CN104624174A - Preparation method of water body low-concentration phosphorus compound adsorbent - Google Patents
Preparation method of water body low-concentration phosphorus compound adsorbent Download PDFInfo
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- CN104624174A CN104624174A CN201510043822.2A CN201510043822A CN104624174A CN 104624174 A CN104624174 A CN 104624174A CN 201510043822 A CN201510043822 A CN 201510043822A CN 104624174 A CN104624174 A CN 104624174A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/44—Materials comprising a mixture of organic materials
- B01J2220/445—Materials comprising a mixture of organic materials comprising a mixture of polymers
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Abstract
The invention discloses a preparation method of a water body low-concentration phosphorus compound adsorbent, and relates to a preparation method of an adsorbent which is used for treating low-concentration orthophosphate in a water body. The preparation method of the compound adsorbent comprises the following steps: I, dissolving La(NO3)3.6H2O into DMF, then adding polyacrylonitrile, heating to 50-100 DEG C, and then reacting for 1-10 hours to obtain a polymer solution; and II, performing electro-spinning on the polymer solution obtained in the step I, and cleaning an obtained electro-spinning film to obtain the water body low-concentration phosphorus compound adsorbent. The compound adsorbent prepared by using the method disclosed by the invention is an La(OH)3 nano-wire/polyacrylonitrile compound nano fiber, and a monodispersed La(OH)3 nano-rod is loaded on the PAN (polyacrylonitrile) nano fiber. The compound nano fiber adsorbent prepared by using the method disclosed by the invention can be used for performing effective adsorption aiming at low-concentration phosphorus in the water body, and ensures that the removal rate of phosphorus in water can reach more than 98%.
Description
Technical field
The present invention relates to a kind of preparation method being applied to the adsorbent of low concentration orthophosphates in process water body.
Background technology
Day by day serious current of body eutrophication, urgently to be resolved hurrilyly in water environment in China be not water resource type lack of water but water quality type lack of water, it is difficult problems that water industry needs to face that the eutrophication how controlling source water solves its a series of Water purification difficult problems brought as early as possible.
In water environment, the discharge beyond standards of P elements is one of major reason causing body eutrophication, phosphorus process is in the past first for the P elements in water body, reduce its concentration, but the phosphorus content in actual water body is usually not high, the main cause of actual body eutrophication is caused to be mostly the P elements release that bed mud adsorbs.The existing process about phosphorus in water, no matter the difficult problem being application coagulating sedimentation, absorption, ion-exchange or microorganism dephosphorization are all faced with low phosphorus control.Although for example in adsorption applications, adsorbent is of a great variety and have higher saturated extent of adsorption, the absorption for low phosphorus does not often reach desirable clearance; The secondary pollution that desorption problem after absorption also may cause phosphorus to discharge again.And fully contact with object for ensureing in the process of absorption, a large amount of adsorbent mostly is powder nanometer structure, although this kind of powder nanometer structure can improve saturated extent of adsorption and the rate of adsorption of adsorbent, its leak caused by secondary pollution problem must receive the concern of people.
Summary of the invention
The object of the invention is to solve the existing problem lower for the clearance of adsorbent to low phosphorus of phosphorus in process water, and a kind of preparation method of water body low phosphorus compound adsorbent is provided.
The preparation method of water body low phosphorus compound adsorbent of the present invention follows these steps to realize:
One, by La (NO
3)
36H
2o is dissolved in DMF (dimethyl formamide), then presses PAN and La (NO
3)
36H
2the mass ratio of O is that 10:1 ~ 1:1 adds PAN (polyacrylonitrile), reacts 1 ~ 10h, obtain the polymer solution of 5 ~ 12wt.%PAN content after being heated to 50 ~ 100 DEG C;
Two, Electrospun is carried out to the polymer solution that step one obtains, the electrospinning film obtained is collected on aluminium-foil paper, then electrospinning film is placed in alkali lye and soaks 10 ~ 16h, take out electrospinning film and re-use washed with de-ionized water to neutral post-drying, obtain water body low phosphorus compound adsorbent.
The water body low phosphorus compound adsorbent that the present invention prepares is La (OH)
3nano wire/polyacrylonitrile (PAN) composite nano fiber is macroscopically flaky texture, microcosmic is load has single dispersing La (OH)
3the multilevel hierarchy of the PAN nanofiber of nanometer rods.
