CN106582577A - Preparation method and applications of attapulgite/polymer porous millimeter-scale small ball - Google Patents
Preparation method and applications of attapulgite/polymer porous millimeter-scale small ball Download PDFInfo
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- CN106582577A CN106582577A CN201710011413.3A CN201710011413A CN106582577A CN 106582577 A CN106582577 A CN 106582577A CN 201710011413 A CN201710011413 A CN 201710011413A CN 106582577 A CN106582577 A CN 106582577A
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- 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
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- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- 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
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- 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
- B01J20/28014—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 form
- B01J20/28016—Particle form
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- 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
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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
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/48—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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic 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
- C02F1/28—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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- 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
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/203—Iron or iron compound
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Abstract
The present invention discloses a preparation method and applications of an attapulgite/polymer porous millimeter-scale small ball. The preparation method comprises: dispersing attapulgite and a polymer in a solvent, adding to a non-solvent phase in a liquid droplet form in a dropwise manner, and forming a ball through phase conversion so as to obtain the small ball with a diameter of several millimeters. According to the present invention, the preparation method is simple and is suitable for large-scale production; the prepared millimeter-scale porous attapulgite/polymer small ball can be suspended on the surface of the water body and can be directly recovered through the filtration screen so as to substantially simplify the recovery problem of the attapulgite as the adsorbent and achieve the 100% recovery effect; and the attapulgite/polymer porous millimeter-scale small ball has good adsorption effects on variety of metal ions, is easily desorbed, can be recycled, has a certain mechanical property and chemical stability, and is easy to store, transport and use.
Description
Technical field
The invention belongs to sorbing material technical field, and in particular to a kind of attapulgite/polyalcohol stephanoporate grade bead
Preparation method and applications.
Background technology
At present, attapulgite there are problems that reclaiming difficult and be difficult directly as adsorbent.Attapulgite powder
End is scattered in after solution system, needs to be separated by way of the complexity such as high speed centrifugation or filtration, and is extremely difficult to
100% recovery, therefore, the rate of recovery of attapulgite how is improved by straightforward procedure, it is to promote attapulgite industrialization to answer
Key.Though there is part research by the way that attapulgite and magnetic iron oxide are combined, the method reclaimed by magnet
(Journal of Industrial and Engineering Chemistry, 34 (2016) 374-381) or by hydrogel
Carrier (Industrial＆Engineering Chemistry Research, 53 (2014) 4277-4285) is done, is carried concavo-convex
The method of rod soil improves to a certain extent the rate of recovery of attapulgite, however it remains many problems.Such as, by magnet
The method of recovery, it is difficult to large-scale operation and large-area process, and carrier is done with hydrogel, it is equivalent that expansion is there is again
Should, the less stable of material.Accordingly, it would be desirable to developing a kind of simple efficient method prepares attapulgite sorbing material.
The content of the invention
The purpose of this part is to summarize some aspects of embodiments of the invention and briefly introduce some preferable enforcements
Example.May do in this part and the description of the present application summary and denomination of invention a little simplified or omit to avoid making our department
Point, the purpose of specification digest and denomination of invention obscure, and this simplification or omission cannot be used for limiting the scope of the present invention.
In view of the skill of the preparation method and applications of above-mentioned and/or existing attapulgite/polyalcohol stephanoporate grade bead
Art is blank, it is proposed that the present invention.
Therefore, one of purpose of the invention is to use not side directly as metal ion adsorbent for attapulgite
Just and be difficult to reclaim the problems such as, there is provided a kind of grade porous attapulgite/polymer composite pellets, it is concavo-convex so as to solve
Rod soil reclaims difficult as adsorbent, and in removal process the problems such as sample loss.
To solve above-mentioned technical problem, the invention provides following technical scheme：A kind of attapulgite/polyalcohol stephanoporate milli
The preparation method of meter level bead, it includes, attapulgite and polymer are disperseed in a solvent, it to be instilled in droplets
In non-solvent phase, by phase transformation process balling-up, the other bead of a diameter of grade is obtained.
