CN108187641B - A kind of preparation method and applications of sodium alginate/polyvinyl alcohol@polyacrylamide core-shell structure gel ball - Google Patents
A kind of preparation method and applications of sodium alginate/polyvinyl alcohol@polyacrylamide core-shell structure gel ball Download PDFInfo
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- CN108187641B CN108187641B CN201711436540.4A CN201711436540A CN108187641B CN 108187641 B CN108187641 B CN 108187641B CN 201711436540 A CN201711436540 A CN 201711436540A CN 108187641 B CN108187641 B CN 108187641B
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- 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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- 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
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- 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
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- 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
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- 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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- 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
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- 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
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Abstract
The present invention provides a kind of preparation method of sodium alginate/polyvinyl alcohol@polyacrylamide core-shell structure gel ball, includes the following steps: that at room temperature, the mixed liquor A of sodium alginate and polyvinyl alcohol is added in calcium chloride solution, forms plural gel ball；Plural gel ball is added in polyacrylamide solution and is stirred, by mixture global transfer into glutaraldehyde solution, reaction obtains sodium alginate-polyvinyl alcohol@polyacrylamide core-shell structure gel ball.The present invention is wrapped in sodium alginate/polyvinyl alcohol gel ball surface using polyacrylamide, and polyacrylamide contains a large amount of amino and oxygroup, realizes sodium alginate/polyvinyl alcohol gel ball functionalization, improves its absorption property to pollutant；Meanwhile stability is improved so that the gel ball hydrophily of core-shell structure reduces by intermolecular, the intramolecular crosslinking of glutaraldehyde, be conducive to recycle.
Description
Technical field
The invention belongs to the preparation of high-molecular compound and environment-friendly engineering technical fields, and in particular to and a kind of sodium alginate/
The preparation method and applications of polyvinyl alcohol@polyacrylamide core-shell structure gel ball.
Background technique
Along with the fast development of the industries such as China's metallurgy, plating, pesticide and weaving, a large amount of heavy metal wastewater thereby is discharged into
Water body, water environment pollution have become environmentalist's urgent problem to be solved.Heavy metal has biological concentration and biomagnification
Characteristic, can by the approach such as food chain be enriched in human body, human metabolism, nerve etc. are damaged, bio-toxicity
Significantly, it is easy to cause slow poisoning etc., seriously threatens the health of human body.
Absorption method has many advantages, such as raw material sources are wide, easy to operate, treatment process is simple, is at heavy metal-containing waste water
One of important development direction of reason.The quality of adsorption effect depends primarily on adsorbent, adsorbent be absorption method key component and
Key foundation, during adsorption treatment, type, property, the quality of kind of adsorbent are related to adsorption treatment effect
Key factor.Existing adsorbent is usually bad to the metal ion removal effect in water environment, and exists after absorption difficult time
It receives and secondary pollution problems, if it is possible to which preparation efficiently removes heavy metal in water, while environmentally protective and be easily recycled
The adsorbent utilized is significant.
Since pollutant component is extremely complex in heavy metal wastewater thereby, wastewater property caused by different industries is different,
Often traditional adsorbent can not effectively meet treatment effect sometimes.Therefore, functionalization adsorbent material becomes the heat of people's research
One of point.Sodium alginate as a kind of natural polymers, since it is wide with source, biodegradable, hydrophilic and
Favor with carboxyl abundant and hydroxy functional group etc., by numerous researchers.But single sodium alginate adsorbent is deposited
The deficiencies of mechanical strength is not high, adsorption capacity is smaller.Currently, researcher is mainly by modified mode, by its with it is other
Organic polymer, metal nano material etc. are compound, so that improving it adsorbs capacitive energy.Therefore, it develops a kind of efficient, high mechanical strong
The adsorbent spend, being easily recycled has actual application prospect.