Single dispersing La (OH) of the present invention
3nanometer rods is the core material of phosphorus absorption, due to the fixation of PAN nanofiber, and La (OH)
3be uniformly dispersed and be one-dimensional nano structure, the absorption for phosphorus provides the adsorption site position of mass efficient, and LaPO
4binding ability is excellent, there will not be secondary release And Spread of Solute.Compared to other phosphorus adsorbent, this La (OH)
3nano wire/polyacrylonitrile (PAN) composite nano fiber fully presents high efficiency and high clearance in the process of adsorbing for low phosphorus.Simultaneously due to the characteristic of PAN itself, this sorbing material also has good mechanics pliability, can shock resistance hydraulic load, and can stablely within the scope of soda acid widely use, widen the range of application of adsorbent, and this compound adsorbent has excellent liquid-solid separation characteristic, this La (OH) in a word
3nano wire/polyacrylonitrile (PAN) composite nano fiber adsorbent is a kind of excellent low phosphorus adsorbent having efficient nano adsorption capacity concurrently and stablize easily separated ability.As when phosphorus (P) concentration is 2mg/L in water body, add La of the present invention (OH) by the throwing amount of 1g/L
3nano wire/polyacrylonitrile composite nano fiber adsorbent, can make the clearance of phosphorus in water body reach more than 98%.
Accompanying drawing explanation
Fig. 1 is the macro morphology figure of the water body low phosphorus compound adsorbent that embodiment obtains;
Fig. 2 is the transmission electron microscope picture of the water body low phosphorus compound adsorbent that embodiment obtains;
Fig. 3 is the adsorption curve figure of water body low phosphorus Composite Adsorbent Absorbing low phosphorus (2mg/L) prepared by Application Example;
Fig. 4 is water body low phosphorus compound adsorbent phosphorus (50mg/L) adsorption curve figure under different pH prepared by Application Example;
Fig. 5 is water body low phosphorus compound adsorbent phosphorus absorption (50mg/L) column statistical chart under different competing ions prepared by Application Example, and wherein abscissa is different competing ions states, and ordinate is the adsorption capacity of phosphorus absorption under different ions.
Detailed description of the invention
Detailed description of the invention one: the preparation method of present embodiment water body low phosphorus compound adsorbent follows these steps to realize:
One, by La (NO
3)
36H
2o is dissolved in DMF (dimethyl formamide), then presses PAN and La (NO
3)
36H
2the mass ratio of O is that 10:1 ~ 1:1 adds PAN (polyacrylonitrile), reacts 1 ~ 10h, obtain the polymer solution of 5 ~ 12wt.%PAN content after being heated to 50 ~ 100 DEG C;
Two, Electrospun is carried out to the polymer solution that step one obtains, the electrospinning film obtained is collected on aluminium-foil paper, then electrospinning film is placed in alkali lye and soaks 10 ~ 16h, take out electrospinning film and re-use washed with de-ionized water to neutral post-drying, obtain water body low phosphorus compound adsorbent.
Present embodiment water body low phosphorus compound adsorbent uses PAN and La (NO
3)
36H
2o is raw material, and DMF is solvent, namely obtains composite nano fiber through Electrospun and original position basic treatment.Wherein La (OH)
3compare the Phosphate Adsorption material of other type various, with phosphate, there is better chemical affinity; PAN has good mechanical property on the other hand, ensures La (OH)
3nanometer rods stable dispersion simultaneously, maintains cardinal principle measure feature in processing procedure and stablizes.Do not detect the leakage of adsorbent in water quality after absorption, avoid the secondary pollution of water body.Apply simple method the adsorbent after absorption to be separated from water.
Present embodiment, in the process of configuration polymer spinning solution heating, ensure not contact with aqueous phase, otherwise electrospinning solute can be separated out.
Detailed description of the invention two: present embodiment and detailed description of the invention one are unlike pressing PAN and La (NO in step one
3)
36H
2the mass ratio of O is that 3:1 ~ 1:1 adds PAN.Other step and parameter identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two obtain the polymer solution of 5 ~ 8wt.%PAN content unlike step one.Other step and parameter identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three are sodium hydroxide solution, potassium hydroxide solution or ammoniacal liquor unlike the alkali lye described in step 2.Other step and parameter identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four are 1mol/L unlike the concentration of the alkali lye described in step 2.Other step and parameter identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five regulate spinning voltage to be 10kv unlike step 2, and humidity is less than 20%, accepting distance is 25cm.Other step and parameter identical with one of detailed description of the invention one to five.
Present embodiment needs controlled humidity lower than less than 20% in the process of electrospinning, otherwise Electrospun is not easily formed.
