CN106750380A - A kind of polymer-modified environmentally friendly composite aquogel and its application in heavy metal containing sewage is processed - Google Patents
A kind of polymer-modified environmentally friendly composite aquogel and its application in heavy metal containing sewage is processed Download PDFInfo
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- 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
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
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- C08L33/00—Compositions of homopolymers or 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 of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- C08J2333/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
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- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
A kind of polymer-modified environmentally friendly hydrogel and its application in heavy metal containing sewage is processed, belong to sorbing material technical field.The present invention is using the carbopol gel of situ aggregation method formation as skeleton, biological fiber or other chemical fibres are used as toughener, then carry out further crosslinking using glutaraldehyde to reinforce, form the good polyacrylic acid hydrogel of new Stability Analysis of Structures, mechanical strength.Polymer-modified environmentally friendly composite aquogel prepared by the present invention is a kind of sorbing material with various active group, and it is to the heavy metal ion (Cu with serious harm in aqueous systems2+、Ni2+、Cd2+、Pb2+) adsorption effect it is fabulous.And gel process for preparing is simple, still there is certain mechanical strength after gel water suction, can be used repeatedly, good adsorption effect is respectively provided with to the heavy metal ion in industrial wastewater, sanitary sewage and natural water.
Description
Technical field
The invention belongs to sorbing material technical field, specific a kind of polymer-modified environmentally friendly hydrogel and its in a treatment huge sum of money
Application in category sewage.
Background technology
Our countries are the big countries of industrial production first in the world, and a large amount of sewage containing heavy metal are discharged in the industrial production
To in environment, the intervention to water Natural Circulation is increasing, and natural environment subject to severe risks of damage, original natural equilibrium is beaten
Broken, how such sewage process makes its harmless be melted into the urgent cardinal task that need to be solved.
Sewage in industrial production typically contains plurality of heavy metal pollution, such as：Electroplate Factory, Leather Factory, the sewage of printing and dyeing mill
Deng all containing substantial amounts of Cu2+、Ni2+、Cd2+、Pb2+Etc. heavy metal ion, if it is not processed just be directly discharged to nature ring
Serious contamination hazard will be caused in border to environment.There are a variety of methods for the treatment of such sewage at present, such as：Physics
Absorption method, biological treatment, chemical reaction method etc..Particularly there is absorption method the reasons such as low, the treatment simplicity of energy consumption have received
Increasing concern.Adsorbent in spite of many heavy metal ion is developed, but their adsorption efficiencies and production cost
Generally require further improvement and optimize.Based on the reason for the above, develop new with low cost, efficient heavy metal ion adsorbed
Agent becomes very urgent and important.
Acrylic acid contains carboxyl because of its end group, and its α and β has undersaturated double bond structure, therefore can be by not
Same method is polymerized and forms different polymer, and cross linked polyacrylate is currently widely used as water absorbing agent and the guarantor of function admirable
Aqua.Still further aspect, polyacrylic acid contain it is substantial amounts of can with the complex bound carboxylic group of heavy metal ion, when itself and water knot
When conjunction forms carbopol gel, tridimensional network is internally formed, substantial amounts of carboxyl distribution is wherein so that it can be as property
The excellent adsorbent for heavy metal of energy.Even so, it is seldom by as adsorbent for heavy metal, main cause is poly- third
The structure of olefin(e) acid gel is not sufficiently stable, and mechanical strength is bad.
The content of the invention
We are using the carbopol gel using situ aggregation method formation as skeleton, and biological fiber or other chemistry are fine
Then dimension carries out further crosslinking and reinforces as toughener using glutaraldehyde, forms new Stability Analysis of Structures, mechanical strength good
Polyacrylic acid hydrogel.