Summary of the invention
Technical problem to be solved by the present invention lies in the defects of the prior art for foregoing description, strengthen at adsorbent
The effect containing middle effluent containing heavy metal ions is managed, is provided a kind of with high-adsorption-capacity, high mechanical strength, environmentally protective recyclable benefit
With synthesis step is relatively easy, the method for the core-shell structure gel ball of preparation easy to industrialized production based on sodium alginate.
Technical solution of the present invention can be realized by following technical measures:
A kind of preparation method of sodium alginate/polyvinyl alcohol@polyacrylamide core-shell structure gel ball, including following sequence
The step of:
(1) at room temperature, the mixed liquor A of sodium alginate and polyvinyl alcohol is added in calcium chloride solution, forms plural gel
Then ball washes away the remaining calcium ion of plural gel ball surface with distilled water；
(2) plural gel ball obtained by step (1) is added in polyacrylamide solution, stirs to get mixture B；
(3) mixture B global transfer is obtained into mixture C into glutaraldehyde solution；
(4) mixture C reacts 0.5~12h at 50~80 DEG C, and gel ball is obtained by filtration, repeatedly with distilled water and ethyl alcohol
Rinse is multiple；
(5) gel ball obtained by step (4) is dried or is freezed, obtain sodium alginate-polyvinyl alcohol@polyacrylamide
Amine core-shell structure gel ball.
Preferably, the mass fraction of sodium alginate is 1%~5% in step (1) mixed liquor A.
Preferably, the mass ratio of sodium alginate and polyvinyl alcohol is (10~90): (90~10) in step (1) mixed liquor A.
Preferably, the mass fraction of polyacrylamide is 0.5%~5% in step (2) mixture B.
Preferably, the type of polyacrylamide includes non-ionic, anionic, cationic, both sexes in step (2)
Type.
Preferably, the mass fraction of glutaraldehyde is 0.5%~5% in step (3) described glutaraldehyde solution.
Preferably, using water-bath or microwave heating or microwave-water-bath combined heat in step (4), wherein water-bath adds
Heat is that continuous heating is reacted under mechanical stirring, and microwave heating is to heat progress machinery after a certain period of time under certain power to stir
It mixes, microwave-water-bath combined heat is reacted for continuous heating under microwave heating under certain power after a certain period of time mechanical stirring.
Preferably, the mode of drying described in step (5) includes vacuum drying, normal temperature and pressure is dry, is freeze-dried.
A kind of sodium alginate/polyvinyl alcohol@polyacrylamide core-shell structure gel ball, is prepared using the above method.
The sodium alginate that the above method is prepared/polyvinyl alcohol@polyacrylamide core-shell structure gel ball is gone in absorption
Except the application in the heavy metal ion in water environment.
Compared with prior art, the invention has the following beneficial effects:
(1) present invention improves the mechanical strength of sodium alginate gel ball, divides after being easy to adsorb by introducing polyvinyl alcohol
From recycling, while the co-ordinating functionality of gel ball is increased, improves the absorption property to heavy metal；
(2) present invention is wrapped in sodium alginate/polyvinyl alcohol gel ball surface using polyacrylamide, and polyacrylamide contains
There are a large amount of amino and oxygroup, realizes sodium alginate/polyvinyl alcohol gel ball functionalization, improve its suction to pollutant
Attached performance；Meanwhile by intermolecular, the intramolecular crosslinking of glutaraldehyde, so that the gel ball hydrophily of core-shell structure reduces, promoted
Stability further solves adsorbent and is separated by solid-liquid separation difficult problem；
(3) preparation step of the present invention is simple, is convenient for operation；
(4) the core-shell structure gel ball product good adsorption performance and property prepared through the invention is stablized, and is easy to save,
Convenient for application, and environmentally protective can repeatedly recycle.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings, but the embodiment in attached drawing is not constituted to any limit of the invention
System.
