CN106554454A - A kind of preparation method and application of polyacrylic acid hydrogel adsorbing material - Google Patents
A kind of preparation method and application of polyacrylic acid hydrogel adsorbing material Download PDFInfo
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- CN106554454A CN106554454A CN201611072981.6A CN201611072981A CN106554454A CN 106554454 A CN106554454 A CN 106554454A CN 201611072981 A CN201611072981 A CN 201611072981A CN 106554454 A CN106554454 A CN 106554454A
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- polyacrylic acid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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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
-
- 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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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
The invention discloses a kind of preparation method and application of polyacrylic acid hydrogel adsorbing material, the polyacrylic acid adsorbing material is the N with acrylic acid as monomer, N' methylene-bisacrylamides are cross-linking agent, Ammonium persulfate. is initiator, and sodium sulfite is flocculation aid, is formed by radical polymerization.Simple synthetic method of the present invention, reaction condition is required low, cost of material is cheap, it is easy to utilization and extention, and synthesize and adsorption operations step simplicity, polyacrylic acid hydrogel adsorbing material effectively can be adsorbed to heavy metal ion such as uranium, copper to reach the purpose for rationally administering sewage, by adjusting different initial concentrations, most suitable PH, time of equilibrium adsorption can obtain the adsorption conditionses of optimum.
Description
Technical field
The present invention relates to biological chemical field, and in particular to a kind of preparation method of polyacrylic acid hydrogel adsorbing material and
Using
Background technology
Absorption has been obtained on a large scale should in the field such as water process, especially heavy-metal ion removal and organic dyestuff
With, in all of adsorbing material, macromolecule hydrogel has substantial amounts of active group (heavy metal ion sequestering activity position because of which
Point) and be widely applied.Most adsorbing material absorption properties are low, bad mechanical strength and be difficult to recycle, polyacrylic acid
Substantial amounts of carboxylic group and chemical stability be good, solvent resistance occupies by force consequence due to having for hydrogel.
Traditional polyacrylic acid hydrogel synthetic method need to be carried out under nitrogen protection, and polymerization time is more long, relatively costly,
It is unfavorable for popularization and application.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of system of polyacrylic acid hydrogel adsorbing material
Preparation Method and application, the inventive method are protected without the need for nitrogen, and simple and efficient, cost is relatively low.
To achieve these goals, the present invention is employed the following technical solutions：
A kind of preparation method of polyacrylic acid hydrogel adsorbing material, is the N with acrylic acid as monomer, N'- di-2-ethylhexylphosphine oxides third
Acrylamide is cross-linking agent, and Ammonium persulfate. is initiator, and sodium sulfite is flocculation aid, is formed by radical polymerization.
Preparation method of the present invention is specific as follows：Acrylic acid solution, ammonium persulfate solution and bisulfite are prepared respectively
Sodium solution, N, N'- methylene-bisacrylamides are dissolved in acrylic acid solution, ammonium persulfate solution and bisulfite is added
Sodium solution, dilute obtain mixed solution, and in the mixed solution, acrylic acid mass fraction is 28-32%, and N, N'- are sub-
The mass fraction of bisacrylamide is 0.8-1.2%, and the mass fraction of Ammonium persulfate. is 0.35-0.45%, bisulfite
The mass fraction of sodium is 0.35-0.45%；
Then above-mentioned mixed liquor is stirred, stands and polyreaction formation hydrogel occurs, the hydrogel is shredded
Lyophilization afterwards, obtains polyacrylic acid hydrogel adsorbing material, and the adsorbing material is stored in 50 DEG C of baking ovens.
Further, in the mixed solution, acrylic acid mass fraction is 30%, N, N'- methylene-bisacrylamides
Mass fraction is 1%, and the mass fraction of Ammonium persulfate. is 0.42%, and the mass fraction of sodium sulfite is 0.42%.
The polymerization temperature of the polyreaction is 23-27 DEG C, and polymerization time is 2-2.5h.
Further, the polymerization temperature of the polyreaction is 25 DEG C, and polymerization time is 2h.
