CN105080483A - Preparation method of aluminum carried pulverized fuel ash applied to recycling of phosphorus resources in waste water - Google Patents
Preparation method of aluminum carried pulverized fuel ash applied to recycling of phosphorus resources in waste water Download PDFInfo
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- CN105080483A CN105080483A CN201510503713.4A CN201510503713A CN105080483A CN 105080483 A CN105080483 A CN 105080483A CN 201510503713 A CN201510503713 A CN 201510503713A CN 105080483 A CN105080483 A CN 105080483A
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Abstract
The invention discloses a preparation method of aluminum carried pulverized fuel ash applied to recycling of phosphorus resources in waste water, and relates to the technical field of preparation methods of phosphorus adsorbents. The preparation method comprises the following steps: soaking pulverized fuel ash in a container accommodating a water soluble aluminum salt solution, thereby adsorbing a surface layer containing aluminum ions onto the surface of the pulverized fuel ash; then, pouring the water soluble aluminum salt solution out of the container, washing the pulverized fuel ash with water, and adding water into the container with the pulverized fuel ash, wherein the water surface is higher than the pulverized fuel ash; subsequently, dropwise adding alkali liquor into the water while stirring to ensure that the pH value of the water slowly increases to 7.5-8.0, wherein the whole process of dropwise adding the alkali liquor lasts for 0.5-1.5 hours; and finally, separating the pulverized fuel ash from the water, and airing. The aluminum carried pulverized fuel ash can be used for effectively adsorbing phosphate radicals in waste water, has large adsorption capacity when the content of phosphorus in a water solution is high, and is easy to recover.
Description
Technical field
The present invention relates to preparation method's technical field of the adsorbent being applied to reclamation of phosphorus resource in phosphorus-containing wastewater, be specially a kind of preparation method carrying aluminium powder coal ash for Phosphorus From Wastewater resource reclaim.
Background technology
Phosphorus is non-renewable resources, how to realize the sustainable use of phosphor resource, is one of crucial problem of facing of various countries' agricultural sustainable development.In traditional agriculture, phosphorus realizes recycling of phosphor resource along " field is returned in agricultural land soil-crops-food-excrement dirt-excrement dirt "; The present age chemical fertilizer industry development, for agricultural provide use convenient, the chemical fertilizer that nutrient density is high, instead of the traditional agriculture source of manure, excrement dirt is often with municipal wastewater discharge, and the phosphor resource in excrement dirt is one-way flow, not only accelerate the consumption of phosphor resource, also threaten to water environment safety.If effectively reclaim phosphor resource from municipal wastewater, in the regeneration of phosphor resource, meaning will have very large meaning, also will be conducive to protection and the improvement of water environment.
The recovery of Phosphorus From Wastewater resource, technically, mainly contains the precipitation method, absorption method two kinds.The guanite production technology be widely studied in the world is a kind of typical precipitation method.This method requires that in environment, phosphate radical, ammonium root, magnesium ion and pH will be in appropriate scope.Therefore, if directly applied in municipal wastewater, efficiency will be very low.In municipal wastewater pipeline, guanite is also only present in pipeline corner, is the result of long term accumulation.Absorption method is extensive use in the tertiary treatment of waste water at present.In three grades of advanced treating of waste water, often adopt polymeric adsorbent as adsorbent, remove the pollutant such as nitrate anion, phosphate radical in waste water.Because the cost of this advanced treatment process is high, the Sewage Plant of carrying out Sewage advanced treatment at present is at home also few.Utilize cheap sorbing material, be conducive to the cost reducing Sewage advanced treatment.
About the sorbing material being applied to Phosphorus From Wastewater resource reclaim, at present, some researchers propose to utilize active carbon as carrier, and high-temperature process under anoxybiotic environment, to load iron at activated carbon surface, makes efficient adsorbent.What propose as Zhang Qiaoli carries iron active carbon preparation method (200510110226.8).But carrying iron active carbon cannot be used for anaerobic environment, and under anaerobic, the iron of activated carbon surface will be converted into ferrous iron and dissolve.On the other hand, activated carbon granule is tiny, and after processing is completed, how realizing Separation of Solid and Liquid is also one of difficulty.
