CN104923151A - Preparation method and application of modified phosphate adsorbent - Google Patents
Preparation method and application of modified phosphate adsorbent Download PDFInfo
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- CN104923151A CN104923151A CN201510274875.5A CN201510274875A CN104923151A CN 104923151 A CN104923151 A CN 104923151A CN 201510274875 A CN201510274875 A CN 201510274875A CN 104923151 A CN104923151 A CN 104923151A
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Abstract
The invention discloses a preparation method and application of a modified phosphate adsorbent. Attapulgite which is rich and low in coat is taken as a raw material, is treated under high temperature by using a potassium hydroxide-combined tube furnace in advance, and is then modified for the second time by using aluminium polychlorid. The obtained modified phosphate adsorbent is thrown into phosphate wastewater, and thereby phosphate in the phosphate wastewater can be removed by adsorption. The modification method sufficiently utilizes the inherent characteristics of attapulgite, a research finds that the wastewater phosphate removal rate of the modified phosphate adsorbent obtained by the method reaches more than 90 percent, moreover, the method is simple, and is easy to implement, and the invention has a very broad application prospect.
Description
Technical field
The invention belongs to water treatment purification techniques field, be specifically related to a kind of preparation method of modified phosphate adsorbent and the application in water treatment field thereof.
Background technology
Phosphorus is a kind of limitative nutrient required for aqueous bio, along with China's modernization construction and economy develop rapidly, phosphatic use has set foot in the every aspect of our life, and it is widely used in food processing as important food ingredient and functional additive, in washing agent and chemical fertilizer.But thing followed excess emissions problem easily grows organic matter, such as algae, bacterium, thus the body eutrophication problem caused.The main source of the phosphorus in present water body mainly concentrates on sanitary sewage, the industrial wastewater of discharge, and through drainage pipeline discharge urban rainfall runoff, in addition, townm refuse and the trade waste of illegal dumping is also derived from, agricultural surface runoff and poultry cultivation waste water etc.
The method of current dephosphorization mainly contains biological degradation method, chemical precipitation method and absorption method, wherein absorption method because removal efficiency is high, be easy to operation, recyclable phosphor resource and the advantage such as regenerate, receive the concern of people gradually.
Attapulgite is a kind of moisture zeopan clay mineral with unique layer chain structure feature, and aboundresources is a kind of natural nano material, the Na containing non-quantitative
+, Ca
2+, Fe
3+, Al
3+, there is the abilities such as high temperature resistant, the anti-good colloidal nature such as saline and alkaline, higher adsorption bleaching and ion-exchange.
Although existing numerous use adsorbent is used for the parkerized research of water body at present, but majority all also exists very large shortcoming, remove phosphate adsorbent and preparation method thereof as the publication number patent of invention that is CN103495390A discloses a kind of zirconia modified activated carbon, this adsorbent is made up of the raw material of following weight portion: active carbon 100-120, zirconium-n-propylate 3-4, sodium phosphate trimer 5-6, sodium alginate 3-4, PETG 1-2, OTAC 3-4, attapulgite modified 8-10, water are appropriate.Obtained acticarbon has good absorption property to phosphate, but preparation method is complicated.
Publication number is that the patent of invention of CN102941063B discloses a kind of phosphatic method in carbon nanotube adsorption removal water body of zirconia modification, the method by pretreated CNT ultrasonic disperse in zirconyl chloride solution, adopt hydrothermal synthesis method to carry out zirconia modification to CNT, prepare the CNT of zirconia modification; The CNT of zirconia modification is joined in phosphate-containing water body, the phosphate in Adsorption water body.It has good removal effect to phosphate, acid and alkali-resistance, and adsorb consuming time short, treatment effeciency is high, but also there is adsorption treatment effect, problem that adsorbance is lower.
Publication number is that the patent of invention of CN102380350A discloses the removal of a kind of hydroxyapatite modified eggshell sorbent material and reclaims the method for phosphate in waste water, and this patent uses hydroxyapatite modified eggshell to remove phosphate in waste water as adsorbent.Based on its use eggshell, raw material twice laid is in the phosphatic process of waste water, have the features such as material source is wide, twice laid, pollution free green environment protection, but preparation method is complicated.
