CN107159154B - It is a kind of using luffa as dephosphorization adsorbent of host material and preparation method thereof - Google Patents
It is a kind of using luffa as dephosphorization adsorbent of host material and preparation method thereof Download PDFInfo
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- CN107159154B CN107159154B CN201710651590.8A CN201710651590A CN107159154B CN 107159154 B CN107159154 B CN 107159154B CN 201710651590 A CN201710651590 A CN 201710651590A CN 107159154 B CN107159154 B CN 107159154B
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- luffa
- dephosphorization adsorbent
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
Abstract
The present invention provides a kind of using luffa as dephosphorization adsorbent of host material and preparation method thereof comprising following steps: taking Loofah powder, is 1:(1.5~3 by solid-liquid ratio) 1~3% MgCl is added2Solution activates 3~5 minutes in supersonic wave cleaning machine, takes out filtering and drains, is prepared into luffa wet slag;In the solution of 0.2~0.5% lauryl sodium sulfate, Na is added2WO4·2H2O and La (NO3)3·6H2Two kinds of solids of O adjust pH to 7 ~ 9 after completely dissolution, are prepared into tungsten-lanthanum ion precursor liquid;Into tungsten-lanthanum ion precursor liquid of S3, pretreated Loofah powder is added, stirs 12~24 h at room temperature, filtering is drained, filter residue is dry under the conditions of 50~80 DEG C, obtained dephosphorization adsorbent finished product;The method of the present invention is simple, and the removal rate of phosphorus is high, adsorption capacity is big is had a wide range of applications in the improvement of eutrophic lake and phosphorus-containing wastewater.
Description
Technical field
The invention belongs to environmental protection technical fields, and in particular to a kind of using luffa as the dephosphorization adsorbent of host material
And preparation method thereof, and for the phosphorus in Adsorption water body in lake.
Background technique
It is a large amount of dirty in industrial and agricultural production due to the fast development of continuous expansion, the growth of population and economy of city size
Water waste water is discharged to lake, and the waste water containing two element of P and N causes the eutrophication problem in Lake Water more and more serious, makes
At the mass propagation of algae.The excessively high of wherein phosphorus content is one of the main reason for causing lake eutrophication to endanger, constantly
The P elements of accumulation eventually result in lake blue algae and spread unchecked, and water quality degenerates smelly, seriously affect daily life.Phosphorus is usual
With PO4 3-、HPO4 2-Form be present in water body, be the control sex factor of water eutrophication.Prevent the growth of lake blue algae
Key is the load of P, N of reduction water body in lake, and the technological approaches for cutting down water body in lake P and N at present (is cut in addition to eliminating point source
Flow pollution sources), reduce and this kind of most basic approach of Control the Plan Pollution Sources outside, the most common method has mechanical dredging method, diversion
Douche, biological restoration, chemiadsorption etc., these methods are to effectively prevent the important channel of water eutrophication.Chemistry
Absorption method is the content for preparing various dephosphorization adsorbents to reduce phosphorus in water, the dephosphorization prepared with agricultural and sideline product biolobic material material
Adsorbent is at low cost, from a wealth of sources, preparation method is simple, adsorption effect is good and the extensive concern by environmentalist.
Currently, patent disclosed in preparation dephosphorization chemosorbent has natural minerals adsorbent, such as patent publication No.
200910223947.8 disclosing the method for zeolite and vermiculite Phosphate Sorption, patent publication No. 201210253526.1 utilizes magnesite
Recycling phosphorus, patent publication No. 201010594623.8 disclose the adsorptivity of the natural minerals confrontation phosphorus such as iron sulphur mine and flyash
Can, find that these materials are relatively low to the adsorption capacity of phosphorus by practical application.In order to improve phosphor-removing effect, patent publication No.
200910186048.5 preparation methods for having disclosed hydrous zirconia gel a kind of and the absorption to phosphorus, but this powdered absorption
Agent, it is difficult to directly apply to water treatment procedure, therefore not be used widely;Therefore, high adsorption capacity, easy to use is prepared
Dephosphorization adsorbent it is necessary.