The polymer-modified environmentally friendly hydrogel of one kind of the present invention, it is prepared by following steps：
(1) preparation of plural gel
1) take cotton or other with long stapled material such as paper scrap, pieces of cloth, wood chip etc., be put in excessive 0.1~
In 0.5M hydrochloric acid, produced in being stirred under 80~90 DEG C of water-baths to White Flocculus, filter, wash to neutrality and dry, after crushing
Obtain environment-protection fiber element powder；
2) with acrylic acid and acrylamide as polymerized monomer, by polymerized monomer dissolving in deionized water, acrylic acid and third
Acrylamide consumption and be 1 with the mass ratio of deionized water：2~4, acrylic acid is 2~5 with the mass ratio of acrylamide：1；
3) to step 2) NaOH is added in the mixed solution that obtains, acrylic acid is neutralized, degree of neutralization be (addition
Alkali and sour mol ratio) it is 0.7~0.8：1；
4) it is well mixed to the shitosan suddenly to addition polymerized monomer gross mass 0.5~2% in the mixed solution for 3) obtaining；
5) to step 4) add the polyvinyl alcohol water solution of 3~5 times of polymerized monomer gross mass (poly- in the mixed solution that obtains
In vinyl alcohol aqueous solution, the mass fraction of polyvinyl alcohol for 10~20%), and the step of polymerized monomer gross mass 10~30% 1)
The environment-protection fiber element powder of preparation, mechanical agitation is uniform；
6) to step 5) ammonium persulfate of polymerized monomer gross mass 0.2%~0.3% is added in the mixed solution that obtains, gather
Close N ' the N- methylene-bisacrylamides of monomer gross mass 0.5~1%, the tetramethyl second two of polymerized monomer gross mass 0.5~1%
Amine, mechanical agitation is uniform；
7) by step 6) solution that obtains is placed in and obtains condensate within static 4~5 hours at room temperature；
8) by step 7) condensate that obtains is placed in 70~90 DEG C of baking ovens further polymerisation 5~6 hours, answered
Close gel；
(2) plural gel is modified
By plural gel immersion be mass fraction 0.3~0.8% glutaraldehyde water solution in 8~12 hours, make shell gather
Sugar is fully crosslinked with glutaraldehyde；Then by plural gel with soaked in absolute ethyl alcohol 24 hours, unreacted monomer in gel is removed,
Again with the multiple detergent gel of distilled water, and dried under the conditions of 40~60 DEG C, finally absorb water saturation, of the present invention so as to obtain
Polymer-modified environmentally friendly composite aquogel.
(3) adsorption applications of the composite aquogel heavy metal that is modified
Using polymer-modified environmentally friendly composite aquogel of the present invention at ambient temperature to a different types of huge sum of money
Category ion is adsorbed, and the staticaccelerator adsorption time is 6 hours~20 hours；The salt acidolysis of 0.5~1M of gel after adion
Analysis 30~60 minutes, is then soaked 10~30 minutes with the sodium hydroxide solution of 0.1~0.5M and regenerated.During taking-up gel is washed to
Property, next adsorption experiment can be carried out.
It is that one kind has various active base the beneficial effects of the invention are as follows the polymer-modified environmentally friendly composite aquogel for preparing
The sorbing material of group, it is to the heavy metal ion (Cu with serious harm in aqueous systems2+、Ni2+、Cd2+、Pb2+) adsorption effect
It is fabulous.And gel process for preparing is simple, still there is certain mechanical strength after gel water suction, can be used repeatedly, it is right
Heavy metal ion in industrial wastewater, sanitary sewage and natural water is respectively provided with good adsorption effect.
Brief description of the drawings
Fig. 1 is the polymer-modified environmentally friendly composite aquogel of the preparation of the embodiment of the present invention 1 to 200ppm Cu2+The suction of solution
Attached capacity and resolution factor figure；
Fig. 2 is the polymer-modified environmentally friendly composite aquogel of the preparation of the embodiment of the present invention 1 to 200ppm Ni2+The suction of solution
Attached capacity and resolution factor figure；
Fig. 3 is the polymer-modified environmentally friendly composite aquogel of the preparation of the embodiment of the present invention 1 to 200ppm Cd2+The suction of solution
Attached capacity and resolution factor figure；
Fig. 4 is the polymer-modified environmentally friendly composite aquogel of the preparation of the embodiment of the present invention 1 to 200ppm Pb2+The suction of solution
Attached capacity and resolution factor figure.
Specific embodiment
Embodiment 1：
1. 15g old and useless cottons are weighed, is added in the single port bottle containing 1L, 0.5M hydrochloric acid, 90 DEG C of water-baths, mechanical agitation 3
Hour, filtering is washed with water and is precipitated to neutrality, and is dried at 50 DEG C, and size-reduced machine crushes the white environment-protection fiber for obtaining 13g
Plain powder.
2. 22.5g acrylic acid and 7.5g acrylamides are weighed, 90mL water dissolves are added；
3. 9g NaOH is weighed, is dissolved in the distilled water of 10mL, be slowly dropped to after NaOH is completely dissolved
In the solution of step 2；
4. 0.3g shitosans are weighed, is placed in the solution of step 3, stirring to whole dissolvings；
5. to PVA-1799 (one kind in polyvinyl alcohol) aqueous solution that addition mass fraction in the solution of step 4 is 15%
Environment-protection fiber element powder prepared by 90g and 6g steps 1, starts mechanical agitation, stirs uniform to system；
6. to the ammonium persulfate that 0.09g is added in the solution obtained in step 5, N ' the N- methylene bisacrylamide acyls of 0.3g
Amine, the tetramethylethylenediamine of 0.3g, is again started up mechanical agitation, all materials is dispersed in system.
