CN108816199A - A kind of AlFu@PS compound adsorbent and preparation method thereof - Google Patents

A kind of AlFu@PS compound adsorbent and preparation method thereof Download PDF

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Publication number
CN108816199A
CN108816199A CN201810588202.0A CN201810588202A CN108816199A CN 108816199 A CN108816199 A CN 108816199A CN 201810588202 A CN201810588202 A CN 201810588202A CN 108816199 A CN108816199 A CN 108816199A
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alfu
solution
preparation
compound adsorbent
water
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CN108816199B (en
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王治科
张柏爽
朱韵怡
王全坤
叶存玲
范顺利
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Henan Normal University
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Henan Normal University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/261Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid 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 form
    • B01J20/28016Particle form
    • B01J20/28021Hollow particles, e.g. hollow spheres, microspheres or cenospheres
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/288Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/105Phosphorus compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention discloses a kind of AlFu@PS compound adsorbent and preparation method thereof, the preparation process of the compound adsorbent is to prepare AlFu by the way that the alkaline solution of fumaric acid to be added drop-wise in aluminum sulfate solution first.Dry AlFu is distributed in the N-Methyl pyrrolidone solution of polystyrene followed by closed container, which must carry out under the conditions of closing is dry anhydrous.Finally above-mentioned solution is instilled in a large amount of water, prepares AlFu@PS microballoon.Preparation process of the present invention is simple, condition is controllable and easy to operate, and the AlFu@PS microballoon of preparation is easily isolated and recycled, has higher Adsorption ability to phosphate radical in water.

Description

A kind of AlFu@PS compound adsorbent and preparation method thereof
Technical field
The invention belongs to the preparation technical fields of phosphorus-containing wastewater adsorbent, and in particular to a kind of AlFu@PS compound adsorbent And preparation method thereof.
Background technique
Eutrophication is a problem more outstanding in current water pollution phenomenon, this is because nitrogenous, two kinds of elements of phosphorus Related compound is largely flowed into the slow flow water bodies such as lake, river, bay, causes algae and planktonic organism rapidly to breed, water body Dissolved oxygen content reduces, water quality deterioration, fish and other biological mortality.It is effectively slow in order to rationally utilize and water conservation The problem for solving water resource insufficient supply, needs the phosphorus in water removal, and the method for dephosphorization mainly has absorption method, bioanalysis, chemistry heavy Shallow lake method etc..Absorption method is required at low cost because easy to operate, high-efficient and become one of most efficient method.
Metal organic frame (MOFs) is a kind of novel crystalline porous material, by metal cation, metal cluster with it is organic Molecule is formed by connecting by coordinate bond, provides the periodic network frame with the aperture and chemical structure easily adjusted.Metal has Machine skeleton has the lot of advantages such as very high surface area, high porosity, not only gas absorption and gas storage, chemical sensitisation and The multiple fields such as catalysis have certain application, also have certain application prospect in terms of water process as adsorbent.But due to gold Belong to organic framework material crystal grain it is small, be not readily separated and mostly powder the disadvantages of, and metal organic framework be easy hydrolysis, Still centainly limited to using upper.
Summary of the invention
The present invention is to solve the above problems, provide a kind of AlFu@PS compound adsorbent and preparation method thereof.
To achieve the above object, the technical solution adopted by the present invention is that, a kind of preparation side of AlFu@PS compound adsorbent Method includes the following steps:
(1)The synthesis of AlFu:
By the Al of 18.55g2(SO4)3·18H2O is dissolved in 79.5ml deionized water, about hour of 60 DEG C of heating stirrings, is obtained To solution A;The sodium hydroxide and 6.45g fumaric acid for weighing 4.75g again are added in 95.5ml deionized water, with glass bar by its Stirring obtains solution B to being completely dissolved;It is added dropwise in solution A with rubber head dropper draw solution B, is being turned when being added dropwise with magneton About 15-20r/min of speed are mixed slowly, and are added dropwise within about 2 hours, generate milky suspension, be centrifuged, wash and 100 DEG C are dried in vacuo 24 hours, and obtained solid is denoted as AlFu;
(2)The preparation of AlFu@PS compound adsorbent:
Take 1g polystyrene(PS)It is added in dry N-Methyl pyrrolidone solution, stirring makes it completely in closed container Dissolution, obtains solution C;2g dry AlFu is added in solution C, is sufficiently stirred, the above process must be in the anhydrous item of drying It is carried out under part, above-mentioned solution is instilled in a large amount of water with dropper later, AlFu PS microballoon is generated, stands overnight, and use deionization Water washing 3 times, ten minutes are stood every time, 100 DEG C of microballoon drying 24 hours obtained is to get AlFu PS compound adsorbent.
The beneficial effect comprise that:Preparation process of the present invention is simple, condition is controllable and easy to operate, preparation AlFu@PS microballoon, is easily isolated and recycled, and has higher Adsorption ability to phosphate radical in water.
Detailed description of the invention
Fig. 1 is the XRD diagram of AlFu and AlFu@PS;
Fig. 2 is PS, the infrared spectrum of AlFu and AlFu@PS;
Fig. 3 is influence of the different adsorption times to absorption property;
Fig. 4 is influence of the AlFu@PS dosage to absorption property;
Fig. 5 is influence of the phosphate radical initial concentration to absorption property;
Fig. 6 is influence of the simulated water sample to absorption property.
Specific embodiment
The preparation of compound adsorbent
The preparation of AlFu@PS includes two steps:
(1)The synthesis of AlFu
By the Al of 18.55g2(SO4)3·18H2O is dissolved in 79.5ml deionized water, about hour of 60 DEG C of heating stirrings, is obtained To solution(A).The sodium hydroxide and 6.45g fumaric acid for weighing 4.75g again are added in 95.5ml deionized water, will with glass bar It is stirred to being completely dissolved, and obtains solution(B).With rubber head dropper draw solution(B)It is added dropwise to solution(A)In, it is used when being added dropwise Magneton is mixed slowly in about 15-20r/min of revolving speed, is added dropwise within about 2 hours, and milky suspension is generated.Be centrifuged, It washs and is dried in vacuo 24 hours at 100 DEG C.Later, the white solid of drying is ground and white powder is made, be denoted as AlFu, filled Enter in vacuum plastic bag and saves, it is spare.
(2)The preparation of AlFu@PS compound adsorbent
Take 1g polystyrene(PS)It is added in dry N-Methyl pyrrolidone solution, stirring makes it completely in closed container Dissolution, obtains solution(C).2g dry AlFu is added in solution C, is sufficiently stirred, the above process must be anhydrous in drying Under the conditions of carry out.Above-mentioned solution is instilled in a large amount of water with dropper later, AlFu@PS microballoon is generated, stands overnight, and spend from Sub- water washing 3 times stands ten minutes every time.100 DEG C of microballoon drying 24 hours obtained, is fitted into vacuum bag and saves, spare.
Characterization
Fig. 1 is the XRD diagram of AlFu and AlFu@PS.As shown in Figure 1, AlFu@PS compound adsorbent remains the characteristic peak of AlFu.
Fig. 2 is the infrared spectrum of PS, AlFu and AlFu@PS.As seen from the figure, it is clearly observed in the infrared spectrum of AlFu@PS The characteristic absorption peak of AlFu has been arrived, also observed the characteristic absorption peak of PS.
Absorption property
The influence of Fig. 3 adsorption time.AlFu@PS dosage is 150mg, and phosphate concentration is respectively 10,20,30mg/L, temperature 25 DEG C, hunting speed 150r/min.When adsorption time reaches 48h, the adsorption rate of phosphate radical is 90% or more.
Fig. 4 is the influence of dosage.The AlFu@PS of 30,60,90,120,150,180,210mg, phosphate radical are weighed respectively Concentration is 10mg/L, and 25 DEG C of temperature, hunting speed 150r/min vibrate 18h.When dosage is 210mg, adsorption rate is up to 87.3%。
Fig. 5 is the influence of phosphate radical initial concentration.By the AlFu@PS of 150mg be added to concentration be respectively 10,20,30, 40, in the phosphate radical solution of 50mg/L, 25 DEG C of temperature, hunting speed 150r/min vibrate 18h.It follows that AlFu@PS is suitable For low phosphorus acid group wastewater treatment.
Fig. 6 is the influence of simulated water sample.150mgAlFu@PS is added in six kinds of different water samples, phosphate concentration is 10mg/L, 25 DEG C of temperature, hunting speed 150r/min vibrate 18h.For different water samples, the adsorption rate of phosphate radical is all 77% More than.

