CN109364887A - A kind of preparation method of the porous Ca-alginate gel beads for heavy metal-polluted water process - Google Patents
A kind of preparation method of the porous Ca-alginate gel beads for heavy metal-polluted water process Download PDFInfo
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- 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
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a kind of preparation methods of porous Ca-alginate gel beads for heavy metal-polluted water process, the method comprises the following steps: configuring certain density sodium alginate aqueous solution first, and micro-/ nano microspheres solution is added in sodium alginate aqueous solution, it is stirred continuously and mixes them thoroughly;Then gained mixed liquor is added dropwise in calcium chloride solution dropwise, obtains the Ca-alginate gel beads containing template microsphere;Again vacuum freeze drying will be carried out after the washing of obtained gel ball;Obtained gel ball is finally put into ultrasound in organic reagent and is soaked for a period of time removing micro-/ nano microsphere template, obtains the porous Ca-alginate gel beads of micro/nano level.The porous Ca-alginate gel beads that pore diameter range is 100nm-10um can be obtained in the present invention.By the adjusting in aperture, the specific surface area of Ca-alginate gel beads is changed, accelerates the exchange rate of adsorption process intermediate ion, improves its adsorption effect to heavy metal ion.
Description
Technical field
The present invention relates to the preparation methods of high-molecular porous material, and in particular to a kind of porous calcium alginate that aperture is controllable
Plural gel ball preparation method.
Background technique
1. sodium alginate is a kind of high molecular material of natural environmental-protective, it has concentrate solution, formation gel and film forming
Ability.Due to containing the carboxyl largely to dissociate easily in conjunction with heavy metal ion, to have very strong chelating to heavy metal ion
Effect.
2. studies have shown that the gel ball (Ca-alginate gel beads) that sodium alginate and calcium ion are formed is to the weight such as lead, copper, cadmium
Metal ion has preferable adsorption capacity, can be used for the processing of heavy metal containing sewage.
3. the mechanism of Ca-alginate gel beads absorption heavy metal is shown in Figure of description 1.
4. the Calcium alginate bead currently used for heavy metal-polluted water process is all medicine ball, specific surface area is relatively small, shadow
Its adsorption effect to heavy metal ion is rung.Though the preparation of porous Ca-alginate gel beads has been reported that, obtained by preparation method
In the micron-scale, aperture is larger and the uniformity in aperture is poor for the gel ball aperture arrived.
Summary of the invention
1. passing through choosing the object of the present invention is to provide a kind of preparation method of the adjustable porous Ca-alginate gel beads in aperture
The template microsphere of different-grain diameter is selected, the adjusting in the aperture to the porous Ca-alginate gel beads of preparation is realized, to improve alginic acid
The adsorption effect of the metal ion of calcium gel ball can be used for the sewage treatment containing heavy metal.
2., should the present invention provides a kind of preparation method of porous Ca-alginate gel beads for heavy metal-polluted water process
Method comprises the following steps:
3. step 1 configures certain density sodium alginate aqueous solution, and micro-/ nano microspheres solution is added to alginic acid
In sodium water solution, it is stirred continuously and mixes them thoroughly;
4. step 2, the uniform mixed liquor that step 1 is obtained is added dropwise in calcium chloride solution dropwise, is obtained micro- containing template
The Ca-alginate gel beads of ball;
5. step 3 will carry out vacuum freeze drying after the washing of gel ball obtained in step 2;
6. the gel ball after vacuum freeze drying in step 3 is put into reagent solution and is soaked for a period of time removing by step 4
Micro-/ nano microsphere template obtains the porous Ca-alginate gel beads of micro/nano level.
7. the preparation method of the above-mentioned porous Ca-alginate gel beads for heavy metal-polluted water process, wherein it is described it is micro-/
The partial size of nanosphere is 100nm-10um;
Preferably, the partial size of micro-/ nano microballoon is 500nm-1.7um;
Optionally, the microballoon is selected from polystyrene microsphere, at least one of silicon dioxide microsphere;
Optionally, the mass fraction of micro-/ nano microballoon is 0.05%-10% in the solution;
Preferably, the mass fraction of micro-/ nano microballoon is 0.5%-2% in the solution;
Optionally, the mass fraction of micro-/ nano microballoon lotion is 0.1%-10% in the mixed liquor.