Luffa is the natural vascular bundle that mature sponge gourd fruit removes the cellulosic reticular structure obtained after crust and seed
Tissue, is mainly made of cellulose, hemicellulose and lignin, content of cellulose is up to 60%.In loofah fiber tube bank
It is dispersed with a large amount of hole, there is very big specific surface area, in addition also there is unique absorption property and hydrophilic, oleophylic and again
Raw recycling characteristic, can show special physical property.The empiric observation to work from wastewater treatment, luffa pass through powder
Broken processing, specific surface area increase can be used as the carriers of some chemisorbed materials, as high activity lanthanum hydroxide (zirconium, aluminium, iron,
Magnesium) pass through precipitation reaction appendix on its surface, these hydroxide can be significantly improved to the adsorbance of phosphorus and convenient for collecting again
It is raw, a kind of new adsorbent material is provided for the water body treating of eutrophication.
Summary of the invention
It in view of the problems of the existing technology, will it is an object of the invention to design using luffa as host material
La(III) and W(VI) hydroxide of salt is supported on its surface, has prepared a kind of efficiently except dephosphorization (PO4 3-) composite adsorption
Agent.The method of the present invention is simple, adsorption capacity is big, adsorption rate is high, can large-scale production, the product of preparation is more conducive to adsorb lake
Or the phosphorus in water body.
Specifically, the present invention provides a kind of using luffa as dephosphorization adsorbent of host material and preparation method thereof, packet
Include following steps:.
S1, it prepares Loofah powder: collecting luffa, cleaned with tap water, 60~120 mesh are crushed to after drying, obtain sponge gourd
Network powder.
S2, Loofah powder pretreatment: being 1:(1.5~3 by solid-liquid ratio in the Loofah powder that S1 is obtained) quality is added
The MgCl that score is 1~3%2Solution after stirring and evenly mixing, places 3~5 h, obtains mixed liquor;It is clear that mixed liquor is placed on ultrasonic wave
It is activated 3~5 minutes in washing machine in 30~50 DEG C, after taking-up wash with distilled water repeatedly, filtering is drained, and pretreated sponge gourd is obtained
Network powder.
S3, prepare tungsten-lanthanum ion precursor liquid: lauryl sodium sulfate being taken to be dissolved with water, be prepared into 0.1~0.5% it is molten
A certain amount of Na is added in liquid under magnetic stirring2WO4·2H2O and La (NO3)3·6H2Two kinds of solids of O, and pH to 7~9 is adjusted,
It is prepared into tungsten-lanthanum ion precursor liquid.
S4, into tungsten-lanthanum ion precursor liquid of S3, be added S2 obtained in pre-process Loofah powder, be stirred at room temperature
12~24 h;Filtering is drained, and filter residue is washed with water to neutrality, obtained dephosphorization adsorbent;It is dry under the conditions of 50~80 DEG C,
Load tungsten-lanthanum luffa dephosphorization adsorbent finished product is made.
S5, adsorption experiment: the phosphorus standard solution (preparing with potassium dihydrogen phosphate) of 50 mg/L is drawn, respectively with 0.12
mol·L-1 HCl and 0.25 molL-1NaOH solution adjusts pH value to 1~7, is settled to 100 mL, 0.25~0.5 g is added
The dephosphorization adsorbent prepared vibrates 0.5~2.5 h on constant temperature oscillator with 180 r/min, filtrate is collected by filtration, uses phosphorus
Molybdenum blue method measures the content of phosphoric residue in filtrate, and dephosphorization adsorbent contains phosphorus in solution when acquiring adsorption equilibrium according to formula (1)
Amount adsorption rate (ƞ, %), it can determine optimal pH adsorption range accordingly.
Absorption dephosphorization adsorbent unit adsorbance when reaching balance (q, mg/g) and it is calculated according to formula (2).
In above-mentioned formula (1) and (2)Q 1For the initial mass (mg) for adsorbing phosphorus in preceding solution;Q 2For the phosphorus after adsorption equilibrium
Balance quality (mg);M is the quality (g) of luffa compound adsorbent.
Preferably, the fineness that luffa crushes in S1 is 80 mesh.
Preferably, be 1 by solid-liquid ratio in S2: the MgCl that mass fraction is 2% is added in (1.5~3)2It is molten be stirred it is mixed
After conjunction, 3~5 h are placed.