7. the material that step 6 is obtained is statically placed under room temperature environment, resting step treats its polymerization forming after 4 hours, obtain
Condensate；
8. the condensate for step 7 being obtained takes out, and cuts 3 × 3mm fritters, and further polymerization 6 is small in 80 DEG C of baking ovens to make it
When, obtain plural gel fritter.
9. it is small that the plural gel fritter for step 8 being obtained is immersed in the glutaraldehyde water solution that mass fraction is 0.5% 12
When, make shitosan fully crosslinked with glutaraldehyde；Then plural gel fritter is placed in container, it is small with soaked in absolute ethyl alcohol 24
When, unreacted monomer in gel piece is removed, with the multiple detergent gel block of distilled water, and dried at 50 DEG C, finally treat that it is inhaled
Polymer-modified environmentally friendly composite aquogel 800g (every gram of gel water suction 20g) of the present invention is obtained after water saturation.
10. the polymer-modified environmentally friendly composite aquogel after the water suction saturation that 1g steps 9 are obtained is weighed respectively is placed in 4 three
In mouth bottle, the Cu of 25mL, 200ppm is then respectively adding2+、Ni2+、Cd2+、Pb2+(correspondence slaine is respectively CuSO to solution4·
5H2O、Ni(NO3)2·6H2O、Cd(NO3)2·4H2O、Pb(NO3)2), adjusted to pH=6, Jiang Sankou with the 0.1M NaOH aqueous solution
Bottle is placed under 25 DEG C of room temperature conditions, and staticaccelerator adsorption is determined before each heavy metal ion solution is adsorbed and after absorption respectively after 6 hours
Concentration, measuring instrument be EDX1800B type X fluorescence spectrometers.By the concentration difference of ion before and after absorption, this can be calculated
Adsorption capacity of the gel to different ions.It is computed, Cu of the gel to 200ppm2+、Ni2+、Cd2+、Pb2+The absorption of solution is held
The average value of amount can reach 127.7mg/g, 108.5mg/g, 88.9mg/g, 160.5mg/g, refer to Fig. 1~4.
Gel after adion is placed in desorption 30 minutes in 25mL, 1M hydrochloric acid by 11., determines stripping liquid concentration, is passed through
The ratio of the ion concentration difference before the ion concentration and gel adsorption of calculating desorbed solution and after absorption, can calculate the gel pair
The resolution factor of different ions.It is computed, the gel is to Cu2+、Ni2+、Cd2+、Pb2+The resolution factor of ion can reach more than 80%,
Refer to Fig. 1-4.
12. are placed in 30 minutes in 25mL, 0.5M sodium hydroxide solution the gel after parsing, are washed to neutrality, can carry out
Next adsorption experiment.
Claims (4)
1. a kind of polymer-modified environmentally friendly hydrogel, it is prepared by following steps：
1) take with long stapled material, be put in excessive 0.1~0.5M hydrochloric acid, in being stirred to white under 80~90 DEG C of water-baths
Floccule is produced, and is filtered, is washed to neutrality and dry, and environment-protection fiber element powder is obtained after crushing；
2) with acrylic acid and acrylamide as polymerized monomer, by polymerized monomer dissolving in deionized water, acrylic acid and acryloyl
Amine consumption and be 1 with the mass ratio of deionized water：2~4, acrylic acid is 2~5 with the mass ratio of acrylamide：1；
3) to step 2) add NaOH in the mixed solution that obtains, acrylic acid is neutralized, degree of neutralization (alkali of addition with
The mol ratio of acid) it is 0.7~0.8：1；
4) it is well mixed to the shitosan suddenly to addition polymerized monomer gross mass 0.5~2% in the mixed solution for 3) obtaining；
5) to step 4) polyvinyl alcohol water solution of 3~5 times of polymerized monomer gross mass, polyethylene are added in the mixed solution that obtains
In alcohol solution, the mass fraction of polyvinyl alcohol is 10~20%；The step of adding polymerized monomer gross mass 10~30% 1)
The environment-protection fiber element powder of preparation, mechanical agitation is uniform；
6) to step 5) ammonium persulfate of polymerized monomer gross mass 0.2%~0.3% is added in the mixed solution that obtains, polymerization is single
N ' the N- methylene-bisacrylamides of body gross mass 0.5~1%, the tetramethylethylenediamine of polymerized monomer gross mass 0.5~1%,
Mechanical agitation is uniform；
7) by step 6) solution that obtains is placed in and obtains condensate within static 4~5 hours at room temperature；
8) by step 7) condensate that obtains is placed in 70~90 DEG C of baking ovens further polymerisation 5~6 hours, obtains compound solidifying
Glue；
9) by step 8) immersion of the plural gel that obtains be mass fraction 0.3~0.8% glutaraldehyde water solution in 8~12h,
Make shitosan fully crosslinked with glutaraldehyde；Then by plural gel with soaked in absolute ethyl alcohol, unreacted monomer in gel is removed,
Again with the multiple detergent gel of distilled water, and dried under the conditions of 40~60 DEG C, finally absorb water saturation, polymer-modified so as to obtain
Environmentally friendly composite aquogel.