Flyash is commonly used for adsorbent, and it obtains the absorption property of various pollutant and studies widely, and utilizing flyash to carry out modification as material has also had a lot of report to strengthen its absorption property.But flyash loading iron, aluminium are not then appeared in the newspapers to make the sorbing material being applied to reclamation of phosphorus resource, this is mainly, it is generally acknowledged, flyash itself is rich in iron aluminium, and (flyash about 50% is silica, 20-30% is aluminium oxide, about 10% is iron oxide), do not need to reload iron aluminium; Be on the other hand, flyash, as the research of adsorbent, is the flying dust adopted mostly.Particle size of fly ash specific activity charcoal is also tiny, owing to having very large surface area, makes it have extremely strong adsorption active.But also just because of particle is tiny, hinder the practical application of flying dust in adsorption cleaning field.Because particle is tiny, it is difficult to carry out Separation of Solid and Liquid, and therefore, although flying dust has very strong adsorption capacity, rarely found its is applied in production practices.
Wet ash discharge is the part that in flyash, particle is larger, although wherein have part because inner bubble-contained, thus form hollow bead, can swim in the water surface, major part is easy to precipitation, is easy to be separated with water.Because wet ash discharge specific area is little, although also containing a large amount of iron, aluminum oxide, be wrapped in granule interior more.Existing research shows, the wet adsorption capacity of ash discharge to the many kinds of substance comprising phosphate radical is more weak.Therefore, under study for action, also seldom there is researcher that wet ash discharge is studied as adsorbent.
Summary of the invention
The object of this invention is to provide a kind of preparation method carrying aluminium powder coal ash for Phosphorus From Wastewater resource reclaim.
For achieving the above object, technical scheme of the present invention is: a kind of preparation method carrying aluminium powder coal ash for Phosphorus From Wastewater resource reclaim, comprises the steps:
(1), by flyash be placed in the container filling aqueous aluminum salt solution and soak, to contain aluminum ions superficial layer at flyash adsorption one deck;
(2), the aqueous aluminum salt solution outwelled in container, and with after water cleaning powder coal ash, add water in the container of flyash place, and make the water surface higher than flyash;
(3), in water, drip alkali lye under stirring action, make the pH value of water slowly be increased to 7.5-8.0, controlling the time that whole alkali lye drips process is 0.5 ~ 1.5 hour;
In this step, controlling alkali lye, to drip time of process be that trivalent aluminium ion and alkali lye in order to make flyash adsorption fully reacts.If add alkali lye soon, owing to reacting incomplete, have trivalent aluminium desorption out.And rapid mixing, is difficult to ensure that aluminum hydroxide precipitation is formed at flyash surface;
(4), by flyash isolate from water, dry.
Described water-soluble aluminum salt is aluminum sulfate, aluminum nitrate or aluminium chloride, by the immersion of aqueous aluminum salt solution, the aluminium ion in solution is adsorbed onto flyash surface, thus forms a kind of superficial layer of rich aluminium at the outer surface of flyash.The concentration of described aqueous aluminum salt solution is 0.05-0.6molL
-1.
Described alkali lye is sodium hydroxide solution or potassium hydroxide solution.Regulated by pH, the trivalent aluminium ion being adsorbed in flyash surface can be formed surface precipitation.Owing to being adsorbed on the trivalent aluminium ion on flyash surface, density is not high generally, therefore, when precipitating with NaOH or potassium hydroxide, the more complete crystal of aluminium hydroxide can't be formed, but forming the amorphous hydroted alumina be similar in soil, this makes it want large many to the adsorption capacity of phosphorus.
The present invention is carried in the preparation method of aluminium powder coal ash, described flyash is the wet ash discharge of next steam power plant, wet ash discharge is larger relative to the flying dust particle of flyash, wet ash discharge is as adsorbing agent carrier, be easy to sedimentation, be beneficial to and be separated with water, the regeneration of adsorbent can be realized, recycle, there is larger actual application value.
Further, after being isolated from water by flyash, then heat 6-16 hour at the temperature being placed on more than 300 DEG C.Flyash after base extraction, surface precipitation one deck aluminium hydroxide, owing to being amorphous hydroted alumina, a large amount of hydrone of its adsorption.Because hydrone can affect the structure of aluminium hydroxide, also may affect its adsorption capacity simultaneously, therefore applicant adopts different temperature to process the obtained aluminium powder coal ash that carries, and examine treatment of different temperature, and without high-temperature process carry aluminium powder coal ash to the difference of the adsorption capacity of phosphorus.Result shows: without high-temperature process, and the sample that treatment temperature is less than 300 DEG C, and it does not have very large difference to the adsorption capacity of phosphorus in maximal absorptive capacity, but more weak to the adsorption capacity of phosphorus in low-concentration phosphorus-containing wastewater.Only have year aluminium powder coal ash through more than 300 DEG C high-temperature process, just have from 1mg-PL
-1the ability of Phosphate Sorption in following concentration.Temperature in this step also can use higher temperature, as 700-800 DEG C.But higher temperature not necessarily, higher temperature can cause energy requirement larger on the one hand, and high temperature can make aluminium hydroxide dehydration be aluminium oxide on the other hand, but how many adsorption capacities is not changed.In concrete operations, high-temperature process 6-16 hour at 300-350 DEG C can be adopted.