Fig. 1 is the Cu of 1 gained gel ball of comparative example 1-3 of the present invention and embodiment2+Ion remaval comparison；
Fig. 2 is the Cu of gel ball obtained by 1-4 of the embodiment of the present invention2+Ion remaval comparison；
Fig. 3 is absorption-parsing loop test result of 1 gained gel ball of the embodiment of the present invention.
Specific embodiment
To keep the present invention easier to understand, specific embodiments of the present invention are further illustrated below.
Control group 1
At room temperature, by 2g sodium alginate, 1g anion-polyacrylamide be added to 100ml mass fraction be 1% it is poly-
In glycohol solution, magnetic agitation for 24 hours, obtains mixed liquor A；Under agitation, the mode that mixed liquor A injection is added is instilled
Into the calcium chloride solution of 400ml mass fraction 5%, gel ball is formed, after continuing hardening for 24 hours, is washed away with distilled water compound solidifying
It is solidifying to obtain sodium alginate/polyvinyl alcohol/polyacrylamide cross-linked gel ball (SA/PVA/PAM) for glueballs calcium ion remained on surface
Glueballs；Obtained gel ball is drained into -4 DEG C of weight in wet bases preservations and 25 DEG C of dryings save afterwards for 24 hours.
Control group 2
At room temperature, 2g sodium alginate is added in the poly-vinyl alcohol solution that 100ml mass fraction is 1%, magnetic agitation
For 24 hours, mixed liquid B is obtained；Under agitation, the mode that mixed liquid B injection is added is added dropwise to 400ml mass fraction 5%
In calcium chloride solution, gel ball is formed, after continuing hardening for 24 hours, washes away the remaining calcium ion of plural gel ball surface with distilled water,
Sodium alginate-polyvinyl alcohol (SA/PVA) gel ball is obtained, obtained gel ball is drained into -4 DEG C of weight in wet bases preservations and 25 DEG C dry
It is dry to save afterwards for 24 hours.
Control group 3
At room temperature, 2g sodium alginate is added to the water magnetic agitation, obtains mixed liquor C；Under agitation, it will mix
The mode that liquid C injection is added is added dropwise in the calcium chloride solution of 400ml mass fraction 5%, forms gel ball, continues hardening for 24 hours
Afterwards, the remaining calcium ion of plural gel ball surface is washed away with distilled water, obtains sodium alginate (SA) gel ball, it will be obtained solidifying
Glueballs drains -4 DEG C of weight in wet bases preservations and 25 DEG C of dryings save afterwards for 24 hours.
Embodiment 1
At room temperature, the sodium alginate of 2g is added in the poly-vinyl alcohol solution that 100ml mass fraction is 1%, magnetic force stirs
It mixes for 24 hours, obtains mixed liquor A；Under stirring condition, the chlorination that mixed liquor A is added dropwise to 400ml mass fraction 5% is added with injection
In calcium solution, gel ball is formed, after continuing hardening for 24 hours, washes away the remaining calcium ion of plural gel ball surface with distilled water；By institute
It obtains plural gel ball to be added in the anion-polyacrylamide solution that 200ml mass fraction is 1%, after magnetic agitation 12h, obtain
To mixture B；In the glutaraldehyde solution for being 2% by mixture B global transfer to 200ml mass fraction, mixed liquor C is obtained；50
Under DEG C water bath with thermostatic control, mechanic whirl-nett reaction 1h；Gel ball product will be obtained by filtration while hot, with 250ml distilled water and 50ml ethyl alcohol
Rinse is multiple repeatedly；By obtained gel ball at 25 DEG C it is dry for 24 hours after to get arriving final product sodium alginate-polyethylene
Alcohol@polyacrylamide (SA/PVA@PAM (1.0)) core-shell structure gel ball.
Embodiment 2
In the way of embodiment 1, the mass fraction of polyacrylamide solution is adjusted to 0.5%, obtained product is used
SA/PVA@PAM (0.5) is indicated.