Preferably, in S2 mixed liquor be placed in supersonic wave cleaning machine in 30~50 DEG C activate 3~5 minutes.
Preferably, the mass concentration of lauryl sodium sulfate is 0.25% in S3.
Preferably, Na in S32WO4·2H2The additional amount of O is 0.5~2 g, La (NO3)3·6H2O additional amount is 1~5 g.
Preferably, 0.25 molL is utilized in S3-1NaOH solution pH value is adjusted.
Preferably, mixing time is 24 hours in S4, and drying temperature is 80 DEG C.
Preferably, the optimal pH range of dephosphorization compound adsorbent Phosphate Sorption is 2.5~6 in S5.
The present invention by La(III) and W(VI), prepared a kind of high on the surface of Loofah powder by the hydroxide appendix of salt
Effect removes dephosphorization (PO4 3-) compound adsorbent.The method of the present invention is simple, and adsorption capacity is big, adsorption rate is high, can large-scale production,
The product of preparation is more conducive to adsorb the phosphorus in lake or water, before having a wide range of applications in eutrophic lake and wastewater treatment
Scape.
Detailed description of the invention
Fig. 1: a kind of using luffa as the production procedure of the dephosphorization adsorbent of host material and preparation method thereof.
Fig. 2: the dephosphorization adsorbent influence of solution ph to adsorption rate in adsorption process.
Fig. 3: XRD curve graph of the dephosphorization adsorbent product of this patent preparation before and after absorption, a. dephosphorization adsorbent powder
XRD curve before absorption, the XRD curve after b. dephosphorization adsorbent Phosphate Sorption.
Specific embodiment
With reference to the accompanying drawing and specific embodiment is further explained structure and working principle of the invention:.
As shown in Fig. 1, the present invention provide it is a kind of using luffa as dephosphorization adsorbent of host material and preparation method thereof,
Itself the following steps are included:.
S1, it prepares Loofah powder: collecting mature luffa in autumn, cleaned with tap water, it is crushed to 60 after drying~
120 mesh, obtain Loofah powder.
S2, Loofah powder pretreatment: in the Loofah powder that S1 is obtained, be 1 by solid-liquid ratio: quality is added in (1.5~3)
The MgCl that score is 1~3%2Solution after stirring and evenly mixing, after placing 3~5 h, obtains mixed liquor;Mixed liquor is placed on ultrasound
It is activated 3~5 minutes in wave cleaning machine in 30~50 DEG C;Filtering drains, is multiple wash with distilled water, and filtering is put into burning after draining
It is spare in cup, obtain pretreated Loofah powder.
S3, prepare tungsten-lanthanum ion precursor liquid: lauryl sodium sulfate being taken to be dissolved with water, be prepared into 0.2~0.5% it is molten
A certain amount of Na is added in liquid under magnetic stirring2WO4·2H2O and La (NO3)3·6H2Two kinds of solids of O, and adjust pH to 9 ~
10, it is prepared into tungsten-lanthanum ion precursor liquid.
S4: it into tungsten-lanthanum ion precursor liquid of S3, is added obtained in S2 and pre-processes Loofah powder, be stirred at room temperature
12~24 h;It filtering, is washed to distillation close to neutrality, obtained composite dephosphorization adsorbent is dry under the conditions of 50~80 DEG C,
The dephosphorization compound adsorbent finished product of luffa appendix tungsten-lanthanum is made.
In order to determine that compound adsorbent to the optimum condition of Phosphorus From Wastewater, first carries out series of influence factors with simulated wastewater
Adsorption test.Use KH2PO4Phosphorous simulated wastewater is configured, composite dephosphorization adsorbent is mixed with simulated wastewater, is packed into conical flask
In, it is vibrated in constant temperature oscillator, is sufficiently mixed reaction, take supernatant through centrifuge separation after reaction, be divided light using P-Mo blue
Degree method measures the concentration of phosphoric residue in filtrate.Initial concentration and residual concentration are compared, it can be learnt that dephosphorization adsorbent is in waste water
The absorption properties such as removal rate, the adsorption capacity of phosphor contaminant.
Embodiment 1:.