As a kind of preferred version of the preparation method of attapulgite of the present invention/polyalcohol stephanoporate grade bead,
Wherein：The attapulgite in organic solvent, and adds polymer by ultrasonic agitation, dispersion, until polymer dissolving, obtains
To attapulgite/mixed with polymers solution.
As a kind of preferred version of the preparation method of attapulgite of the present invention/polyalcohol stephanoporate grade bead,
Wherein：The attapulgite is (0.1～1.5) with the mass ratio of polymer：1.
As a kind of preferred version of the preparation method of attapulgite of the present invention/polyalcohol stephanoporate grade bead,
Wherein：The polymer is one or more of polyether sulfone, polysulfones, Kynoar.
As a kind of preferred version of the preparation method of attapulgite of the present invention/polyalcohol stephanoporate grade bead,
Wherein：The organic solvent is in 1-METHYLPYRROLIDONE, dimethyl acetamide, dimethylformamide or diethyl acetamide
One or more.
As a kind of preferred version of the preparation method of attapulgite of the present invention/polyalcohol stephanoporate grade bead,
Wherein：The non-solvent is mutually water or water and 1-METHYLPYRROLIDONE, dimethyl acetamide, dimethylformamide or diethyl second
The mixed liquor that one or more in acid amides are formed.
The present invention another purpose therein is to provide a kind of attapulgite/polyalcohol stephanoporate grade bead in ADSORPTION OF GOLD
The application of category ions.
As attapulgite of the present invention/application of the polyalcohol stephanoporate grade bead in terms of adsorbing metal ions
A kind of preferred version, wherein：The metal ion is copper, and cadmium, iron, nickel, europium weighs one or more.
As attapulgite of the present invention/application of the polyalcohol stephanoporate grade bead in terms of adsorbing metal ions
A kind of preferred version, wherein：Attapulgite after adsorbing metal ions/polyalcohol stephanoporate grade bead, Jing pH<2 dilute salt
Acid desorption, repetitive cycling is used.
The present invention is had the advantage that：
1) attapulgite of the porous with mm size/polymer globules method that prepared by the present invention is simple, it is easy to big rule
Mould is produced.
2) attapulgite/polymer globules can be suspended in water surface, can directly be reclaimed by filter screen, enormously simplify
Attapulgite and can reach the effect of 100% recovery as the recovery problem of adsorbent.
3) attapulgite/polymer globules have preferable adsorption effect to each metal ion species, and are easily desorbed, can be again
It is multiple to recycle.
4) attapulgite/polymer globules have certain mechanical performance and chemical stability, facilitate accumulating and use.
Description of the drawings
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below will be to use needed for embodiment description
Accompanying drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this
For the those of ordinary skill of field, without having to pay creative labor, can be obtaining other according to these accompanying drawings
Accompanying drawing.Wherein：
Fig. 1 is the SEM shape appearance figures of attapulgite.
Fig. 2, wherein, it is (a) attapulgite/polymer globules cross section SEM patterns, (b) it is dispersed in for attapulgite little
SEM figures inside ball.
Specific embodiment
It is understandable to enable the above objects, features and advantages of the present invention to become apparent from, with reference to specific embodiment pair
The specific embodiment of the present invention is described in detail.
Many details are elaborated in the following description in order to fully understand the present invention, but the present invention can be with
It is different from alternate manner described here to implement using other, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by following public specific embodiment.
Secondly, " one embodiment " or " embodiment " referred to herein is referred to and may be included at least one realization side of the invention
Special characteristic, structure or characteristic in formula." in one embodiment " that in this manual different places occur not refers both to
Same embodiment, nor single or selectively mutually exclusive with other embodiment embodiment.