Embodiment 3
In the way of embodiment 1, the mass fraction of polyacrylamide solution is adjusted to 1.5%, obtained product is used
SA/PVA@PAM (1.5) is indicated.
Embodiment 4
In the way of embodiment 1, the mass fraction of polyacrylamide solution is adjusted to 2.0%, obtained product is used
SA/PVA@PAM (2.0) is indicated.
Product of the present invention is used for Cu in water2+The removal of ion, process are as follows:
(1) sodium alginate (SA) gel ball is investigated by Staticadsorption experiment, sodium alginate/polyvinyl alcohol (SA/PVA) coagulates
Glueballs, sodium alginate/non-core-shell structure gel ball of polyvinyl alcohol/polyacrylamide (SA/PVA/PAM) and sodium alginate/poly-
Vinyl alcohol@polyacrylamide (SA/PVA@PAM (1.0)) core-shell structure gel ball is to Cu2+Removal effect.
Concrete operations are as follows: be packed into the Cu that the initial concentration of 50ml is 50mg/L with centrifuge tube with cover2+Solution uses 0.1mol/L
HCl/NaOH solution tune pH be 5；The different gel ball of comparative example 1-3 and 1 gained of embodiment is thrown as adsorbent respectively
It adds, dosage 1.0g/L；At 25 DEG C, revolving speed 180rpm, oscillation is until absorption reaches balance；Take supernatant with 0.45 μm
After filtering with microporous membrane, with Cu in spectrophotometry measurement solution2+The concentration of ion.As a result as shown in Figure 1.Change as shown in Figure 1
Property after core-shell structure gel ball compared to unmodified gel ball to Cu2+Removal effect be obviously improved.
(2) PVA/SA@PAM gel ball modified under polyacrylamide different quality containing is investigated by Staticadsorption experiment
To Cu2+Removal capacity.
Concrete operations are as follows: being packed into the Cu that the initial concentration of 50ml is 50mg/L with centrifuge tube with cover2+Solution is used
The HCl/NaOH solution tune pH of 0.1mol/L is 5；It is added into using gel ball obtained by embodiment 1-4 as adsorbent, dosage
For 1.0g/L；At 25 DEG C, revolving speed 180rpm, oscillation is until absorption reaches balance；Take supernatant with 0.45 μm of filtering with microporous membrane
Afterwards, with Cu in spectrophotometry measurement solution2+The concentration of ion.As a result as shown in Figure 2.Polyacrylamide quality as shown in Figure 2
Score is 1.0% as modified concentration, and gained gel ball is to Cu2+Removal effect it is optimal.
(3) parsing-adsorption experiment: using the hydrochloric acid solution of 0.2mol/L as parsing solvent, by 1 gained PVA/ of embodiment
SA PAM (1.0) puts into desorbed solution products therefrom after heavy metal adsorption, and at room temperature, 180rpm vibrates 2h, will parse back
The rinse repeatedly of resulting adsorbent is received, later according to Staticadsorption experiment condition experiment method test, the results showed that PVA/SA@
PAM (1.0) core-shell structure gel ball is after 12 absorption-parsing circulation, to Cu2+Removal rate still can reach initial removal
80% or more of effect, and good spherical shape is kept, it is not damaged, as shown in Figure 3.This illustrates PVA/SA@PAM nucleocapsid
Structural gel ball is with good stability, can cost-effectively remove the Cu in water removal2+, have potential practical value.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Invention is explained in detail for good embodiment, those skilled in the art should understand that, it can be to of the invention
Technical solution is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered
In scope of the presently claimed invention.