Polyacrylic acid hydrogel adsorbing material prepared by the present invention is applied to water process, the heavy metal in energy active adsorption water
Ion, such as uranyl ion, copper ion etc..In the case of without N, N'- methylene-bisacrylamides, acrylic monomerss are linear
The polyacrylic acid hydrogel that polymerization is formed is water miscible, cannot be returned after the water miscible adsorbing material Adsorption of Heavy Metal Ions
Receive, cause resource utilization low.And the present invention with the addition of N, N'- methylene-bisacrylamides are used as cross-linking agent, acrylic monomerss
Cross-linked polymeric formed polyacrylic acid hydrogel be it is non-water-soluble, therefore the present invention polyacrylic acid adsorbing material absorption a huge sum of money
It is recyclable after category ion, recycle.
The present invention adopts above technical scheme, and acrylic monomerss are cross-linked to form polyacrylic acid by radical polymerization effect
Hydrogel, in the case of addition flocculation aid, protects without the need for nitrogen, and just energy rapid polymerization obtains polyacrylic acid adsorbing material.This
The polyacrylic acid adsorbing material of invention synthesis is positioned over water in polyacrylic acid using substantial amounts of carboxyl-reactive group on polyacrylic acid
Carboxylate radical is formed when middle, with metal ion by being coordinated bond formed complex, heavy-metal ion removal pollutant is reached
Purpose.By adjusting different initial concentrations, most suitable PH, time of equilibrium adsorption can obtain the adsorption conditionses of optimum.
The present invention remarkable advantage be：Simple synthetic method, quick, condition needed for reaction is few, workable, formation
Adsorbing material is placed in sewage, can fast and effectively heavy-metal ion removal, solve the pollution problem of heavy metal ion in water,
It is a kind of method with applications well prospect, removal of heavy metal ions rate can meet sewage disposal requirement.
Description of the drawings
The present invention is described in more detail below in conjunction with the drawings and specific embodiments：
Fig. 1 is FTIR structural analyses figures；A, b, c are respectively acrylic acid, polyacrylic acid and acrylic acid-uranium complex；
Fig. 2 is the TEM morphology analysis before and after polyacrylic acid hydrogel adsorbs uranyl ion：Before a, c are for absorption, b, d are suction
It is attached；
Fig. 3 is the EDX surface-elements analysis before and after polyacrylic acid hydrogel adsorbs uranyl ion：Before a is for absorption, b is suction
It is attached；
Fig. 4 is impacts of the pH to absorbability in embodiment 5；
Fig. 5 is impact of the initial concentration to adsorbing in embodiment 5；
Fig. 6 is impact of the time to adsorbing in embodiment 5；
Adsorption isotherms of the Fig. 7 for embodiment 5；
Plan second-order kineticses curves of the Fig. 8 for embodiment 5.
Specific embodiment
Several instantiations of the invention below, further describe the present invention, but the present invention are not limited only to this.Embodiment
1
A kind of preparation method of polyacrylic acid hydrogel adsorbing material, it is specific as follows：Acrylic acid solution, over cure are prepared respectively
Acid ammonium solution and sodium sulfite solution, N, N'- methylene-bisacrylamides are dissolved in acrylic acid solution, over cure is added
Acid ammonium solution and sodium sulfite solution, dilute obtain mixed solution, in the mixed solution, acrylic acid mass fraction
For 30%, N, the mass fraction of N'- methylene-bisacrylamides is 1%, and the mass fraction of Ammonium persulfate. is 0.42%, sulfurous acid
The mass fraction of hydrogen sodium is 0.42%；
Then above-mentioned mixed liquor is stirred, stands and polyreaction occurs form hydrogel, the polyreaction it is poly-
It is 25 DEG C to close temperature, and polymerization time is 2h, lyophilization after the hydrogel for obtaining is shredded, and obtains polyacrylic acid hydrogel absorption
Material, is stored in 50 DEG C of baking ovens.
Polyacrylic acid hydrogel manufactured in the present embodiment effectively can be adsorbed to reach to heavy metal ion such as uranium, copper
To the purpose for rationally administering sewage.