Embodiment: the preparation method of the present embodiment water body low phosphorus compound adsorbent follows these steps to realize:
One, by the La (NO of 1g
3)
36H
2o is dissolved in 20gDMF (dimethyl formamide), then presses PAN and La (NO
3)
36H
2the mass ratio of O is that 1:1 adds PAN (polyacrylonitrile), reacts 3h, obtain the polymer solution of 5wt.%PAN content after being heated to 60 DEG C;
Two, Electrospun is carried out to the polymer solution that step one obtains, adjustment spinning voltage is 10kv, humidity is 15%, accepting distance is 25cm, the electrospinning film obtained is collected on aluminium-foil paper, then electrospinning film is placed in potassium hydroxide solution and soaks 12h, take out electrospinning film and re-use washed with de-ionized water to neutral post-drying, obtain water body low phosphorus compound adsorbent.
Use the La (OH) that the present embodiment obtains
3nano wire/PAN composite nano fiber is tested, and COD, TN and P concentration in simulation water body is respectively 100mg/L, 10mg/L and 2mg/L, takes 0.05g compound adsorbent La (OH)
3nano wire/PAN composite nano fiber is fed into 50mL and simulates in water body, ensures adsorbent throwing amount 1g/L, after 1h absorption, measures its adsorption capacity, phosphorus eliminating rate of absorption.
After absorption 20min, in simulation water body, the clearance of phosphorus reaches 98.92%, and influent density is reduced to 22.15 μ g P/L, sufficiently lower phosphate concn in water body, decreases the possibility of body eutrophication.And illustrated by pH experiment and anion competing ions adsorption experiment, adsorbent all has good characterization of adsorption between pH 3 ~ 9, and competing ions (concentration is 0.01mol/L) is as F
-, Cl
-, SO
4 2-, CO
3 2-and NO
3 -on the absorption of phosphorus substantially without impact, illustrate that adsorbent has good selective.Illustrate that load has La (OH) according to pH and competing ions absorption experiment of single factor result
3the PAN nano wire of nanometer rods is a kind of scope of application comparatively wide (pH 3 ~ 9) and environmental friendliness adsorbent with strong points.
The exterior appearance figure of Fig. 1 shows this water body low phosphorus compound adsorbent and has lamellar structure, and after ensure that absorption, adsorbent is easily separated, and the transmission electron microscope picture of Fig. 2 can find out La (OH) in this compound adsorbent
3nanometer rods single dispersing, on polyacrylonitrile nanofiber, ensure that the adsorption activity of nanometer rods.The dynamics matched curve display compound adsorbent of Fig. 3 has the ability of efficient adsorption, and final tp removal rate, up to 98.97%, plays the ability of prevention body eutrophication, ensure that water quality.Can find out at different acid or alkali environment (pH 3 ~ 9) from Fig. 4 and Fig. 5 and exist the environment of competing ions, this water body low phosphorus compound adsorbent all has good adsorption capacity, illustrate that it is that a kind of stability is high, adaptability is excellent, the water systems'phosphorus sorbent material that specific aim is outstanding.
Claims (6)
1. a preparation method for water body low phosphorus compound adsorbent, it is characterized in that following these steps to realize:
One, by La (NO
3)
36H
2o is dissolved in DMF, then presses PAN and La (NO
3)
36H
2the mass ratio of O is that 10:1 ~ 1:1 adds PAN, reacts 1 ~ 10h, obtain the polymer solution of 5 ~ 12wt.%PAN content after being heated to 50 ~ 100 DEG C;
Two, Electrospun is carried out to the polymer solution that step one obtains, the electrospinning film obtained is collected on aluminium-foil paper, then electrospinning film is placed in alkali lye and soaks 10 ~ 16h, take out electrospinning film and re-use washed with de-ionized water to neutral post-drying, obtain water body low phosphorus compound adsorbent.
2. the preparation method of a kind of water body low phosphorus compound adsorbent according to claim 1, is characterized in that in step one by PAN and La (NO
3)
36H
2the mass ratio of O is that 3:1 ~ 1:1 adds PAN.
3. the preparation method of a kind of water body low phosphorus compound adsorbent according to claim 1, is characterized in that step one obtains the polymer solution of 5 ~ 8wt.%PAN content.
4. the preparation method of a kind of water body low phosphorus compound adsorbent according to claim 1, is characterized in that the alkali lye described in step 2 is sodium hydroxide solution, potassium hydroxide solution or ammoniacal liquor.
5. the preparation method of a kind of water body low phosphorus compound adsorbent according to claim 1, is characterized in that the concentration of the alkali lye described in step 2 is 1mol/L.