Not enough in order to overcome these, the present invention selects has wide application prospect, large surface area, mechanical strength is high and chemical stability is good attapulgite, uses aluminium polychloride to carry out modification to it, for the adsorption treatment of heavy metal and dyeing waste water.
Summary of the invention
The technical problem solved: for deficiency of the prior art, of the present inventionly provides a kind of attapulgite modified phosphate adsorbent and preparation method thereof for water treatment purification.
Technical scheme: the preparation method of modified phosphate adsorbent, comprises the steps: 1, potassium hydroxide pretreatment attapulgite; 2, aluminium polychloride modification; 3, shaping.
Concrete step is:
Step one, adds attapulgite in potassium hydroxide solution, and after reaction 0.5 ~ 3h, centrifugal segregation supernatant, at 200 ~ 400 DEG C, fires 3 ~ 12h in nitrogen environment, then naturally cools, and pulverizes, obtains attapulgite powder;
Step 2, takes out step one gained attapulgite powder after calcination 30 ~ 60min at 400 ~ 600 DEG C, sprays polymeric aluminum chlorides solution, and then calcination 3 ~ 12 hours again at 200 ~ 400 DEG C, obtains modified attapulgite powder end;
Step 3, by the grinding of step 2 gained modified attapulgite powder end, obtains described modified phosphate adsorbent.
More specifically, preparation method of the present invention is:
Step one, attapulgite is added in 0.1 ~ 2mol/L potassium hydroxide solution, attapulgite and potassium hydroxide mass volume ratio is made to be 0.1 ~ 0.5g/ml, stirring at room temperature reaction 0.5 ~ 3h, rear centrifugation, naturally cool after sediment is fired 3 ~ 12h with ramp to 200 ~ 400 of 25 ~ 50 DEG C/min DEG C in nitrogen environment, pulverize, obtain attapulgite powder;
The particle diameter of described powder is 40 ~ 200 orders.
Described potassium hydroxide solution concentration is preferably 0.5mol/L.
Step 2, step one gained attapulgite powder is dropped into Muffle furnace 400 ~ 600 DEG C of high temperature sinterings, calcination time is set as 30 ~ 60min, after taking-up, evenly spray concentration is the polymeric aluminum chlorides solution of 10 ~ 100mg/L immediately, make attapulgite powder with spray polymeric aluminum chlorides solution mass volume ratio be 0.02 ~ 0.1g/ml, and calcination 3 ~ 12 hours again at 200 ~ 400 DEG C, obtain modified attapulgite powder end;
The concentration of polymeric aluminum chlorides solution is preferably 50mg/L.
Step 3, by the grinding of step 2 gained modified attapulgite powder end, obtains described modified phosphate adsorbent.
Utilize the modified phosphate adsorbent that above-mentioned preparation method prepares.
The application of the modified phosphate adsorbent utilizing above-mentioned preparation method to prepare in water treatment purification.Especially for phosphatic removal.
Beneficial effect: the present invention uses potassium hydroxide and aluminium polychloride to carry out modification to it, make use of the feature of attapulgite itself fully, obtains modified attapulgite earth adsorbing phosphate being had to excellent adsorption effect.Find that the attapulgite phosphate adsorbent by this method modification removes the attapulgite of ability far above non-modified of phosphate in waste water after deliberation, clearance reaches more than 90%, and attapulgite is rich in minerals, with low cost, preparation method of the present invention is simple, has boundless application prospect in phosphorus in waste water hydrochlorate process field.
Detailed description of the invention:
Below in conjunction with embodiment, the present invention will be further described, raw material not specified in the present invention and instrument, all by commercial acquisition.