Further, before being soaked by flyash aqueous aluminum salt solution, carry out pretreatment, namely first flyash watery hydrochloric acid or dilute sulfuric acid are soaked, to etch flyash surface.Flyash is formation of at high temperature burning, and based on silica, wrap up various hopcalite matter, these oxides comprise calcium oxide, magnesia, iron oxide, aluminium oxide etc.After with watery hydrochloric acid or dilute sulfuric acid process, the part in these oxides just defines chloride, is dissolved in the aqueous solution, thus forms various hole at silica surface, is conducive to the surface area increasing flyash, improves adsorption capacity.
Beneficial effect: prepared by the present invention carry an aluminium powder coal ash can effectively adsorb the phosphate radical in waste water, for when phosphorus content is higher in the aqueous solution, has very large adsorption capacity, thus can phosphor resource preferably in recycle-water solution.
Through higher than after the Temperature Treatment of 300 DEG C carry aluminium powder coal ash, it has from 1mg-PL
-1the ability of Phosphate Sorption in following concentration, for when in the aqueous solution, phosphorus content is lower, it has very strong concentration control effects, within the specific limits, effectively can play cushioning effect to the phosphorus in solution, thus phosphorus concentration is controlled within the scope of safety dumping (as 0.5mgL
-1).
Year aluminium powder coal ash prepared by the present invention is the solid waste flyash of employing power plant is raw material, has both achieved the resource of discarded object, and has achieved again the recovery of phosphor resource, kill two birds with one stone.
Compared with year iron active carbon, prepared by the present invention carries an aluminium powder coal ash 2 remarkable advantages in preparation method: one, do not need anoxybiotic; Two, the high-temperature process of more than 700 DEG C is not needed.Preparation method is simple, mild condition, consumes energy low, and a prepared year aluminium powder coal ash can adapt to anaerobic environment.
Prepared by the present invention carries aluminium powder coal ash as phosphorus sorbing material, and it brings back to life easily, and after bringing back to life, adsorption capacity declines little, is easy to apply in actual production.
Detailed description of the invention
In following examples, flyash adopts the wet ash discharge of steam power plant to be raw material, and particle diameter is about 60 orders.
Embodiment 1
Carry the preparation method of aluminium powder coal ash: first, be placed in by flyash and fill 0.05molL
-1aluminum sulfate solution container in, soak 1 round the clock; Then, outwell the aluminum sulfate solution in container, and with water cleaning powder coal ash, after cleaned, water is outwelled, then adds water in the container of flyash place, and makes the water surface higher than flyash; Afterwards, drip sodium hydroxide solution under stirring action in water, make the pH value of water slowly be increased to 7.5-8.0, the time controlling whole sodium hydroxide solution dropping process is 0.5 hour; Finally, flyash is isolated from water, dry.
Embodiment 2
Carry the preparation method of aluminium powder coal ash: first, be placed in by flyash and fill 0.6molL
-1aluminum nitrate solution container in, soak 1 round the clock; Then, outwell the aluminum nitrate solution in container, and with water cleaning powder coal ash, after cleaned, water is outwelled, then adds water in the container of flyash place, and makes the water surface higher than flyash; Afterwards, drip potassium hydroxide solution under stirring action in water, make the pH value of water slowly be increased to 7.5-8.0, the time controlling whole potassium hydroxide solution dropping process is 1.5 hours; Finally, flyash is isolated from water, and puts into Muffle furnace high-temperature process 16 hours at 300 DEG C.
Embodiment 3
Carry the preparation method of aluminium powder coal ash: first, by flyash at 0.1molL
-1dilute sulfuric acid in soak 3 round the clock; Then, flyash is placed in fills 0.3molL
-1liquor alumini chloridi container in, soak 1 round the clock; Then, outwell the liquor alumini chloridi in container, and with water cleaning powder coal ash, after cleaned, water is outwelled, then adds water in the container of flyash place, and makes the water surface higher than flyash; Afterwards, drip potassium hydroxide solution under stirring action in water, make the pH value of water slowly be increased to 7.5-8.0, the time controlling whole potassium hydroxide solution dropping process is 1 hour; Finally, flyash is isolated from water, dry.