Embodiment 2
A kind of preparation method of polyacrylic acid hydrogel adsorbing material, it is specific as follows：Acrylic acid solution, over cure are prepared respectively
Acid ammonium solution and sodium sulfite solution, N, N'- methylene-bisacrylamides are dissolved in acrylic acid solution, over cure is added
Acid ammonium solution and sodium sulfite solution, dilute obtain mixed solution, in the mixed solution, acrylic acid mass fraction
For 28%, N, the mass fraction of N'- methylene-bisacrylamides is 1.2%, and the mass fraction of Ammonium persulfate. is 0.35%, sulfurous
The mass fraction of sour hydrogen sodium is 0.35%；
Then above-mentioned mixed liquor is stirred, stands and polyreaction occurs form hydrogel, the polyreaction it is poly-
It is 23 DEG C to close temperature, and polymerization time is 2.5h, lyophilization after the hydrogel for obtaining is shredded, and obtains polyacrylic acid hydrogel suction
Enclosure material, is stored in 50 DEG C of baking ovens.
Polyacrylic acid hydrogel manufactured in the present embodiment effectively can be adsorbed to reach to heavy metal ion such as uranium, copper
To the purpose for rationally administering sewage.
Embodiment 3
A kind of preparation method of polyacrylic acid adsorbing material, it is specific as follows：It is molten that acrylic acid solution, Ammonium persulfate. are prepared respectively
Liquid and sodium sulfite solution, N, N'- methylene-bisacrylamides are dissolved in acrylic acid solution, Ammonium persulfate. is added molten
Liquid and sodium sulfite solution, dilute obtain mixed solution, and in the mixed solution, acrylic acid mass fraction is
The mass fraction of 32%, N, N'- methylene-bisacrylamide is 0.8%, and the mass fraction of Ammonium persulfate. is 0.45%, sulfurous acid
The mass fraction of hydrogen sodium is 0.45%；
Then above-mentioned mixed liquor is stirred, stands and polyreaction occurs form hydrogel, the polyreaction it is poly-
It is 27 DEG C to close temperature, and polymerization time is 2-2.5h, and lyophilization after the hydrogel for obtaining is shredded obtains polyacrylic acid hydrogel
Adsorbing material, is stored in 50 DEG C of baking ovens.
The polyacrylic acid hydrogel that the present embodiment is prepared effectively can adsorb to heavy metal ion such as uranium, copper
To reach the purpose for rationally administering sewage.
Embodiment 4
A kind of preparation method of polyacrylic acid adsorbing material, it is specific as follows：Weigh 0.5g N, N'- methylene bisacrylamide acyls
Amine solvent adds the 0.21g Ammonium persulfate .s and 0.21g sulfurous acids being dissolved completely in water in 15g acrylic monomerss solution
Solution is finally diluted to 50ml by hydrogen sodium, is stood until formation hydrogel, is placed on freezing after hydrogel is shredded after stirring
24h is dried in drying machine, polyacrylic acid hydrogel adsorbing material is obtained, 50 DEG C of baking ovens is put in and is preserved.
The polyacrylic acid hydrogel that the present embodiment is prepared effectively can adsorb to heavy metal ion such as uranium, copper
To reach the purpose for rationally administering sewage.
Embodiment 5
Polyacrylic acid hydrogel adsorbs uranyl ion
Dried polyacrylic acid hydrogel is taken to UO2 2+Carry out absorption research.The measure of uranyl ion concentration：With azo
Arsine III is chelating agent, determines its concentration with ultraviolet spectrophotometer at 650nm wavelength.
Absorbability is calculated：
Wherein, qeRepresent absorbability, ceAnd c0Balance and initial concentration are represented respectively, and m represents the quality of adsorbing material.
Have studied initial pH, initial concentration, impact of the response time to adsorption process, while intending to adsorption isotherm and kinetics
Close.