Optionally, the solution containing micro-/ nano microballoon is that micro-/ nano microballoon is dispersed in aqueous solvent;Wherein, described
Dispersing mode is selected from supersonic cell and crushes at least one of 1-2h, ultrasound 1-6h, stirring 1-24h.
8. the preparation method of the above-mentioned porous Ca-alginate gel beads for heavy metal-polluted water process, wherein the sea
The mass fraction of sodium alginate is 0.5%-3% in alginic acid sodium water solution;
Preferably, the mass fraction of sodium alginate is 1%-2% in sodium alginate aqueous solution;
Optionally, the dispersing mode of sodium alginate in water crushes in 0.5-1h, stirring 1-6h selected from supersonic cell
It is at least one.
9. the preparation method of the above-mentioned porous Ca-alginate gel beads for heavy metal-polluted water process, wherein the chlorine
The amount of substance concentration for changing calcium solution is 0.02M-0.3M;
Preferably, the amount of substance concentration of calcium chloride solution is 0.1M-0.2M.
10. the preparation method of the above-mentioned porous Ca-alginate gel beads for heavy metal-polluted water process, wherein the step
The volume ratio of uniform mixed liquor and calcium chloride in rapid 2 is 1:4-6;
Preferably, the volume ratio of the uniform mixed liquor in the step 2 and calcium chloride is 1:5.
11. the preparation method of the above-mentioned porous Ca-alginate gel beads for heavy metal-polluted water process, wherein the step
Processing mode in rapid 3 should include freezing and two processes of vacuum freeze drying.
Optionally, the cooling time under -20 DEG C of low temperature refrigerators of the plural gel ball in step 3 is 12-24h;
Optionally, cryogenically treated plural gel ball vacuum freeze drying time under the conditions of -60 DEG C, vacuum degree 15Pa
For 24-72h.
12. the preparation method of the above-mentioned porous Ca-alginate gel beads for heavy metal-polluted water process, wherein the step
The method of micro-/ nano microsphere template is removed in rapid 4 as the immersion of solution ultrasound.
Optionally, the solution in the solution ultrasound soaking process includes toluene, acetone, tetrahydrofuran, hydrogen fluoride solution
At least one of;
Optionally, ultrasonic time is 24-72h in ultrasonic soaking process.
13. the mesh that the present invention reaches to regulate and control porous calcium alginate composite gel ball aperture by changing the partial size of template microsphere
, pore diameter range 100nm-10um.By the adjusting in aperture, change the specific surface area of porous calcium alginate composite gel ball, from
And improve its adsorption effect to heavy metal ion, it is suitable for heavy metal-polluted water process.
Detailed description of the invention
Fig. 1 is the mechanism schematic diagram that Ca-alginate gel beads adsorb heavy metal
Fig. 2 is that the SEM of comparative example Ca-alginate gel beads is characterized.
Fig. 3 is that the SEM of porous Ca-alginate gel beads is characterized.
Fig. 4 is 4 kinds of gel balls (embodiment 1-3 and comparative example) to the chart of heavy metal ion adsorbed effect.
Fig. 5 is 4 kinds of gel balls (embodiment 1-3 and comparative example) to the histogram of Heavy Metals ionic adsorption effect.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
In the case where not illustrating, raw material described herein for example sodium alginate, styrene, potassium peroxydisulfate, acetone,
Tetrahydrofuran, hydrofluoric acid, calcium chloride etc. are bought from Aladdin company or Sinopharm Chemical Reagent Co., Ltd..
Analysis method is as follows in embodiments herein:
Sem analysis is carried out using FEI Co. of U.S. Sirion200 field emission scanning electron microscope thermal field.
Adsorption effect analysis is carried out using the OPTIMA ICP in the U.S..
Embodiment 1
20g deionized water, 0.2g sodium alginate are added to be placed on blender in 100ml beaker and stir 6h, is configured
At 1% sodium alginate soln.
The polystyrene microsphere lotion that 0.05g 2% is added into above-mentioned sodium alginate soln forms mixed solution, microballoon
Partial size about 600nm, and mixed solution is placed on blender and stirs 6h.
Above-mentioned uniform mixed solution is added drop-wise in the calcium chloride solution of 0.2M dropwise with dropper, and by the gel of formation
Ball is put into low temperature refrigerator and carries out freezing 12h after being washed with deionized 3 times.
The above-mentioned sample that freezing is completed is put on vacuum freeze dryer progress vacuum freeze drying 48h, after i.e.
Obtain porous Ca-alginate gel beads.Gained sample is denoted as 2#.
