CN110420626A - Acrylic acid/acrylamide/styrene terpolymer hydrogel and its preparation method and application - Google Patents
Acrylic acid/acrylamide/styrene terpolymer hydrogel and its preparation method and application Download PDFInfo
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- CN110420626A CN110420626A CN201910747441.0A CN201910747441A CN110420626A CN 110420626 A CN110420626 A CN 110420626A CN 201910747441 A CN201910747441 A CN 201910747441A CN 110420626 A CN110420626 A CN 110420626A
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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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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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
- B01J20/28—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
- B01J20/28047—Gels
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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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- 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
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract
The invention discloses a kind of acrylic acid/acrylamide/styrene terpolymer hydrogels and its preparation method and application, the hydrogel is the three-element copolymerized hydrogel being made of three kinds of acrylic acid, acrylamide and styrene monomer atactic polymerizations, acrylic acid, three kinds of monomers of acrylamide and styrene molar ratio be (1~3): (1~3): 1.Using potassium peroxydisulfate as initiator, N, N- methylene-bisacrylamide is crosslinking agent, and acrylic acid degree of neutralization is polymerize under the conditions of being 80%, obtains the acrylic acid/acrylamide/styrene terpolymer hydrogel.Acrylic acid/acrylamide of the invention/styrene terpolymer hydrogel is high to the adsorbance of heavy metal in waste water, good cycle.
Description
Technical field
The present invention relates to a kind of preparation method and applications of adsorption of metal ions hydrogel, belong to polyalcohol hydrogel absorption
Agent field.
Background technique
Heavy metal ion toxicity is very big, is not easy to be metabolized in vivo, they can be with teratogenesis, carcinogenic, mutagenesis, can be with
Make endocrine disturbance, this can seriously threaten the mankind, the health and existence of animals and plants.The current contaminated by heavy metals side of anti-water-stop body
Method has chemical precipitation method, hyperfiltration, biological restoration, ion exchange and absorption method etc..Work efficiency is high because of it for absorption method,
It is easy to operate and environmental-friendly and receive significant attention.Selection can form having compared with high stable constant complex with heavy metal ion
Machine functional group matrix, obtained hydrogel adsorbent, which has, prepares convenient, adsorbance height, steady performance.Hydrogel is inhaled
Attached dose because having good hydrophily, and it is cheap, have good market prospects, industry, agricultural etc. can be widely used in
Field.Zhang etc. makees mixed solvent with water and Isosorbide-5-Nitrae-dioxane, makees crosslinking agent with acrylamide, n-isopropyl acrylamide,
Then by free radical polymerization, the temperature-sensitive hydrogel of removable swelling has been made.Kuila etc. is raw material, over cure with acrylic acid
Sour potassium is initiator, and chain-transferring agent is added, and is made to Ca2+There is the polyacrylic acid hydrogel of very strong chelation.Zhao etc. with
Acrylamide, phytic acid and dopamine are that monomer is prepared for composite hydrogel, and the hydrogel is to Cu2+Equilibrium adsorption capacity reach
(231.36±4.70)mg/g.PP type hydrogel plays an important role in heavy metal ion adsorbed.
Summary of the invention
For present polymer hydrogel adsorbent to heavy metal adsorption type is few in sewage, is difficult to adapt to current heavy metal
The problem of sewage treatment of complicated composition, the object of the present invention is to provide a kind of acrylic acid/acrylamide/styrene terpolymers
Hydrogel and its preparation method and application is adsorbed with being suitable for various metals, and adsorption efficiency is high.
To achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of acrylic acid/acrylamide/styrene terpolymer hydrogel, for by acrylic acid, acrylamide and benzene second
The three-element copolymerized hydrogel that three kinds of monomer atactic polymerizations of alkene are constituted, mole of three kinds of acrylic acid, acrylamide and styrene monomers
Than for (1~3): (1~3): 1.
A kind of preparation method of acrylic acid/acrylamide/styrene terpolymer hydrogel, with acrylic acid, acrylamide
It is raw material with styrene, using potassium peroxydisulfate as initiator, N, N- methylene-bisacrylamide is crosslinking agent, and acrylic acid degree of neutralization is
It is polymerize under the conditions of 80%, obtains the acrylic acid/acrylamide/styrene terpolymer hydrogel.
Preferably, the dosage of the potassium peroxydisulfate is 0.5~0.8%, N of three kinds of monomer gross mass, N- di-2-ethylhexylphosphine oxide third
The dosage of acrylamide is the 1~5% of three kinds of monomer gross mass.