Embodiment 1
Attapulgite is added in 0.1 ~ 2mol/L potassium hydroxide solution, the mass volume ratio added is made to be 0.25g/ml, stirring at room temperature reaction 1.5h, rear centrifugal segregation supernatant, is warming up to 300 DEG C, fire in nitrogen environment, programming rate is 50 DEG C/min, and the firing time is 3h, after in nitrogen environment naturally cool, pulverize, obtain attapulgite powder;
Above-mentioned gained attapulgite powder is dropped into Muffle furnace 600 DEG C of high temperature sinterings, calcination time is set as 30min, then take out rapidly, even sprinkling 10mL concentration is the polymeric aluminum chlorides solution of 25mg/L, make attapulgite powder with spray polymeric aluminum chlorides solution mass volume ratio be 0.02g/ml, and calcination 3 hours again at 400 DEG C, obtain modified attapulgite powder end;
By above-mentioned gained modified attapulgite powder end grinding, obtain described modified phosphate adsorbent.
Get modified phosphate adsorbent prepared by the above-mentioned method of modifying of 0.1g, be placed in the potassium dihydrogen phosphate that 50mL concentration is 30mg/L, then at room temperature constant temperature oscillation 30min, rotating speed is 160rpm, reaction terminates rear centrifugal solid-liquid and is separated, and employing molybdenum antimony resistance colorimetric method records the phosphate concn in filtrate.Result of the test finds that the modified phosphate adsorbent under this modified condition is 86.6% to clearance phosphatic in solution.This explanation has good removal effect by phosphate in the modified phosphate Adsorbent For Removal of Heavy of this method of modifying gained.
Embodiment 2
Attapulgite is added in 0.5mol/L potassium hydroxide solution, the mass volume ratio added is made to be 0.14g/ml, stirring at room temperature reaction 0.5h, rear centrifugal segregation supernatant, is warming up to 200 DEG C, fire in nitrogen environment, programming rate is 25 DEG C/min, and the firing time is 6h, after in nitrogen environment naturally cool, pulverize, obtain attapulgite powder;
Above-mentioned gained attapulgite powder is dropped into Muffle furnace 400 DEG C of high temperature sinterings, calcination time is set as 30min, then take out rapidly, even sprinkling 25mL concentration is the polymeric aluminum chlorides solution of 100mg/L, make attapulgite powder with spray polymeric aluminum chlorides solution mass volume ratio be 0.1g/ml, and calcination 6 hours again at 200 DEG C, obtain modified attapulgite powder end;
By above-mentioned gained modified attapulgite powder end grinding, obtain described modified phosphate adsorbent.
Get modified phosphate adsorbent prepared by the above-mentioned method of modifying of 0.1g, be placed in the potassium dihydrogen phosphate that 50mL concentration is 30mg/L, then at room temperature constant temperature oscillation 30min, rotating speed is 160rpm, reaction terminates rear centrifugal solid-liquid and is separated, and employing molybdenum antimony resistance colorimetric method records the phosphate concn in filtrate.Result of the test finds that the modified modified adsorbent under this modified condition is 92.7% to clearance phosphatic in solution.This explanation has good removal effect by phosphate in the modified phosphate Adsorbent For Removal of Heavy of this method of modifying gained.
Embodiment 3
Attapulgite is added in 0.5mol/L potassium hydroxide solution, the mass volume ratio added is made to be 0.5g/ml, stirring at room temperature reaction 0.5h, rear centrifugal segregation supernatant, is warming up to 400 DEG C, fire in nitrogen environment, programming rate is 25 DEG C/min, and the firing time is 9h, after in nitrogen environment naturally cool, pulverize, obtain attapulgite powder;
Above-mentioned gained attapulgite powder is dropped into Muffle furnace 600 DEG C of high temperature sinterings, calcination time is set as 60min, then take out rapidly, even sprinkling 50mL concentration is the polymeric aluminum chlorides solution of 10mg/L, make attapulgite powder with spray polymeric aluminum chlorides solution mass volume ratio be 0.1g/ml, and calcination 9 hours again at 400 DEG C, obtain modified attapulgite powder end;
By above-mentioned gained modified attapulgite powder end grinding, obtain described modified phosphate adsorbent.
Get modified phosphate adsorbent prepared by the above-mentioned method of modifying of 0.1g, be placed in the potassium dihydrogen phosphate that 50mL concentration is 30mg/L, then at room temperature constant temperature oscillation 30min, rotating speed is 160rpm, reaction terminates rear centrifugal solid-liquid and is separated, and employing molybdenum antimony resistance colorimetric method records the phosphate concn in filtrate.Result of the test finds that the modified phosphate adsorbent under this modified condition is 88.3% to clearance phosphatic in solution.This explanation has good removal effect by phosphate in the modified phosphate Adsorbent For Removal of Heavy of this method of modifying gained.
