dephosphorization adsorbent that in embodiment 1, sequence number 1 is obtained) is housed, alkali lye is circulated in fixed bed reactors; Wherein the mass ratio of high efficiency composition iron-based dephosphorization adsorbent and highly basic is 1:20;
Two, after circulation 1h, alkali lye is emptying;
Three, using clean water fixed bed reactors, is 6.8 to cleaning fluid pH.
Embodiment 12
The renovation process of the present embodiment to high efficiency composition iron-based dephosphorization adsorbent carries out according to the following steps:
One, the highly basic of 1mol/L is pumped in the fixed bed reactors that the saturated high efficiency composition iron-based dephosphorization adsorbent of absorption (the high efficiency composition iron-based dephosphorization adsorbent that in embodiment 1, sequence number 1 is obtained) is housed, alkali lye is circulated in fixed bed reactors; Wherein the mass ratio of high efficiency composition iron-based dephosphorization adsorbent and highly basic is 1:15;
Two, after circulation 2h, alkali lye is emptying;
Three, using clean water fixed bed reactors, is 7.3 to cleaning fluid pH.
The adsorption capacity of the operating procedure of embodiment 4 to the high efficiency composition iron-based dephosphorization adsorbent after embodiment 7-12 regeneration is used to detect, after measured, use the high efficiency composition iron-based dephosphorization adsorbent full recovery adsorption capacity after embodiment 7-12 step process, after flowing through the water source to be clean of 95 times of packing volumes, in water outlet, phosphorus concentration is just higher than 0.5mg/L.
Known by above embodiment, high efficiency composition iron-based dephosphorization adsorbent of the present invention has excellent adsorption to phosphorus within the scope of broad-spectrum pH, and this is because he has moderate pore passage structure and abundant activated adoption position.High efficiency composition iron-based dephosphorization adsorbent of the present invention has fast, the capacious feature of adsorption rate, when filtering velocity is 5m/h, still can keep good adsorption and dephosphorization ability.The renovation process of high efficiency composition iron-based dephosphorization adsorbent of the present invention is simple, and regeneration effect is good; Only need simple regenerative operation can recover excellent dephosphorization ability.
Although the foregoing describe the specific embodiment of the present invention, it will be understood by those of skill in the art that these only illustrate, protection scope of the present invention is defined by the appended claims.Those skilled in the art, under the prerequisite not deviating from principle of the present invention and essence, can make various changes or modifications to these embodiments, but these change and amendment all falls into protection scope of the present invention.
Claims (10)
1. a high efficiency composition iron-based dephosphorization adsorbent, is characterized in that: comprise iron-based oxide and carrier; The mass ratio of described iron-based oxide and carrier is 1:2-10;
Wherein, described iron-based oxide is the mixture of ferric hydrous oxide (FeOxHy) and hydration lanthanum-oxides (LaOxHy); Described carrier is diatomite.
2. a preparation method for high efficiency composition iron-based dephosphorization adsorbent, is characterized in that comprising the following steps:
One, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye is prepared respectively;
Two, under the condition of aeration agitation and 60-90 DEG C of water-bath, iron salt solutions, ferrous salt solution, lanthanum salting liquid and alkali lye that step one is obtained fully mix, and continue aeration agitation 2-6h;
Three, adding diatomite and shake 2-4h, leaving standstill 2-24h, abandon supernatant, is 6.8-7.8 with clean water solid to cleaning fluid pH;
Four, by the solid dry 2-12h at 50-75 DEG C after cleaning in step 3, be then warming up to 100-105 DEG C and keep 2-24h, be i.e. obtained high efficiency composition iron-based dephosphorization adsorbent.
3. the preparation method of high efficiency composition iron-based dephosphorization adsorbent according to claim 2, is characterized in that: described iron salt solutions is one or more in ferric chloride solution, ferrum sulfuricum oxydatum solutum, iron nitrate solution; Described ferrous salt solution is one or more in solution of ferrous chloride, copperas solution, ferrous nitrate solution; Described lanthanum salting liquid is lanthanum chloride solution; Described alkali lye is one or more in NaOH, potassium hydroxide.
4. the preparation method of high efficiency composition iron-based dephosphorization adsorbent according to claim 2, is characterized in that: in described iron salt solutions and ferrous salt solution, ferro element is 1-10 with the ratio of the molal quantity of lanthanum element in lanthanum salting liquid; In described iron salt solutions and ferrous salt solution, ferro element is 0.5-2 with the molal quantity sum of lanthanum element in lanthanum salting liquid and the ratio of the molal quantity of hydroxide ion in alkali lye.
5. the preparation method of high efficiency composition iron-based dephosphorization adsorbent according to claim 2, is characterized in that: use air or pure oxygen during described aeration.
6. the using method of a high efficiency composition iron-based dephosphorization adsorbent, it is characterized in that, comprise the following steps: high efficiency composition iron-based dephosphorization adsorbent is filled in fixed bed reactors, be filled with by the water inlet of fixed bed reactors at water source to be clean and flowed out by delivery port, the filtering velocity of described water source to be clean in fixed bed reactors is 0.5-5m/h.
7. a renovation process for high efficiency composition iron-based dephosphorization adsorbent, is characterized in that: described renovation process is dystopy renovation process or in situ regeneration method.
8. the renovation process of high efficiency composition iron-based dephosphorization adsorbent according to claim 7, is characterized in that: described dystopy renovation process, comprises the following steps:
One, the saturated high efficiency composition iron-based dephosphorization adsorbent of absorption is taken out from fixed bed reactors;
Two, while stirring the high efficiency composition iron-based dephosphorization adsorbent in step one is added in the highly basic of 1mol/L;
Three, continue to stir 0.5-2h, rinsing solid with clear water, is 6.8-7.8 to cleaning fluid pH.
9. the renovation process of high efficiency composition iron-based dephosphorization adsorbent according to claim 7, is characterized in that: described in situ regeneration method, comprises the following steps:
One, the highly basic of 1mol/L is pumped in the fixed bed reactors that high efficiency composition iron-based dephosphorization adsorbent is housed, alkali lye is circulated in fixed bed reactors;
Two, after circulation 0.5-2h, alkali lye is emptying;
Three, using clean water fixed bed reactors, is 6.8-7.8 to cleaning fluid pH.
10. the renovation process of high efficiency composition iron-based dephosphorization adsorbent according to claim 8 or claim 9, is characterized in that: the mass ratio of described high efficiency composition iron-based dephosphorization adsorbent and highly basic is 1:50-20.
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