In 100 mL, 2% MgCl2In solution, the Loofah powder of 15 gram of 80 mesh is added, after placing 5 h after mixing evenly;
It is placed in supersonic wave cleaning machine and is activated 4 minutes in 40 DEG C, take out filtering and drain, is multiple wash with distilled water, obtain pretreated silk
Melon network powder.
Under magnetic stirring, in the solution of 0.5% lauryl sodium sulfate, 1 gram of Na is added2WO4·2H2O and 5 gram of La
(NO3)3·6H2Two kinds of solid stirring and dissolvings of O, with 0.25 molL-1NaOH solution adjust pH to 8, be prepared into tungsten-lanthanum ion
Precursor liquid;It is added into above-mentioned tungsten-lanthanum ion precursor liquid obtained in S2 and pre-processes Loofah powder, 15 h are stirred at room temperature;
Filtering is drained, and is washed to distillation close to neutrality, and obtained composite dephosphorization adsorbent is dry under the conditions of 60 DEG C, and sponge gourd is made
Network appendix tungsten-lanthanum dephosphorization compound adsorbent finished product.
Embodiment 2:.
In 100 mL, 1% MgCl2In solution, the Loofah powder of 20 gram of 80 mesh is added, after placing 3 h after mixing evenly;
Mixed liquor is placed in supersonic wave cleaning machine and is activated 3 minutes in 50 DEG C, pretreated Loofah powder is obtained, transfers them to
In the solution of 0.4% lauryl sodium sulfate, 2 grams of Na are added under magnetic stirring2WO4·2H2O and 1 gram of La (NO3)3·6H2O two
Kind solid, sufficiently dissolution, with 0.25 molL-1NaOH solution adjust pH to 7.5,24 h are stirred at room temperature;Filtering is taken out
It is dry, it is washed to distillation close to neutrality, obtained composite dephosphorization adsorbent is dry under the conditions of 80 DEG C, and luffa appendix is made
Tungsten-lanthanum dephosphorization compound adsorbent finished product.
Embodiment 3:.
In 100 mL, 3% MgCl2In solution, the Loofah powder of 30 gram of 80 mesh is added, after placing 4 h after mixing evenly;It sets
In microwave activates 5 minutes in the micro-wave oven of 700 W, under moderate heat state;It takes out filtering drain, is multiple wash with distilled water, obtain
Pretreated Loofah powder;The solution of 0.5% lauryl sodium sulfate is added into this pretreated Loofah powder, and in magnetic force
It is added with stirring 5 grams of La (NO3)3·6H2O and 1 gram of Na2WO4·2H2Two kinds of solids of O, after completely dissolution with 0.25 molL-1's
NaOH solution adjusts pH to 9, and 12 h are stirred at room temperature;Filtering is drained, and is washed to distillation close to neutrality, what is obtained is compound
Dephosphorization adsorbent is dry under the conditions of 70 DEG C, and the dephosphorization compound adsorbent finished product of luffa appendix tungsten-lanthanum is made.
Application examples 1:.
It is 50 mg/L that the dephosphorization adsorbent prepared in Example 1, which is added to phosphorus content in the ratio of 0.4 g/100 mL,
Waste water in, pH value of solution is about 3;It is placed in constant temperature oscillator, is 25 DEG C, 200 r/min of hunting speed in temperature, when oscillation
Between under conditions of 2.5 hours carry out adsorption equilibrium experiment, oscillation finish centrifuge separation, with P-Mo blue spectrophotometry measurement supernatant
Phosphorus concentration in liquid;The results show that phosphor contaminant in waste water by refuse removal rate is up to 96.7%, saturated extent of adsorption is 31.7 mg/g.
Application examples 2:.
It is 40 mg/L solution containing phosphates in 100 mL concentration, adds dephosphorization adsorbent 0.30 g prepared in embodiment 2, it is molten
Liquid pH is about 5 conical flask to be put into constant temperature oscillator, and speed is 120 revs/min, temperature is 35 DEG C, is vibrated 60 minutes
Afterwards, the concentration for filtering, taking phosphoric residue in clear liquid P-Mo blue spectrophotometry measurement filtrate, obtains dephosphorization according to formula (1) and inhales
Attached dose of adsorption rate is 87%, and saturated extent of adsorption is 28.38 mg/g.