Claims (2)

1. a kind of preparation method of AlFu@PS compound adsorbent, which is characterized in that include the following steps:
(1)The synthesis of AlFu:
By the Al of 18.55g2(SO4)3·18H2O is dissolved in 79.5ml deionized water, one hour of 60 DEG C of heating stirrings, is obtained Solution A;The sodium hydroxide and 6.45g fumaric acid for weighing 4.75g again are added in 95.5ml deionized water, are stirred to completely molten Solution, obtains solution B;Solution B is added dropwise in solution A, is stirred when being added dropwise, milky suspension is generated, be centrifuged, It washs and is dried in vacuo 24 hours at 100 DEG C, obtained solid is denoted as AlFu;
(2)The preparation of AlFu@PS compound adsorbent:
1g polystyrene is taken to be added in dry N-Methyl pyrrolidone solution, stirring keeps it completely molten in closed container Solution, obtains solution C;2g AlFu is added in solution C, is sufficiently stirred, later instills acquired solution in water, generates AlFu@PS Microballoon is stood overnight, and is washed with deionized 3 times, and 100 DEG C of microballoon drying 24 hours obtained is to get the compound suction of AlFu@PS Attached dose.
2. the AlFu@PS compound adsorbent that method as claimed in claim 1 is prepared.
CN201810588202.0A 2018-06-08 2018-06-08 AlFu @ PS composite adsorbent and preparation method thereof Expired - Fee Related CN108816199B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104069831A (en) * 2014-07-24 2014-10-01 中国地质大学(北京) Efficient nitrate-removing granular absorbent and preparation method thereof
CN105664884A (en) * 2016-03-29 2016-06-15 中国地质大学(北京) Magnetic adsorbent for removing heavy metal in water and method for preparing magnetic adsorbent
CN107081138A (en) * 2017-05-19 2017-08-22 上海工程技术大学 Magnetic polystyrene base enclosure glycan composite adsorbent and preparation method and application
CN107376863A (en) * 2017-08-30 2017-11-24 河南师范大学 A kind of preparation method of AlFu@CB composite adsorbing materials for the processing of high-concentration fluorine-containing waste water adsorption cleaning

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104069831A (en) * 2014-07-24 2014-10-01 中国地质大学(北京) Efficient nitrate-removing granular absorbent and preparation method thereof
CN105664884A (en) * 2016-03-29 2016-06-15 中国地质大学(北京) Magnetic adsorbent for removing heavy metal in water and method for preparing magnetic adsorbent
CN107081138A (en) * 2017-05-19 2017-08-22 上海工程技术大学 Magnetic polystyrene base enclosure glycan composite adsorbent and preparation method and application
CN107376863A (en) * 2017-08-30 2017-11-24 河南师范大学 A kind of preparation method of AlFu@CB composite adsorbing materials for the processing of high-concentration fluorine-containing waste water adsorption cleaning

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