Specific step is as follows for acrylic acid/acrylamide of the invention/styrene terpolymer hydrogel preparation method:
Step 1, the sodium hydroxide solution that mass fraction is 40% is added in acrylic acid, stirs 10-20min, it is then cold
But to room temperature；
Step 2, acrylamide, styrene are then sequentially added, 10-20min is stirred；
Step 3, potassium peroxydisulfate is added, after stirring 5-10min, N is added, N '-methylene-bisacrylamide pours into container,
70 DEG C are warming up to, successive reaction 8h；It reacts obtained product drying and crushing and obtains powder.
Preferably, in the step 3, reaction and drying carry out in pallet, and reaction system solution height is protected when reaction
Hold 5-10cm.
Preferably, it in the step 3, crushes as 200 mesh powders.
Acrylic acid/acrylamide of the invention/styrene terpolymer hydrogel can be used for as heavy metal absorbent
Heavy metal ion in absorption effluent.
The acrylic acid/acrylamide/styrene terpolymer hydrogel can be fitted very well to heavy metal ion adsorbed
Second kinetics equation.
Preferably, the heavy metal ion be lead ion, cadmium ion, nickel ion, cobalt ions, copper ion, magnesium ion, zinc from
Sub is one or more.
Preferably, the acrylic acid/acrylamide/styrene terpolymer hydrogel optimal adsorption condition are as follows: 0.1g
Acrylic acid/acrylamide/styrene terpolymer hydrogel corresponds to the heavy metal ion that concentration of heavy metal ion is 1000mg/L
Solution, adsorption time are 2 hours.
Preferably, the acrylic acid/acrylamide/styrene terpolymer hydrogel is for different heavy metal ion,
It is specific as follows with different optimal adsorption pH value:
Adsorb Pd2+When, Optimal pH 4.4-5.5, maximal absorptive capacity 458.7mg/g；
Adsorb Mg2+When, Optimal pH 2.5-3.5, maximal absorptive capacity 264.3mg/g；
Adsorb Cd2+When, Optimal pH 4.5-6.5, maximal absorptive capacity 205.6mg/g；
Adsorb Zn2+When, Optimal pH 5.5, maximal absorptive capacity 190.0mg/g；
Adsorption of Cu2+When, Optimal pH 4.5, maximal absorptive capacity 156.3mg/g；
Adsorb Ni2+When, Optimal pH 3.5-4.5, maximal absorptive capacity 165.3mg/g；
Adsorb Co2+When, Optimal pH 4.5-6, maximal absorptive capacity 246.3mg/g.
The acrylic acid/acrylamide/styrene terpolymer hydrogel can recycle reuse three times.
The utility model has the advantages that compared with the prior art, the present invention has the advantages that
(1) Biosorbent for heavy metals prepared by has wide applicability, in sewage lead, nickel, cadmium, copper, cobalt,
The heavy metals such as magnesium have significant adsorption effect, and adsorbance reaches 156mg/g or more, especially selectively good to lead ion, maximum
Adsorbance reaches 459mg/g, and removal rate is up to 93%；
(2) it carries out test to the adsorption capacity of polyalcohol hydrogel adsorbent prepared by the present invention to learn, polymer water
The adsorbable lead ion 458.7mg of gel adsorber, cadmium ion 205.6mg, cobalt ions 246.3mg, nickel ion 165.3mg, copper from
Sub- 156.3mg, magnesium ion 264.3mg, zinc ion 190.0mg, from the above data, polymer water-setting prepared by the present invention
Glue adsorbent is to heavy metal adsorbance with higher；
(3) Biosorbent for heavy metals preparation method of the present invention is simple, and mild condition is easy to operate, can carry out commercial introduction
With production.
Detailed description of the invention
Fig. 1 is acrylic acid/acrylamide/styrene terpolymer hydrogel infrared spectroscopy in embodiment 1；
Fig. 2 is acrylic acid/acrylamide/styrene terpolymer hydrogel IR spectrum scanning electronics in embodiment 1
Microscope；
Fig. 3 is acrylic acid/acrylamide/styrene terpolymer hydrogel thermogravimetric analysis in embodiment 1；
Fig. 4 is acrylic acid/acrylamide/competition of the styrene terpolymer hydrogel to heavy metal ion in embodiment 1
Adsorb schematic diagram.