Claims (10)
1. a kind of sodium alginate/polyvinyl alcohol@polyacrylamide core-shell structure gel ball preparation method, which is characterized in that packet
It includes following steps in sequence:
(1) at room temperature, the mixed liquor A of sodium alginate and polyvinyl alcohol is added in calcium chloride solution, forms plural gel ball, so
The remaining calcium ion of plural gel ball surface is washed away with distilled water afterwards；
(2) plural gel ball obtained by step (1) is added in polyacrylamide solution, stirs to get mixture B；
(3) mixture B global transfer is obtained into mixture C into glutaraldehyde solution；
(4) mixture C reacts 0.5~12h at 50~80 DEG C, and gel ball is obtained by filtration, with distilled water and ethyl alcohol rinse repeatedly
Repeatedly；
(5) gel ball obtained by step (4) is dried or is freezed, obtain sodium alginate-polyvinyl alcohol@polyacrylamide core
Shell structure gel ball.
2. a kind of preparation of sodium alginate according to claim 1/polyvinyl alcohol@polyacrylamide core-shell structure gel ball
Method, it is characterised in that: the mass fraction of sodium alginate is 1%~5% in step (1) mixed liquor A.
3. a kind of preparation of sodium alginate according to claim 1/polyvinyl alcohol@polyacrylamide core-shell structure gel ball
Method, it is characterised in that: the mass ratio of sodium alginate and polyvinyl alcohol is (10~90) in step (1) mixed liquor A: (90~
10)。
4. a kind of preparation of sodium alginate according to claim 1/polyvinyl alcohol@polyacrylamide core-shell structure gel ball
Method, it is characterised in that: the mass fraction of polyacrylamide is 0.5%~5% in step (2) mixture B.
5. a kind of preparation of sodium alginate according to claim 1/polyvinyl alcohol@polyacrylamide core-shell structure gel ball
Method, it is characterised in that: the type of polyacrylamide includes non-ionic, anionic, cationic, both sexes in step (2)
Type.
6. a kind of preparation of sodium alginate according to claim 1/polyvinyl alcohol@polyacrylamide core-shell structure gel ball
Method, it is characterised in that: the mass fraction of glutaraldehyde is 0.5%~5% in step (3) described glutaraldehyde solution.
7. a kind of preparation of sodium alginate according to claim 1/polyvinyl alcohol@polyacrylamide core-shell structure gel ball
Method, it is characterised in that: using water-bath or microwave heating or microwave-water-bath combined heat in step (4), wherein water-bath adds
Heat is that continuous heating is reacted under mechanical stirring, and microwave heating is to heat progress machinery after a certain period of time under certain power to stir
It mixes, microwave-water-bath combined heat is reacted for continuous heating under microwave heating under certain power after a certain period of time mechanical stirring.
8. a kind of preparation of sodium alginate according to claim 1/polyvinyl alcohol@polyacrylamide core-shell structure gel ball
Method, it is characterised in that: the mode of drying described in step (5) includes vacuum drying, normal temperature and pressure is dry, is freeze-dried.
9. a kind of sodium alginate/polyvinyl alcohol@polyacrylamide core-shell structure gel ball, it is characterised in that: use aforesaid right
It is required that the described in any item methods of 1-8 are prepared.
10. sodium alginate/polyvinyl alcohol@polyacrylamide the nucleocapsid being prepared such as any one of claim 1-8 the method
Application of the structural gel ball in the heavy metal ion in Adsorption water environment.
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| CN112221477A (en) * | 2020-09-28 | 2021-01-15 | 湖北富邦科技股份有限公司 | Polyacrylamide modified Fe-Mn-S/sodium alginate composite microsphere and preparation method thereof |
| CN112844333B (en) * | 2021-01-13 | 2023-11-24 | 袁依婷 | Preparation method of organic phosphine doped polyvinyl alcohol chitosan composite sphere |
| CN113861513B (en) * | 2021-10-09 | 2023-05-02 | 包头稀土研究院 | Composite additive, polylactic acid composition and preparation method |
| CN114146694B (en) * | 2021-12-07 | 2024-02-13 | 广西博世科环保科技股份有限公司 | Preparation method, product and application of sodium alginate/polyvinyl alcohol/polyacrylamide/kaolin adsorption material |
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