Embodiment 2
The polystyrene microsphere lotion of 0.1g 2% is added in 1% sodium alginate soln configured into embodiment 1
Mixed solution, the partial size of microballoon about 600nm are formed, and mixed solution is placed on blender and stirs 6h.
Above-mentioned uniform mixed solution is added drop-wise in the calcium chloride solution of 0.2M dropwise with dropper, and by the gel of formation
Ball is put into low temperature refrigerator and carries out freezing 12h after being washed with deionized 3 times.
The above-mentioned sample that freezing is completed is put on vacuum freeze dryer progress vacuum freeze drying 48h, after i.e.
Obtain porous Ca-alginate gel beads.Gained sample is denoted as 3#.
Embodiment 3
The polystyrene microsphere lotion of 0.5g 2% is added in 1% sodium alginate soln configured into embodiment 1
The partial size about 600nm of mixed solution microballoon is formed, and mixed solution is placed on blender and stirs 6h.
Above-mentioned uniform mixed solution is added drop-wise in the calcium chloride solution of 0.2M dropwise with dropper, and by the gel of formation
Ball is put into low temperature refrigerator and carries out freezing 12h after being washed with deionized 3 times.
The above-mentioned sample that freezing is completed is put on vacuum freeze dryer progress vacuum freeze drying 48h, after i.e.
Obtain porous Ca-alginate gel beads.Gained sample is denoted as 4#.
Embodiment 4
20g deionized water, 0.4g sodium alginate are added to be placed on blender in 100ml beaker and stir 6h, is configured
At 2% sodium alginate soln.
The polystyrene microsphere lotion that 0.05g 2% is added into above-mentioned sodium alginate soln forms mixed solution, microballoon
Partial size about 200nm, and mixed solution is placed on blender and stirs 6h.
Above-mentioned uniform mixed solution is added drop-wise in the calcium chloride solution of 0.2M dropwise with dropper, and by the gel of formation
Ball is put into low temperature refrigerator and carries out freezing 12h after being washed with deionized 3 times.
The above-mentioned sample that freezing is completed is put on vacuum freeze dryer progress vacuum freeze drying 48h, after i.e.
Obtain porous Ca-alginate gel beads.Gained sample is denoted as 5#.
Embodiment 5
The polystyrene microsphere lotion of 0.1g 2% is added in 2% sodium alginate soln configured into embodiment 4
Mixed solution, the partial size of microballoon about 200nm are formed, and mixed solution is placed on blender and stirs 6h.
Above-mentioned uniform mixed solution is added drop-wise in the calcium chloride solution of 0.2M dropwise with dropper, and by the gel of formation
Ball is put into low temperature refrigerator and carries out freezing 12h after being washed with deionized 3 times.
The above-mentioned sample that freezing is completed is put on vacuum freeze dryer progress vacuum freeze drying 48h, after i.e.
Obtain porous Ca-alginate gel beads.Gained sample is denoted as 6#.
Embodiment 6
The polystyrene microsphere lotion of 0.5g 2% is added in 2% sodium alginate soln configured into embodiment 4
Mixed solution, the partial size of microballoon about 200nm are formed, and mixed solution is placed on blender and stirs 6h.
Above-mentioned uniform mixed solution is added drop-wise in the calcium chloride solution of 0.2M dropwise with dropper, and by the gel of formation
Ball is put into low temperature refrigerator and carries out freezing 12h after being washed with deionized 3 times.
The above-mentioned sample that freezing is completed is put on vacuum freeze dryer progress vacuum freeze drying 48h, after i.e.
Obtain porous Ca-alginate gel beads.Gained sample is denoted as 7#.
As a comparison, it is prepared for being not added with the Ca-alginate gel beads of template microsphere, 1% sodium alginate is drawn with dropper
It is added dropwise in the calcium chloride solution of 0.2M, solid Ca-alginate gel beads is made.Sample is denoted as 1#.
Fig. 1 is that the scanning electron microscope that comparative example Ca-alginate gel beads obtain under the conditions of different amplification is shone
Piece.Fig. 2 is the electron scanning micrograph that porous Ca-alginate gel beads obtain under different amplification;It can from figure
With find out remove template microsphere after in Ca-alginate gel beads pore size and its distribution it is all relatively uniform.Fig. 3 and Fig. 4 is 4 kinds
Gel ball (embodiment 1-3 and comparative example) is to the diagram of heavy metal ion adsorbed effect;It can be seen from the graph that porous seaweed
Sour calcium gel ball improves a lot to the adsorption capacity of heavy metal ion compared with comparative example Ca-alginate gel beads, and is added different
There is also certain differences for adsorption capacity of the Ca-alginate gel beads of proportional template microballoon to heavy metal ion.