Specific embodiment
Below with reference to embodiment, the invention will be further described, following embodiment be intended to illustrate invention rather than it is right
Of the invention further limits.
Embodiment 1
The present embodiment the following steps are included:
(1) acrylic acid/acrylamide/styrene terpolymer hydrogel preparation
The sodium hydroxide solution that 24.0mL mass fraction is 40% is added in 20.6mL acrylic acid, stirs 15min, then
It is cooled to room temperature.Then 7.108g acrylamide, 5.7Ml styrene are sequentially added, 15min is stirred.The over cure of 0.509g is added
After stirring 6min, the N of 0.170g is added in sour potassium, and N '-methylene-bisacrylamide pours into pallet, keeps liquid level thickness 8cm, rises
Temperature is to 70 DEG C, successive reaction 8h.Drying and crushing obtains the hydrogel powders of 200 mesh or so, obtains acrylic acid/acrylamide/benzene
Ethylene three-element copolymerized hydrogel.
(2) influence that different plumbum ion concentrations adsorb lead ion
In pH=5.3, adsorption time is tested under conditions of being 120min, is measured to obtain weight by atomic spectrophotometer
Concentration of metal ions calculates Pb2+The adsorbance Q and adsorption rate R of each concentration hydrogel of ion.
As shown in Table 1, with Pb2+Initial concentration be continuously increased, hydrogel is to Pb2+Adsorbance be continuously increased, in Pb2 +Concentration in 5~1000mg/L, adsorbance rises to 448.959mg/g from 1.22mg/g, and adsorbance ascendant trend is obvious.
In Pb2+When concentration is greater than 1000mg/g, hydrogel is to Pb2+Adsorbance ascendant trend slow down, it is basic to maintain to stablize.This is main
It is because having many adsorption sites on hydrogel, when between 5mg/L to 1000mg/L, adsorption site gives full play to absorption and makees
With when initial concentration continues to increase, adsorption site has been occupied full, and can not be continued to adsorb heavy metal ion, be led to adsorbance
Hardly increase.With the raising of lead ion solution concentration, adsorption rate also constantly rises, in Pb2+When concentration is 1000mg/L,
Adsorption rate reaches 94.6%, in Pb2+When concentration is 2000mg/L, it is only 49% that adsorption rate, which sharply declines, it can be seen that the water-setting
Glue is lower to the heavy metal ion solution adsorption rate of higher concentration.To sum up, the influence by initial concentration to hydrogel adsorption effect
Analysis can obtain, and hydrogel is not much different to the concentration of heavy metal ion adsorbance of 1000mg/L and 2000mg/L, it is contemplated that save
Cost, when the concentration that heavy metal ion solution may be selected is 1000mg/L, the adsorbance of hydrogel reaches saturation.
1 difference Pb of table2+Initial concentration hydrogel adsorpting data table
(3) analysis of hydrogel difference adsorption time
In pH=5.3, plumbum ion concentration is tested under conditions of being 1000mg/L, is measured by atomic spectrophotometer
To concentration of heavy metal ion, by calculating Pb2+Under ion different time, the adsorbance Q of hydrogelt。
From the figure 3, it may be seen that hydrogel is to Pb2+Adsorbance and adsorption rate can increase and then become with the increase of adsorption time
In steady.In preceding 60min, Pb2+Adsorbance ascendant trend it is the most obvious, within 5min~60min this period, hydrogel
To Pb2+Adsorbance promptly rise to 429.764mg/g from 353.183mg/g, in 60min~120min this period,
Hydrogel is to Pb2+Adsorbance is increased speed gradually gently, and adsorbance tends to be steady after 120min, and adsorption rate reaches 93.1%.From
As can be seen that Pb in figure2+The time for reaching adsorption equilibrium is about that absorption has just been opened in the main reason for 120min or so, this trend
There is the adsorption site of a large amount of skies when the beginning, on hydrogel, therefore adsorption rate is very fast, adsorbance increases rapidly.With pushing away for time
It moves, absorption point is reduced, and adsorption process is hindered, and causes adsorption rate gradually slow.To sum up, by adsorption time to hydrogel
The impact analysis of adsorption effect can obtain, Pb2+Time when adsorption equilibrium is 120min.