Embodiment 4
Carry the preparation method of aluminium powder coal ash: first, by flyash at 0.1molL
-1watery hydrochloric acid in soak 3 round the clock; Then, flyash is placed in fills 0.2molL
-1aluminum sulfate solution container in, soak 1 round the clock; Then, outwell the aluminum sulfate solution in container, and with water cleaning powder coal ash, after cleaned, water is outwelled, then adds water in the container of flyash place, and makes the water surface higher than flyash; Afterwards, drip sodium hydroxide solution under stirring action in water, make the pH value of water slowly be increased to 7.5-8.0, the time controlling whole sodium hydroxide solution dropping process is 1 hour; Finally, flyash is isolated from water, and puts into Muffle furnace high-temperature process 6-8 hour at 350 DEG C.
Prepared by the present invention carries aluminium powder coal ash in the application of reclaiming Phosphorus From Wastewater resource, can mix, shaking carrying aluminium powder coal ash 1 hour, staticly settling, discharging tail water, reclaiming and carry aluminium powder coal ash with the ratio of phosphorus-containing wastewater according to cement-water ratio 1:5.If Phosphorus From Wastewater concentration is very low, after a year aluminium powder coal ash can repeatedly utilize, then bring back to life; If Phosphorus From Wastewater concentration is higher, carrying after aluminium powder coal ash needs bring back to life of recovery just can reuse.
Carry the resurrection of aluminium powder coal ash: year aluminium powder coal ash and the 0.3-0.6molL that have adsorbed phosphorus
-1sodium bicarbonate solution mixing, shake 1 hour, isolates a year aluminium powder coal ash, namely complete resurrection process.A year aluminium powder coal ash after resurrection can again for the absorption of phosphorus.Bring back to life the phosphate radical containing higher concentration in the tail water produced, can be used for guanite technique phosphorus precipitation and reclaim.
Carry aluminium powder coal ash as phosphate fertilizer: the aluminium powder coal ash that carries saturated for absorption is directly used as phosphate fertilizer, in being manured into soil.Because flyash is through the pretreatment of watery hydrochloric acid or dilute sulfuric acid, carry toxic heavy metal content in aluminium powder coal ash extremely low, its activity is not high yet, can not produce poison crop.This is because some heavy metal ion and phosphate radical can form the extremely low salt of solubility, and in the environment being rich in phosphate radical, these heavy metals can only exist with water-fast form, can not be Crop.
Phosphorus adsorption experiment: for preparing for the embodiment of the present invention 4 carries aluminium powder coal ash, tests its adsorption capacity in the phosphorus-containing wastewater of variable concentrations, and the adsorption capacity of carrying aluminium powder coal ash after bringing back to life is tested, result of the test is as follows:
Aluminium powder coal ash is carried to the adsorbance of phosphorus and equilibrium concentration in table 1 low-concentration phosphorus-containing wastewater
Table 2: carry aluminium powder coal ash in high-concentration phosphorus-containing wastewater to the adsorbance of phosphorus and equilibrium concentration
Illustrate: in table 1 and table 2, identical to the method for testing of carrying aluminium powder Coal Ash Adsorption ability.Initial concentration refers to phosphate concentration initial in solution containing phosphate; Equilibrium concentration refers to after adsorption equilibrium, the phosphorus concentration in solution containing phosphate; Adsorbance refers to after adsorption equilibrium, carries the quality of the phosphorus that aluminium powder coal ash adsorbs; First time refers to that year aluminium powder coal ash first time of preparation is for adsorbing the phosphorus in solution containing phosphate; Second time refers to that year aluminium powder coal ash used once is after bringing back to life through sodium acid carbonate, and second time is used for absorption; Third time refers to that year aluminium powder coal ash after second time absorption is after bringing back to life through sodium acid carbonate, and third time is used for absorption.In table 1 and table 2, same to data line, desorption balance data each time for the phosphorus concentration of solution containing phosphate be identical, namely before absorption each time, in solution containing phosphate, the concentration of phosphorus is the first row data of every a line in table.
Table 1 result of the test shows: for year aluminium powder coal ash of fresh first use, for phosphorus content not higher than 4mgL
-1solution containing phosphate, final phosphate concentration in solution containing phosphate can be controlled and be less than 0.5mgL
-1.And when using a year aluminium powder coal ash once to reuse after resurrection, when phosphorus concentration content is too low in solution, can phosphorus be discharged.