Embodiment 1
1g attapulgites and 1g polyether sulfones are added in 8.5gN- methyl pyrrolidones (NMP) prepares attapulgite/polymerization
Thing solution, and solution is added in needle tubing, by advancing needle tubing (fltting speed is 1mL/min), by polymer solution with liquid
The form of drop, in being added dropwise to water, drop passes through inversion of phases process settings balling-up.Its balling-up attapulgite theory solid content be
50wt%.Its detailed process is as follows：250mg attapulgites/polymer globules are added to the copper that 25mL initial concentrations are 500ppm
Solion (CuSO4·5H2O in), Jing after adsorption saturation (8h), the adsorbance of copper ion is 25.13mg/g.
Embodiment 2
It is molten that 0.5g attapulgites and 1g polyether sulfones are added to preparation attapulgite/polymer in 8.5g dimethyl acetamides
Liquid, and solution is added in needle tubing, by advancing needle tubing (fltting speed is 1mL/min), by polymer solution with drop
Form, in being added dropwise to the mixed solution of water and dimethyl acetamide, drop passes through inversion of phases process settings balling-up.Its balling-up it is recessed
Convex rod soil theory solid content is 33wt%.250mg attapulgites/polymer globules are added to 25mL initial concentrations for 500ppm's
Copper ion solution (CuSO4·5H2O in), Jing after adsorption saturation (8h), the adsorbance of copper ion is 11.80mg/g.
Embodiment 3
It is molten that 0.1g attapulgites and 1g polyether sulfones are added to preparation attapulgite/polymer in 8.5g, dimethylformamide
Liquid, and solution is added in needle tubing, by advancing needle tubing (fltting speed is 1mL/min), by polymer solution with drop
Form, in being added dropwise to the mixed solution of water and dimethylformamide, drop passes through inversion of phases process settings balling-up.Its balling-up it is recessed
Convex rod soil theory solid content is 9.1wt%.250mg attapulgites/polymer globules are added to 25mL initial concentrations for 500ppm
Copper ion solution (CuSO4·5H2O in), Jing after adsorption saturation (8h), the adsorbance of copper ion is 2.85mg/g.
Embodiment 4
1g attapulgites and 1g polysulfones are added to preparation attapulgite/polymer solution in 8.5g diethyl acetamides, and
Solution is added in needle tubing, by advancing needle tubing (fltting speed is 1mL/min), by polymer solution in droplets,
In being added dropwise to the mixed solution of water and diethyl acetamide, drop passes through inversion of phases process settings balling-up.The concave convex rod of its balling-up
Native theory solid content is 50wt%.250mg attapulgites/polymer globules be added to 25mL initial concentrations be 500ppm copper from
Sub- solution (CuSO4·5H2O in), Jing after adsorption saturation (8h), the adsorbance of copper ion is 24.90mg/g.
Embodiment 5
It is molten that 1g attapulgites and 1g Kynoar (PVDF) are added to preparation attapulgite/polymer in 8.5g NMP
Liquid, and solution is added in needle tubing, by advancing needle tubing (fltting speed is 1mL/min), by polymer solution with drop
Form, in being added dropwise to the mixed solution of water and NMP, drop passes through inversion of phases process settings balling-up.The attapulgite reason of its balling-up
It is 50wt% by solid content.It is molten that 250mg attapulgites/polymer globules are added to the copper ion that 25mL initial concentrations are 500ppm
Liquid (CuSO4·5H2O in), Jing after adsorption saturation (8h), the adsorbance of copper ion is 25.80mg/g.
Embodiment 6
1g attapulgites and 1g polyether sulfones are added in 8.5g NMP preparation attapulgite/polymer solution, and by solution
In being added to needle tubing, by advancing needle tubing (fltting speed is 1mL/min), it is added dropwise to by polymer solution in droplets
In water, drop passes through inversion of phases process settings balling-up.The attapulgite theory solid content of its balling-up is 50wt%.250mg is concavo-convex
Rod soil/polymer globules are added to the copper ion solution that 25mL initial concentrations are 100ppm, and the bead after adsorption saturation is placed on
It is desorbed in 0.2mL hydrochloric acid, the bead washing after desorption is dried, is carried out the adsorption/desorption circulation (copper of 100ppm next time
Solion).The adsorbance of the first six bead copper ion is respectively 10.2,8.2,4.1,4.0,3.8 and 4.0mg/g, shows
Excellent recycling performance.