2. polymer-modified environmentally friendly hydrogel as claimed in claim 1 a kind of, it is characterised in that：Long stapled material is cotton
Flower, paper scrap, pieces of cloth or wood chip.
3. application of the polymer-modified environmentally friendly hydrogel described in claim 1 or 2 in heavy metal containing sewage is processed.
4. application of the polymer-modified environmentally friendly hydrogel as claimed in claim 3 in heavy metal containing sewage is processed, its feature exists
In：The ion of heavy metal is Cu2+、Ni2+、Cd2+Or Pb2+。
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445289A (en) * | 2017-08-22 | 2017-12-08 | 西安交通大学 | PVA/ chitosan sphere bio-carriers and preparation method thereof |
| CN107501384A (en) * | 2017-07-17 | 2017-12-22 | 长沙湘资生物科技有限公司 | Utilize the method for yellow ginger clean manufacturing Chinese yam saponin |
| CN107552008A (en) * | 2017-09-12 | 2018-01-09 | 齐鲁工业大学 | A kind of method of corn cob fiber element based aquagel absorption heavy metal ion |
| CN110485158A (en) * | 2019-08-06 | 2019-11-22 | 广东省资源综合利用研究所 | A kind of chelating agent and its preparation method and application |
| CN113372577A (en) * | 2021-06-01 | 2021-09-10 | 河南农业大学 | Modified biochar composite hydrogel, and preparation method and application thereof |
| CN114437379A (en) * | 2020-11-05 | 2022-05-06 | 中国石油化工股份有限公司 | Composite gel plugging agent system for fracture-cavity oil reservoir and preparation method thereof |
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| CN103769062A (en) * | 2014-02-27 | 2014-05-07 | 江南大学 | Functionalized polyvinyl alcohol hydrogel and preparation method thereof |
| CN104945639A (en) * | 2015-06-17 | 2015-09-30 | 华南理工大学 | Sulfur-containing modified chitosan containing aerogel as well as preparation method and application thereof |
| CN105903442A (en) * | 2016-05-10 | 2016-08-31 | 西北师范大学 | Preparation of polysaccharide-base hydrogel and application of polysaccharide-base hydrogel as adsorbent to waste water treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107501384A (en) * | 2017-07-17 | 2017-12-22 | 长沙湘资生物科技有限公司 | Utilize the method for yellow ginger clean manufacturing Chinese yam saponin |
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| CN107445289A (en) * | 2017-08-22 | 2017-12-08 | 西安交通大学 | PVA/ chitosan sphere bio-carriers and preparation method thereof |
| CN107445289B (en) * | 2017-08-22 | 2020-04-28 | 西安交通大学 | PVA/chitosan spherical biological carrier and preparation method thereof |
| CN107552008A (en) * | 2017-09-12 | 2018-01-09 | 齐鲁工业大学 | A kind of method of corn cob fiber element based aquagel absorption heavy metal ion |
| CN107552008B (en) * | 2017-09-12 | 2020-04-07 | 齐鲁工业大学 | Method for adsorbing heavy metal ions by corncob cellulose-based hydrogel |
| CN110485158A (en) * | 2019-08-06 | 2019-11-22 | 广东省资源综合利用研究所 | A kind of chelating agent and its preparation method and application |
| CN110485158B (en) * | 2019-08-06 | 2022-02-22 | 广东省资源综合利用研究所 | Chelating agent and preparation method and application thereof |
| CN114437379A (en) * | 2020-11-05 | 2022-05-06 | 中国石油化工股份有限公司 | Composite gel plugging agent system for fracture-cavity oil reservoir and preparation method thereof |
| CN114437379B (en) * | 2020-11-05 | 2023-07-28 | 中国石油化工股份有限公司 | Composite gel plugging agent system for fracture-cavity oil reservoir and preparation method thereof |
| CN113372577A (en) * | 2021-06-01 | 2021-09-10 | 河南农业大学 | Modified biochar composite hydrogel, and preparation method and application thereof |
| CN113372577B (en) * | 2021-06-01 | 2024-01-26 | 河南农业大学 | Modified biochar composite hydrogel, preparation method and application thereof |
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