Table 2 result of the test shows: when in solution containing phosphate, phosphorus concentration is higher, and carrying aluminium powder coal ash also has very large adsorption capacity to the phosphorus in solution containing phosphate.And, even if employing after twice, to concentration at 25mgL
-1above solution containing phosphate still has stronger absorption crystallized ability.
Claims (7)
1., for the preparation method carrying aluminium powder coal ash of Phosphorus From Wastewater resource reclaim, it is characterized in that: comprise the steps:
(1), by flyash be placed in the container filling aqueous aluminum salt solution and soak, to contain aluminum ions superficial layer at flyash adsorption one deck;
(2), the aqueous aluminum salt solution outwelled in container, and with after water cleaning powder coal ash, add water in the container of flyash place, and make the water surface higher than flyash;
(3), in water, drip alkali lye under stirring action, make the pH value of water slowly be increased to 7.5-8.0, controlling the time that whole alkali lye drips process is 0.5 ~ 1.5 hour;
(4), by flyash isolate from water, dry.
2. a kind ofly as claimed in claim 1 carry the preparation method of aluminium powder coal ash for Phosphorus From Wastewater resource reclaim, it is characterized in that: after flyash is isolated from water, then heat 6-16 hour at the temperature being placed on more than 300 DEG C.
3. a kind ofly as claimed in claim 1 carry the preparation method of aluminium powder coal ash for Phosphorus From Wastewater resource reclaim, it is characterized in that: described water-soluble aluminum salt is aluminum sulfate, aluminum nitrate or aluminium chloride.
4. a kind ofly as claimed in claim 3 carry the preparation method of aluminium powder coal ash for Phosphorus From Wastewater resource reclaim, it is characterized in that: the concentration of described aqueous aluminum salt solution is 0.05-0.6molL
-1.
5. a kind ofly as claimed in claim 1 carry the preparation method of aluminium powder coal ash for Phosphorus From Wastewater resource reclaim, it is characterized in that: described alkali lye is sodium hydroxide solution or potassium hydroxide solution.
6. a kind ofly as claimed in claim 1 carry the preparation method of aluminium powder coal ash for Phosphorus From Wastewater resource reclaim, it is characterized in that: before flyash aqueous aluminum salt solution is soaked, first flyash watery hydrochloric acid or dilute sulfuric acid are soaked, to etch flyash surface.
7. a kind of preparation method carrying aluminium powder coal ash for Phosphorus From Wastewater resource reclaim as described in any one of claim 1 ~ 6, is characterized in that: described flyash is the wet ash discharge of next steam power plant.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330000A (en) * | 2015-12-16 | 2016-02-17 | 武汉工程大学 | Treatment method of phosphoric acid wastewater |
| CN110385104A (en) * | 2019-05-17 | 2019-10-29 | 北京化工大学 | A kind of modified zeolite flyash composite adsorbing material and preparation method thereof |
| CN111097374A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院生态环境研究中心 | Preparation method of oxygen-carrying and adsorption composite functional material and application of oxygen-carrying and adsorption composite functional material in water body remediation |
| CN111097373A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院生态环境研究中心 | Porous adsorption material, oxygen-carrying and adsorption composite functional material and application thereof |
| CN111892229A (en) * | 2020-07-31 | 2020-11-06 | 江苏启创环境科技股份有限公司 | Method for deeply purifying and efficiently recovering trace phosphorus in biochemical tail water |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105330000A (en) * | 2015-12-16 | 2016-02-17 | 武汉工程大学 | Treatment method of phosphoric acid wastewater |
| CN105330000B (en) * | 2015-12-16 | 2017-10-10 | 武汉工程大学 | A kind of processing method of phosphoric acid waste water |
| CN111097374A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院生态环境研究中心 | Preparation method of oxygen-carrying and adsorption composite functional material and application of oxygen-carrying and adsorption composite functional material in water body remediation |
| CN111097373A (en) * | 2018-10-25 | 2020-05-05 | 中国科学院生态环境研究中心 | Porous adsorption material, oxygen-carrying and adsorption composite functional material and application thereof |
| CN110385104A (en) * | 2019-05-17 | 2019-10-29 | 北京化工大学 | A kind of modified zeolite flyash composite adsorbing material and preparation method thereof |
| CN111892229A (en) * | 2020-07-31 | 2020-11-06 | 江苏启创环境科技股份有限公司 | Method for deeply purifying and efficiently recovering trace phosphorus in biochemical tail water |
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Application publication date: 20151125 |