Embodiment 7
1g attapulgites and 1g polyether sulfones are added in 8.5g NMP preparation attapulgite/polymer solution, and by solution
In being added to needle tubing, by advancing needle tubing (fltting speed is 1mL/min), it is added dropwise to by polymer solution in droplets
In water, drop passes through inversion of phases process settings balling-up.The attapulgite theory solid content of its balling-up is 50wt%.250mg is concavo-convex
Rod soil/polymer globules are added to the cadmium-ion solution (Cd (CH that 25mL initial concentrations are 500ppm3COO)2·2H2O in), Jing
After adsorption saturation (8h), the adsorbance of cadmium ion is 31.0mg/g.
Embodiment 8
1g attapulgites and 1g polyether sulfones are added in 8.5g NMP preparation attapulgite/polymer solution, and by solution
In being added to needle tubing, by advancing needle tubing (fltting speed is 1mL/min), it is added dropwise to by polymer solution in droplets
In water, drop passes through inversion of phases process settings balling-up.The attapulgite theory solid content of its balling-up is 50wt%.250mg is concavo-convex
Rod soil/polymer globules are added to the cadmium-ion solution that 25mL initial concentrations are 100ppm, and the bead after adsorption saturation is placed on
It is desorbed in 0.2mol/L hydrochloric acid, the bead washing after desorption is dried, is carried out adsorption/desorption circulation (100ppm next time
Cadmium-ion solution).The adsorbance of the first six bead cadmium ion is respectively 10.3,8.1,7.9,8.1,8.0 and 8.4mg/g, opens up
Reveal excellent recycling performance.
Embodiment 9
1g attapulgites and 1g polyether sulfones are added in 8.5g NMP preparation attapulgite/polymer solution, and by solution
In being added to needle tubing, by advancing needle tubing (fltting speed is 1mL/min), it is added dropwise to by polymer solution in droplets
In water, drop passes through inversion of phases process settings balling-up.The attapulgite theory solid content of its balling-up is 50wt%.1274mg is concavo-convex
Rod soil/polymer globules are immersed in 0.2mol/L hydrochloric acid after 3 days and take out, and washing is dried, and weighs, and its weight loss is 28mg,
Show that the bead has good chemical stability in hydrochloric acid (desorbing agent).
Embodiment 10
1g attapulgites and 1g polyether sulfones are added in 8.5g NMP preparation attapulgite/polymer solution, and by solution
In being added to needle tubing, by advancing needle tubing (fltting speed is 1mL/min), it is added dropwise to by polymer solution in droplets
In the mixed solution of water and NMP, drop passes through inversion of phases process settings balling-up.Its balling-up attapulgite theory solid content be
50wt%.
The attapulgite theory solid content of its balling-up is 50wt%.250mg attapulgites/polymer globules are added to 25mL
Initial concentration is the cadmium-ion solution of 100ppm, the difference pH hydrochloric acid solutions desorption of the bead after adsorption saturation, little after desorption
Ball is washed, and is dried, and carries out adsorption/desorption circulation (cadmium-ion solution of 100ppm) next time.
Concrete outcome such as following table：
From the point of view of by result, with the rising of the pH of desorption hydrochloric acid solution used, 6 adsorption/desorption circulations of Jing, sample institute body
The negative change increase of existing adsorbance.That is, in desorption process, hydrochloric acid solution pH value is controlled below 2, to embody preferably
The property of can be recycled.
This is because, the prepared product of the present invention, its adsorbing metal ions, dominant mechanism is that its surface hydroxyl position (SOH) is same
In solution there is surface coordination, complex reaction in heavy metal ion, and also it occurs ion exchange with heavy metal ion, its
In, dominant mechanism is ion exchange.