Embodiment 4
Attapulgite is added in 1mol/L potassium hydroxide solution, the mass volume ratio added is made to be 0.1g/ml, stirring at room temperature reaction 3h, rear centrifugal segregation supernatant, is warming up to 400 DEG C, fire in nitrogen environment, programming rate is 35 DEG C/min, and the firing time is 12h, after in nitrogen environment naturally cool, pulverize, obtain attapulgite powder;
Above-mentioned gained attapulgite powder is dropped into Muffle furnace 500 DEG C of high temperature sinterings, calcination time is set as 45min, then take out rapidly, even sprinkling 100mL concentration is the polymeric aluminum chlorides solution of 10mg/L, make attapulgite powder with spray polymeric aluminum chlorides solution mass volume ratio be 0.05g/ml, and calcination 12 hours again at 400 DEG C, obtain modified attapulgite powder end;
By above-mentioned gained modified attapulgite powder end grinding, obtain described modified phosphate adsorbent.
Get modified phosphate adsorbent prepared by the above-mentioned method of modifying of 0.1g, be placed in the potassium dihydrogen phosphate that 50mL concentration is 30mg/L, then at room temperature constant temperature oscillation 30min, rotating speed is 160rpm, reaction terminates rear centrifugal solid-liquid and is separated, and employing molybdenum antimony resistance colorimetric method records the phosphate concn in filtrate.Result of the test finds that the modified phosphate adsorbent under this modified condition is 92.2% to clearance phosphatic in solution.This explanation has good removal effect by phosphate in the modified phosphate Adsorbent For Removal of Heavy of this method of modifying gained.
Embodiment 5
Attapulgite is added in 0.5mol/L potassium hydroxide solution, the mass volume ratio added is made to be 0.25g/ml, stirring at room temperature reaction 3h, rear centrifugal segregation supernatant, is warming up to 300 DEG C, fire in nitrogen environment, programming rate is 35 DEG C/min, and the firing time is 6h, after in nitrogen environment naturally cool, pulverize, obtain attapulgite powder;
Above-mentioned gained attapulgite powder is dropped into Muffle furnace 500 DEG C of high temperature sinterings, calcination time is set as 45min, then take out rapidly, even sprinkling 100mL concentration is the polymeric aluminum chlorides solution of 50mg/L, make attapulgite powder with spray polymeric aluminum chlorides solution mass volume ratio be 0.05g/ml, and calcination 12 hours again at 300 DEG C, obtain modified attapulgite powder end;
By above-mentioned gained modified attapulgite powder end grinding, obtain described modified phosphate adsorbent.
Get modified phosphate adsorbent prepared by the above-mentioned method of modifying of 0.1g, being placed in 50mL concentration is 30mg/L potassium dihydrogen phosphate, then at room temperature constant temperature oscillation 30min, rotating speed is 160rpm, reaction terminates rear centrifugal solid-liquid and is separated, and employing molybdenum antimony resistance colorimetric method records the phosphate concn in filtrate.Result of the test finds that the modified phosphate adsorbent under this modified condition is 96.3% to clearance phosphatic in solution.This explanation has good removal effect by phosphate in the modified phosphate Adsorbent For Removal of Heavy of this method of modifying gained.
Embodiment 6
Attapulgite is added in 1mol/L potassium hydroxide solution, the mass volume ratio added is made to be 0.25g/ml, stirring at room temperature reaction 3h, rear centrifugal segregation supernatant, is warming up to 250 DEG C, fire in nitrogen environment, programming rate is 25 DEG C/min, and the firing time is 6h, after in nitrogen environment naturally cool, pulverize, obtain attapulgite powder;
Above-mentioned gained attapulgite powder is dropped into Muffle furnace 500 DEG C of high temperature sinterings, calcination time is set as 60min, then take out rapidly, even sprinkling 10mL concentration is the polymeric aluminum chlorides solution of 100mg/L, make attapulgite powder with spray polymeric aluminum chlorides solution mass volume ratio be 0.1g/ml, and calcination 6 hours again at 400 DEG C, obtain modified attapulgite powder end;
By above-mentioned gained modified attapulgite powder end grinding, obtain described modified phosphate adsorbent.