As a result show, polyacrylic acid hydrogel adsorbing material has good adsorption to uranyl ion.Such as Fig. 4 institutes
Show, when pH value is relatively low, adsorption effect than relatively low, when 1<pH<When 4, adsorption effect gradually increases, when pH value reaches 4,
Adsorption effect reaches best, no longer changes substantially.The impact of initial concentration is as shown in figure 5, absorbability is before this with concentration
Increase increases sharply, and increases slow afterwards.The impact in response time as shown in fig. 6, increase sharply in initial time adsorbance, afterwards
Increase slow, during to 120min, reach adsorption equilibrium.Fig. 7 shows that absorption best suits Langmuir adsorption isotherms, by
The calculated maximum uranyl ion adsorbance of Langmuir adsorption isotherms is 455.11mg g-1.Fig. 8 shows that adsorption process is accorded with
Close and intend second- order reaction kinetics.
Embodiment 6
Polyacrylic acid hydrogel adsorbs copper ion
Dried polyacrylic acid hydrogel is taken to Cu2+Carry out absorption research.The measure of copper ion concentration：With hexichol phosphinylidyne
Two hydrazines are chelating agent, determine its concentration with ultraviolet spectrophotometer at 546nm wavelength.
Absorbability is calculated：
Wherein, qeRepresent absorbability, ceAnd c0Balance and initial concentration are represented respectively, and m represents the quality of adsorbing material.
Have studied initial pH, initial concentration, impact of the response time to adsorption process, while intending to adsorption isotherm and kinetics
Close.
As a result show, adsorption process has obtained the result similar with example 5.
Claims (7)
1. a kind of preparation method of polyacrylic acid hydrogel adsorbing material, it is characterised in that：The polyacrylic acid hydrogel absorption
Material is the N with acrylic acid as monomer, and N'- methylene-bisacrylamides are cross-linking agent, and Ammonium persulfate. is initiator, bisulfite
Sodium is flocculation aid, is formed by radical polymerization.
2. the preparation method of a kind of polyacrylic acid hydrogel adsorbing material according to claim 1, it is characterised in that：It is described
Preparation method is as follows：Acrylic acid solution, ammonium persulfate solution and sodium sulfite solution are prepared respectively, by N, N'- di-2-ethylhexylphosphine oxides
Acrylamide is dissolved in acrylic acid solution, adds ammonium persulfate solution and sodium sulfite solution, and dilute is mixed
Solution is closed, in the mixed solution, acrylic acid mass fraction is 28-32%, the quality of N, N'- methylene-bisacrylamide point
Number is 0.8-1.2%, and the mass fraction of Ammonium persulfate. is 0.35-0.45%, and the mass fraction of sodium sulfite is 0.35-0.45%；
Then above-mentioned mixed liquor is stirred, stands and polyreaction formation hydrogel occurs, hydrogel lyophilization is obtained
The polyacrylic acid hydrogel adsorbing material.
3. the preparation method of a kind of polyacrylic acid hydrogel adsorbing material according to claim 2, it is characterised in that：It is described
In mixed solution, acrylic acid mass fraction is 30%, N, and the mass fraction of N'- methylene-bisacrylamides is 1%, Ammonium persulfate.
Mass fraction be 0.42%, the mass fraction of sodium sulfite is 0.42%.
4. the preparation method of a kind of polyacrylic acid hydrogel adsorbing material according to claim 2, it is characterised in that：It is described
The polymerization temperature of polyreaction is 23-27 DEG C, and polymerization time is 2-2.5h.
5. the preparation method of a kind of polyacrylic acid hydrogel adsorbing material according to claim 4, it is characterised in that：It is described
The polymerization temperature of polyreaction is 25 DEG C, and polymerization time is 2h.
6. the application of the polyacrylic acid hydrogel adsorbing material as described in one of claim 1-5, it is characterised in that：Described poly- third
Olefin(e) acid hydrogel adsorbing material is applied to water process, adsorbs the heavy metal ion in water.