2 different time hydrogel of table is to Pb2+The adsorbance of ion
(4) adsorption dynamics adsorption kinetics research of the hydrogel to lead ion
Table 3 is hydrogel to Pb2+The kinetic parameter of suction-operated, works as R2When > 0.995, it can prove that adsorption process accords with
Close the kinetic model.It can be obtained by graphic analyses, Pb2+First _ order kinetics equation in, R2=0.9295 < 0.995, Pb2+'s
In second-order kinetic equation, R2=0.9996 > 0.995, therefore hydrogel adsorbs Pb2+Process be fitted quasi- second motive force well
Model is learned, because adsorption process has been fitted quasi- second order dynamic model, therefore should consider to compare second-order kinetics rate constant.Two
K in grade kinetic model2Size reflect hydrogel absorption and reach the speed of balance, i.e. k2 is bigger, and absorption reaches balance
Speed is faster.But quasi- First order dynamic model and quasi- second order dynamic model cannot explain diffusion process, at this moment just need water
Gel is to Pb2+Particle in diffusion model, R2Although=0.8973 explanation hydrogel is to pb2+Adsorption process in there are particle expansions
It dissipates, but is not the speed control stage only at absorption initial stage, it is not high for entire adsorption process correlation.To sum up hydrogel
To Pb2+Adsorption process be fitted second order dynamic model well.
3 hydrogel of table is to Pb2+The kinetic parameter of suction-operated
(5) influence of the PH to hydrogel adsorbing metal ions
It can be obtained by table 4: Pb being adsorbed to hydrogel by different pH2+Performance test, obtain and constantly increase as pH value obtains,
The adsorbance and adsorption rate of hydrogel also constantly increase, and in pH=1.5, adsorbance 7.28mg/g, hydrogel is to Pb2+Suction
Attached rate is almost 0, and when the section pH is 4.5~5.5, it is 94.8% that adsorption rate, which reaches peak value,.This is because when pH is too low, solution
In there are a large amount of H+, and these a large amount of H+Ion will form adsorption site with metal ion existing for script in solution competing
Relationship is striven, so that the adsorption site that metal ion enters in hydrogel is hindered, so when pH is lower, hydrogel counterweight
Metal ion Pb2+Adsorbance is seldom, when the ph is increased, H in solution+Relatively fewer, competition weakens, and hydrogel is to Pb2+Absorption
Amount increases.To sum up, work as Pb2+For pH value of solution between 4.5 to 5.5, adsorbance is up to 458.7mg/g.If we want this kind
In material application to reality, we can first adjust the pH value of sewage before the use, be allowed in optimal absorption
Within the scope of PH.
4 difference Pb of table2+PH value of solution hydrogel adsorpting data table
(6) the reusable property analysis of hydrogel
As shown in Table 5, hydrogel is to Pb2+Adsorbance drop to 300mg/g or so, this is because being used in test process
The aperture of tea-bag is too small, prevents hydrogel and heavy metal ion solution from caused by coming into full contact with.With absorption and desorption
The increase of number, hydrogel obtain adsorption capacity to ion and constantly decline, and the adsorption rate of hydrogel gradually decreases.This is because using
The nitric acid of pH=1 is as stripping liquid, and acid too strong, nitric acid can destroy the structure of adsorbent to a certain extent, affect hydrogel
It adsorbs again.But hydrogel desorbed four times with the nitric acid solution of pH=1, when the 5th time, hydrogel is remained to
To Pb2+Solution has the adsorbance of 50mg/g or so, and this also illustrates hydrogels to have certain desorption and regeneration performance, Ke Yichong
It is multiple to utilize.
Table 5 surveys recycling of the hydrogel to heavy metal in parallel three times
(7) competitive Adsorption is analyzed
It is 5.5 in pH, adsorption time 2h, each solion concentration is the absorption that is at war under conditions of 1000mg/L
Experiment.Known by table 6 and Fig. 4, in the presence of 5 kinds of ions are with different mixed forms, acrylic acid/acrylamide/polystyrene ternary is total
Polyglycerol hydrogel can reduce the adsorbance of 5 kinds of ions.The Pb in five systems2+Adsorbance be only 87.80mg/g, but Pb2+In
Adsorbance when its independent system is 458.70mg/g.This is because when metal ion separately exists in system, metal from
Son can sufficiently combine the activated adoption point on hydrogel, so that adsorbance is very big.When several ions have a system jointly
In, since every heavy metal species ion concentration is larger, and the absorption point limited bits on hydrogel, cause activated adoption point to be easy
Overlapping, the activated adoption point being occupied cannot be in conjunction with other heavy metal ion, to make the absorption of every heavy metal species ion
Amount has different degrees of decline[12]。Pb2+In Pb2+/Cd2+/Co2+/Cu2+/Ni2+、Pb2+/Cd2+、Pb2+/Ni2+、Pb2+/Co2+、
Pb2+/Cu2+In this five systems, the Kd coefficient and adsorbance of lead ion are maximum, illustrate that lead ion is more competed compared with other ions
Property and hydrogel is to Pb2+Affinity be greater than other four kinds of ions.