6. the preparation method of a kind of water body low phosphorus compound adsorbent according to claim 1, it is characterized in that step 2 regulates spinning voltage to be 10kv, humidity is less than 20%, and accepting distance is 25cm.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105289521A (en) * | 2015-10-30 | 2016-02-03 | 无锡市新都环保科技有限公司 | Preparation method of surface modified pine needle loaded lanthanum hydroxide phosphorus adsorbent |
| CN105617990A (en) * | 2016-02-25 | 2016-06-01 | 哈尔滨工业大学 | Adsorbent for simultaneously strengthening removal of trace phosphorus and organic matter and preparation method thereof |
| CN106311170A (en) * | 2016-08-30 | 2017-01-11 | 中山朗清膜业有限公司 | Hollow porous adsorption material for removing inorganic phosphorus and preparation method thereof |
| CN107413303A (en) * | 2016-05-24 | 2017-12-01 | 上海新昇半导体科技有限公司 | A kind of sorbing material, adsorbent equipment and preparation method |
| CN109317123A (en) * | 2018-12-03 | 2019-02-12 | 同济大学 | A kind of phosphorus high throughput absorption nano fibrous membrane and preparation method thereof |
| CN109499552A (en) * | 2018-12-20 | 2019-03-22 | 天津科技大学 | A kind of Novel dephosphorization bacteriostatic PP filter core and preparation method thereof |
| CN111558367A (en) * | 2020-05-25 | 2020-08-21 | 广东维清环境工程有限公司 | Preparation method of hollow fiber composite filtering adsorption dephosphorization material |
| CN111871389A (en) * | 2020-08-06 | 2020-11-03 | 哈尔滨工业大学 | Preparation method of lanthanum hydroxide modified aerogel phosphorus removal adsorbent |
| CN112675804A (en) * | 2020-12-02 | 2021-04-20 | 哈尔滨工业大学 | Hydrated cerium carbonate phosphorus removal adsorbent and preparation method and application thereof |
| CN114950571A (en) * | 2022-04-21 | 2022-08-30 | 天津大学 | Photocatalytic spinning membrane material and preparation method and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105289521A (en) * | 2015-10-30 | 2016-02-03 | 无锡市新都环保科技有限公司 | Preparation method of surface modified pine needle loaded lanthanum hydroxide phosphorus adsorbent |
| CN105289521B (en) * | 2015-10-30 | 2019-03-22 | 无锡市新都环保科技有限公司 | The preparation method of the modified pine needle load lanthanum hydroxide dephosphorization adsorbent in surface |
| CN105617990A (en) * | 2016-02-25 | 2016-06-01 | 哈尔滨工业大学 | Adsorbent for simultaneously strengthening removal of trace phosphorus and organic matter and preparation method thereof |
| CN107413303A (en) * | 2016-05-24 | 2017-12-01 | 上海新昇半导体科技有限公司 | A kind of sorbing material, adsorbent equipment and preparation method |
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| CN106311170B (en) * | 2016-08-30 | 2019-12-13 | 中山朗清膜业有限公司 | Hollow porous adsorption material for removing inorganic phosphorus and preparation method thereof |
| CN109317123A (en) * | 2018-12-03 | 2019-02-12 | 同济大学 | A kind of phosphorus high throughput absorption nano fibrous membrane and preparation method thereof |
| CN109317123B (en) * | 2018-12-03 | 2020-04-17 | 同济大学 | Phosphorus high-flux adsorption nanofiber membrane and preparation method thereof |
| CN109499552A (en) * | 2018-12-20 | 2019-03-22 | 天津科技大学 | A kind of Novel dephosphorization bacteriostatic PP filter core and preparation method thereof |
| CN111558367A (en) * | 2020-05-25 | 2020-08-21 | 广东维清环境工程有限公司 | Preparation method of hollow fiber composite filtering adsorption dephosphorization material |
| CN111871389A (en) * | 2020-08-06 | 2020-11-03 | 哈尔滨工业大学 | Preparation method of lanthanum hydroxide modified aerogel phosphorus removal adsorbent |
| CN112675804A (en) * | 2020-12-02 | 2021-04-20 | 哈尔滨工业大学 | Hydrated cerium carbonate phosphorus removal adsorbent and preparation method and application thereof |
| CN114950571A (en) * | 2022-04-21 | 2022-08-30 | 天津大学 | Photocatalytic spinning membrane material and preparation method and application thereof |
| CN114950571B (en) * | 2022-04-21 | 2023-12-05 | 天津大学 | Photocatalytic spinning film material and preparation method and application thereof |
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