It should be noted that above example is only unrestricted to illustrate technical scheme, although with reference to preferably
Embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the technology of the present invention
Scheme is modified or equivalent, and without deviating from the spirit and scope of technical solution of the present invention, it all should cover at this
In the middle of bright right.
Claims (9)
1. the preparation method of a kind of attapulgite/polyalcohol stephanoporate grade bead, it is characterised in that：Including,
Attapulgite and polymer are disperseed in a solvent, it to be instilled in droplets in non-solvent phase, by phase transformation
Process balling-up, obtains the other bead of a diameter of grade.
2. the preparation method of attapulgite as claimed in claim 1/polyalcohol stephanoporate grade bead, it is characterised in that：It is described
Attapulgite in organic solvent, and adds polymer by ultrasonic agitation, dispersion, until polymer dissolving, obtains concave convex rod
Soil/mixed with polymers solution.
3. the preparation method of attapulgite as claimed in claim 1 or 2/polyalcohol stephanoporate grade bead, it is characterised in that：Institute
It is (0.1～1.5) that attapulgite is stated with the mass ratio of polymer：1.
4. the preparation method of attapulgite as claimed in claim 1 or 2/polyalcohol stephanoporate grade bead, it is characterised in that：Institute
State one or more that polymer is polyether sulfone, polysulfones, Kynoar.
5. the preparation method of attapulgite as claimed in claim 2/polyalcohol stephanoporate grade bead, it is characterised in that：It is described
Organic solvent is the one kind or several in 1-METHYLPYRROLIDONE, dimethyl acetamide, dimethylformamide or diethyl acetamide
Kind.
6. as any one of claim 1,2 or 5 attapulgite/polyalcohol stephanoporate grade bead preparation method, its
It is characterised by：The non-solvent is mutually water or water and 1-METHYLPYRROLIDONE, dimethyl acetamide, dimethylformamide or diethyl
The mixed liquor that one or more in yl acetamide are formed.
7. a kind of attapulgite/application of the polyalcohol stephanoporate grade bead in terms of adsorbing metal ions.
8. attapulgite as claimed in claim 7/application of the polyalcohol stephanoporate grade bead in terms of adsorbing metal ions, its
It is characterised by：The metal ion be copper, cadmium, iron, nickel, one or more in europium.
9. attapulgite as claimed in claim 7/application of the polyalcohol stephanoporate grade bead in terms of adsorbing metal ions, its
It is characterised by：Attapulgite after adsorbing metal ions/polyalcohol stephanoporate grade bead, Jing pH<2 watery hydrochloric acid desorption, weight
It is multiple to recycle.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107185419A (en) * | 2017-07-04 | 2017-09-22 | 合肥市大卓电力有限责任公司 | A kind of air purifier dedusting film and preparation method |
| WO2019165598A1 (en) * | 2018-02-28 | 2019-09-06 | Honeywell International Inc. | Polymer composite granule and method of processing the same |
| CN110302743A (en) * | 2019-06-24 | 2019-10-08 | 上海交通大学 | The preparation method of Adsorption of Radioactive nucleic and the concave convex rod bead of heavy metal ion |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101219367A (en) * | 2007-09-30 | 2008-07-16 | 四川大学 | Amino acid modified montmorillonite-synthesized polymer hybridisation microsphere, preparation method and application thereof |
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| CN107185419A (en) * | 2017-07-04 | 2017-09-22 | 合肥市大卓电力有限责任公司 | A kind of air purifier dedusting film and preparation method |
| WO2019165598A1 (en) * | 2018-02-28 | 2019-09-06 | Honeywell International Inc. | Polymer composite granule and method of processing the same |
| CN110302743A (en) * | 2019-06-24 | 2019-10-08 | 上海交通大学 | The preparation method of Adsorption of Radioactive nucleic and the concave convex rod bead of heavy metal ion |
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