Get modified phosphate adsorbent prepared by the above-mentioned method of modifying of 0.1g, be placed in the potassium dihydrogen phosphate that 50mL concentration is 30mg/L, then at room temperature constant temperature oscillation 30min, rotating speed is 160rpm, reaction terminates rear centrifugal solid-liquid and is separated, and employing molybdenum antimony resistance colorimetric method records the phosphate concn in filtrate.Result of the test finds that the modified phosphate adsorbent under this modified condition is 93.6% to clearance phosphatic in solution.This explanation has good removal effect by phosphate in the modified phosphate Adsorbent For Removal of Heavy of this method of modifying gained.
Claims (9)
1. a preparation method for modified phosphate adsorbent, is characterized in that comprising the following steps:
Step one, adds attapulgite in potassium hydroxide solution and reacts 0.5 ~ 3h, then centrifugation, sediment is fired 3 ~ 12h at 200 ~ 400 DEG C in nitrogen environment, then naturally cools, and pulverizes, obtains attapulgite powder;
Step 2, takes out step one gained attapulgite powder after calcination 30 ~ 60min at 400 ~ 600 DEG C, sprays polymeric aluminum chlorides solution, and then calcination 3 ~ 12 hours again at 200 ~ 400 DEG C, obtains modified attapulgite powder end;
Step 3, by the grinding of step 2 gained modified attapulgite powder end, obtains described modified phosphate adsorbent.
2. the preparation method of modified phosphate adsorbent as claimed in claim 1, it is characterized in that described step one is: added by attapulgite in 0.1 ~ 2mol/L potassium hydroxide solution, attapulgite and potassium hydroxide mass volume ratio is made to be 0.1 ~ 0.5g/ml, stirring at room temperature reaction 0.5 ~ 3h, rear centrifugation, naturally cool after sediment is fired 3 ~ 12h with ramp to 200 ~ 400 of 25 ~ 50 DEG C/min DEG C in nitrogen environment, pulverize, obtain attapulgite powder.
3. the preparation method of modified phosphate adsorbent as claimed in claim 2, is characterized in that the particle diameter of described powder is 40 ~ 200 orders.
4. the preparation method of modified phosphate adsorbent as claimed in claim 2, is characterized in that described potassium hydroxide solution concentration is 0.5mol/L.
5. the preparation method of modified phosphate adsorbent as claimed in claim 1, it is characterized in that described step 2 is: step one gained attapulgite powder is dropped into Muffle furnace 400 ~ 600 DEG C of high temperature sinterings, calcination time is 30 ~ 60min, the polymeric aluminum chlorides solution that 10 ~ 100mL concentration is 10 ~ 100mg/L is evenly sprayed immediately after taking-up, make attapulgite powder with spray polymeric aluminum chlorides solution mass volume ratio be 0.02 ~ 0.1g/ml, and calcination 3 ~ 12 hours again at 200 ~ 400 DEG C, obtain modified attapulgite powder end.
6. the preparation method of modified phosphate adsorbent as claimed in claim 5, is characterized in that the concentration of described polymeric aluminum chlorides solution is 50mg/L.
7. the preparation method of modified phosphate adsorbent as claimed in claim 1, is characterized in that described step 3 is: by the grinding of step 2 gained modified attapulgite powder end, obtain described modified phosphate adsorbent.
8. a modified phosphate adsorbent, is characterized in that utilizing the preparation method described in claim 1 to prepare.
9. the application of adsorbent as claimed in claim 8, is characterized in that utilizing it to remove phosphate in waste water.
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| CN113304728A (en) * | 2021-06-23 | 2021-08-27 | 四川农业大学 | Secondary modified carbon-based phosphorus adsorption composite material and preparation method and application thereof |
| CN114950346A (en) * | 2022-05-11 | 2022-08-30 | 内蒙古大学 | Efficient phosphorus removal agent prepared from natural calcium-rich mixed clay and preparation method thereof |
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