Through, to heavy metal ion adsorbed Experimental Comparison, being found porous calcium alginate compounded with comparative example Ca-alginate gel beads
Gel ball significantly improves the removal rate of heavy metal ion, and it is potential to illustrate that this kind of new material has in heavy metal-polluted water harnessing
Value.
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (9)
1. a kind of preparation method of the porous Ca-alginate gel beads for heavy metal-polluted water process, which is characterized in that this method
It comprises the following steps: step 1, configuring certain density sodium alginate aqueous solution, and micro-/ nano microspheres solution is added to seaweed
In acid sodium aqueous solution, it is stirred continuously and mixes them thoroughly;Step 2, uniform mixed liquor step 1 obtained is added dropwise to chlorination dropwise
In calcium solution, the Ca-alginate gel beads containing template microsphere are obtained;Step 3, gel ball obtained in step 2 is washed laggard
Row vacuum freeze drying;Step 4, the gel ball after vacuum freeze drying in step 3 is put into ultrasound in reagent solution and impregnates one
The section time removes micro-/ nano microsphere template, obtains the porous Ca-alginate gel beads of micro/nano level.
2. the method according to claim 1, wherein the partial size of micro-/ nano microballoon is 100nm-10um;
Preferably, the partial size of micro-/ nano microballoon is 500nm-1.7um;
Preferably, the microballoon is selected from polystyrene microsphere, at least one of silicon dioxide microsphere;
Preferably, the mass fraction of micro-/ nano microballoon is 0.05%-10% in the solution;
It is further preferred that the mass fraction of micro-/ nano microballoon is 0.5%-2% in the solution;
Preferably, the solution containing micro-/ nano microballoon is that micro-/ nano microballoon is dispersed in aqueous solvent;Wherein, the dispersion
Mode is selected from supersonic cell and crushes at least one of 1-2h, ultrasound 1-6h, stirring 1-24h.
3. the method according to claim 1, wherein the quality of sodium alginate is divided in the sodium alginate aqueous solution
Number is 0.5%-3%;
Preferably, the mass fraction of sodium alginate is 1%-2% in sodium alginate aqueous solution;
Preferably, the dispersing mode of sodium alginate in water crushes in 0.5-1h, stirring 1-6h at least selected from supersonic cell
It is a kind of.
4. the method according to claim 1, wherein the amount of substance concentration of the calcium chloride solution is 0.02M-
0.3M。
Preferably, the amount of substance concentration of calcium chloride solution is 0.1M-0.2M.
5. the method according to claim 1, wherein the body of uniform mixed liquor and calcium chloride in the step 2
Product is than being 1:4-6;
Preferably, the volume ratio of the uniform mixed liquor in the step 2 and calcium chloride is 1:5.
6. the method according to claim 1, wherein the vacuum freezedrying in the step 3 should include freezing
With two processes of vacuum freeze drying.
Preferably, the cooling time under -20 DEG C of low temperature refrigerators of the plural gel ball in step 3 is 12-24h;
Preferably, cryogenically treated plural gel ball vacuum freeze drying time under the conditions of -60 DEG C, vacuum degree 15Pa is
24-72h。
7. the method according to claim 1, wherein the method for removing micro-/ nano microsphere template in the step 4
For the immersion of solution ultrasound.
Preferably, the solution in the solution ultrasound soaking process include toluene, acetone, tetrahydrofuran, in hydrogen fluoride solution
It is at least one;
Preferably, ultrasonic time is 24-72h in ultrasonic soaking process.
8. a kind of purposes of the porous Ca-alginate gel beads using method described in claim 1 preparation, which is characterized in that should
Porous Ca-alginate gel beads are used as the absorption of heavy metal ion in water.
9. a kind of porous Ca-alginate gel beads, which is characterized in that comprising according to claim 1 to any one of 8 the method systems
Standby obtained at least one of the porous Ca-alginate gel beads of micro/nano level.
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CN112191234A (en) * | 2020-10-09 | 2021-01-08 | 厦门理工学院 | Sodium alginate adsorption stent and preparation method and application thereof |
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