7. the application of polyacrylic acid hydrogel adsorbing material according to claim 6, it is characterised in that：The heavy metal from
Son is uranyl ion or copper ion.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108341906A (en) * | 2018-03-12 | 2018-07-31 | 福州大学 | A kind of preparation method and application of dye of positive ion composite adsorbing material |
| CN110368916A (en) * | 2019-08-30 | 2019-10-25 | 福州大学 | One heavy metal species composite adsorbing material and the preparation method and application thereof |
| CN110404516A (en) * | 2019-08-14 | 2019-11-05 | 徐州工程学院 | A kind of adsorption of metal ions hydrogel and its preparation method and application |
| CN112973654A (en) * | 2021-03-08 | 2021-06-18 | 吉林化工学院 | Preparation method of double-concentration interval hydrogel adsorbent |
| CN113368835A (en) * | 2021-05-12 | 2021-09-10 | 重庆文理学院 | Environment repairing material and preparation method and application thereof |
| CN114045167A (en) * | 2021-11-23 | 2022-02-15 | 南京林业大学 | Preparation method of rutin hydrogel with optical activity |
| CN115386136A (en) * | 2022-08-30 | 2022-11-25 | 南京大学 | Preparation method and application of aminated polyacrylamide foam adsorbent |
| CN115475607A (en) * | 2022-09-28 | 2022-12-16 | 安徽农业大学 | Cationic amphiphilic fluorine-containing hydrogel adsorbent and preparation method and application thereof |
| CN115724698A (en) * | 2022-11-30 | 2023-03-03 | 中昇南阳生物科技有限公司 | Acidic soil conditioner and preparation method thereof |
| CN115999521A (en) * | 2023-02-28 | 2023-04-25 | 陕西科技大学 | Efficient adsorption material for ammonia nitrogen in wastewater, preparation method and application thereof |
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Cited By (16)
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| CN108341906A (en) * | 2018-03-12 | 2018-07-31 | 福州大学 | A kind of preparation method and application of dye of positive ion composite adsorbing material |
| CN108341906B (en) * | 2018-03-12 | 2020-03-17 | 福州大学 | Preparation method and application of cationic dye composite adsorption material |
| CN110404516A (en) * | 2019-08-14 | 2019-11-05 | 徐州工程学院 | A kind of adsorption of metal ions hydrogel and its preparation method and application |
| CN110368916A (en) * | 2019-08-30 | 2019-10-25 | 福州大学 | One heavy metal species composite adsorbing material and the preparation method and application thereof |
| CN110368916B (en) * | 2019-08-30 | 2022-03-22 | 福州大学 | Heavy metal composite adsorption material and preparation method and application thereof |
| CN112973654A (en) * | 2021-03-08 | 2021-06-18 | 吉林化工学院 | Preparation method of double-concentration interval hydrogel adsorbent |
| CN113368835A (en) * | 2021-05-12 | 2021-09-10 | 重庆文理学院 | Environment repairing material and preparation method and application thereof |
| CN114045167A (en) * | 2021-11-23 | 2022-02-15 | 南京林业大学 | Preparation method of rutin hydrogel with optical activity |
| CN115386136A (en) * | 2022-08-30 | 2022-11-25 | 南京大学 | Preparation method and application of aminated polyacrylamide foam adsorbent |
| CN115386136B (en) * | 2022-08-30 | 2023-07-28 | 南京大学 | Preparation method and application of aminated polyacrylamide foam adsorbent |
| CN115475607A (en) * | 2022-09-28 | 2022-12-16 | 安徽农业大学 | Cationic amphiphilic fluorine-containing hydrogel adsorbent and preparation method and application thereof |
| CN115475607B (en) * | 2022-09-28 | 2024-01-23 | 安徽农业大学 | Cationic amphiphilic fluorine-containing hydrogel adsorbent and preparation method and application thereof |
| CN115724698A (en) * | 2022-11-30 | 2023-03-03 | 中昇南阳生物科技有限公司 | Acidic soil conditioner and preparation method thereof |
| CN115999521A (en) * | 2023-02-28 | 2023-04-25 | 陕西科技大学 | Efficient adsorption material for ammonia nitrogen in wastewater, preparation method and application thereof |
| CN116870842A (en) * | 2023-09-08 | 2023-10-13 | 中创宏远（北京）环保科技有限公司 | Preparation process of novel kitchen equipment filler |
| CN116870842B (en) * | 2023-09-08 | 2024-02-02 | 中创宏远（北京）环保科技有限公司 | Preparation process of kitchen equipment filler |
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