Competitive Adsorption amount of 6 hydrogel of table to heavy metal ion
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of acrylic acid/acrylamide/styrene terpolymer hydrogel, it is characterised in that: it is by acrylic acid, acryloyl
The three-element copolymerized hydrogel that three kinds of monomer atactic polymerizations of amine and styrene are constituted, three kinds of acrylic acid, acrylamide and styrene lists
The molar ratio of body is (1~3): (1~3): 1.
2. a kind of preparation method of acrylic acid/acrylamide described in claim 1/styrene terpolymer hydrogel, special
Sign is: using acrylic acid, acrylamide and styrene as raw material, using potassium peroxydisulfate as initiator, N, and N- methylene bisacrylamide acyl
Amine is crosslinking agent, and acrylic acid degree of neutralization is polymerize under the conditions of being 80%, obtains the acrylic acid/acrylamide/styrene three
First copolymer hydrogel.
3. acrylic acid/acrylamide according to claim 2/styrene terpolymer hydrogel preparation method, special
Sign is: the dosage of the potassium peroxydisulfate is 0.5~0.8%, N of three kinds of monomer gross mass, N- methylene-bisacrylamide
Dosage is the 1~5% of three kinds of monomer gross mass.
4. acrylic acid/acrylamide according to claim 2 or 3/styrene terpolymer hydrogel preparation method,
Be characterized in that: specific step is as follows:
Step 1, the sodium hydroxide solution that mass fraction is 40% is added in acrylic acid, stirs 10-20min, is subsequently cooled to
Room temperature；
Step 2, acrylamide, styrene are then sequentially added, 10-20min is stirred；
Step 3, potassium peroxydisulfate is added, after stirring 5-10min, N is added, N '-methylene-bisacrylamide pours into container, heats up
To 70 DEG C, successive reaction 8h；It reacts obtained product drying and crushing and obtains powder.
5. acrylic acid/acrylamide according to claim 4/styrene terpolymer hydrogel preparation method, special
Sign is: in the step 3, reaction and drying carry out in pallet, and reaction system solution height keeps 5-10cm when reaction；
Crushing is 200 mesh powders.
6. acrylic acid/acrylamide described in claim 1/styrene terpolymer hydrogel is being inhaled as heavy metal absorbent
The application of heavy metal ion in attached sewage.
7. application according to claim 6, it is characterised in that: the heavy metal ion be lead ion, cadmium ion, nickel from
Son, cobalt ions, copper ion, magnesium ion, zinc ion it is one or more.
8. application according to claim 6, it is characterised in that: the acrylic acid/acrylamide/styrene terpolymer water
The adsorption conditions of gel are as follows: 0.1g acrylic acid/acrylamide/styrene terpolymer hydrogel corresponds to concentration of heavy metal ion and is
The heavy metal ion solution of 1000mg/L, adsorption time are 2 hours.
9. application according to claim 7, it is characterised in that: when adsorpting lead ion, the pH of sewage is adjusted to 4.4-
5.5；When adsorbing magnesium ion, the pH of sewage is adjusted to 2.5-3.5；When Adsorption of Cadmium, the pH of sewage is adjusted to 4.5-
6.5；When adsorbing zinc ion, the pH of sewage is adjusted to 5.5；When adsorbing copper ion, the pH of sewage is adjusted to 4.5；Adsorb nickel
When ion, the pH of sewage is adjusted to 3.5-4.5；When adsorbing cobalt ions, the pH of sewage is adjusted to 4.5-6.
10. application according to claim 6, it is characterised in that: the acrylic acid/acrylamide/styrene terpolymer
Hydrogel can recycle reuse three times.
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| CN114832789A (en) * | 2022-03-23 | 2022-08-02 | 江门市新会区中盛生物科技有限公司 | Method for removing polymerization inhibitor in acrylic acid by replacing activated carbon adsorption and adsorbent |
| CN117050339A (en) * | 2023-08-22 | 2023-11-14 | 江苏绿安擎峰新材料有限公司 | Synthesis process and application of functionalized polystyrene hydrogel |
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