Application examples 3:
It is 20 mg/L that the dephosphorization adsorbent prepared in Example 3, which is added to phosphorus content in the ratio of 0.2 g/100 mL,
Waste water in, pH value of solution is about 4, is placed in constant temperature oscillator, is 30 DEG C, 150 r/min of hunting speed in temperature, when oscillation
Between 1.5 hours conditions carry out adsorption equilibrium experiment, oscillation is finished and is centrifuged, in the measurement of P-Mo blue spectrophotometry
Phosphorus concentration in clear liquid;The results show that phosphor contaminant in waste water by refuse removal rate is up to 92.6%, saturated extent of adsorption is 32.91 mg/g.
Effect example.
As Fig. 1 be according to the present invention provided by dephosphorization adsorbent obtained in preparation method, pH value in practical applications
Relationship between adsorption rate, as can be seen from the figure the optimal pH range of Phosphate Sorption solution medium is 2.5~6.
As Fig. 2 be according to the present invention provided by the obtained dephosphorization adsorbent product of preparation method, consolidating before and after absorption
The XRD change curve of body powder.After the dephosphorization adsorbent Phosphate Sorption known in XRD diagram, 10~50 (o) between there is phosphorus
The characteristic diffraction peak of compound is this explanation due to the tungsten in phosphorus and adsorbent and caused by lanthanum forms phosphotungstic acid class compound
The product of this patent preparation has specific adsorptivity to phosphorus.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of using luffa as the preparation method of the dephosphorization adsorbent of host material, it is characterised in that: the following steps are included:
S1, it prepares Loofah powder: the mature luffa that autumn collects being cleaned with tap water, 60~120 mesh are crushed to after drying,
Obtain Loofah powder;
The pretreatment of S2, Loofah powder: in the Loofah powder that S1 is obtained, by quality gram: the solid-liquid ratio of volume milliliter is 1:
(1.5~3) it is 1~3% MgCl that mass concentration, which is added,2Solution, stir 3~5 h after;It is then placed within supersonic wave cleaning machine
In activated 3~5 minutes at 30~50 DEG C;After taking-up wash with distilled water repeatedly, filtering is drained, pretreated luffa
Powder;
S3, it prepares tungsten-lanthanum ion precursor liquid: lauryl sodium sulfate being taken to be dissolved with water, being prepared into mass concentration is 0.2~0.5%
Solution, under magnetic stirring be added 0.5~2g Na2WO4·2H2La (the NO of O and 1~5 g3)3·6H2Two kinds of solids of O,
PH to 7~9 is adjusted after completely dissolution, is prepared into tungsten-lanthanum ion precursor liquid;
S4: into tungsten-lanthanum ion precursor liquid of S3, being added obtained in S2 and pre-process Loofah powder, it is stirred at room temperature 12~
24 h;It filters, product is washed with water, obtained dephosphorization adsorbent is dry under the conditions of 50~80 DEG C, and load tungsten-lanthanum silk is made
The dephosphorization adsorbent finished product of melon network.
2. according to claim 1 a kind of using luffa as the preparation method of the dephosphorization adsorbent of host material, feature
Be: the support materials for preparing dephosphorization adsorbent are luffa biological material, and the fineness of Loofah powder is 80 mesh.
3. according to claim 1 a kind of using luffa as the preparation method of the dephosphorization adsorbent of host material, feature
Be: luffa and mass concentration are 2%MgCl in S22Solution is by quality gram: the solid-liquid ratio of volume milliliter is located in advance for 1: 2
Reason places 5 h.
4. according to claim 3 a kind of using luffa as the preparation method of the dephosphorization adsorbent of host material, feature
Be: Loofah powder and mass concentration are 2% MgCl in S22Mixed solution be placed in supersonic wave cleaning machine in 30~50 DEG C
Activation 4 minutes.
5. according to claim 1 a kind of using luffa as the preparation method of the dephosphorization adsorbent of host material, feature
Be: the mass concentration of lauryl sodium sulfate is 0.25% in S3.
6. according to claim 1 a kind of using luffa as the preparation method of the dephosphorization adsorbent of host material, feature
Be: mixing time is 24 hours in S4, and drying temperature is 80 DEG C.
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