CN104211856A - Preparation method of loess-based polyacrylamide adsorbent - Google Patents
Preparation method of loess-based polyacrylamide adsorbent Download PDFInfo
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- CN104211856A CN104211856A CN201410342949.XA CN201410342949A CN104211856A CN 104211856 A CN104211856 A CN 104211856A CN 201410342949 A CN201410342949 A CN 201410342949A CN 104211856 A CN104211856 A CN 104211856A
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Abstract
The invention discloses a preparation method of a loess-based polyacrylamide adsorbent and belongs to the technical field of wastewater treatment. In the invention, loess is employed as a base body, acrylamide is employed as a chelation-type functional monomer, N,N-methylene-bisacrylamide is employed as a crosslinking agent and ammonium persulfate is employed as an initiator. A co-polymerization reaction is carried out through an in-situ polymerization method. The loess-based polyacrylamide adsorbent is quite strong in chelating capability and adsorbing capability, has a quite good adsorption performance on Pb(II) and MB in wastewater and is very easy to precipitate and separate from water after being used for adsorbing heavy metal ions and cationic dyes, so that the loess-based polyacrylamide adsorbent has a significant application advantage in wasterwater treatment.
Description
Technical field
The invention belongs to technical field of waste water processing, relate to a kind of preparation of loess base adsorbent, particularly relate to a kind of loess base polyacrylamide amine absorber in preparation method.
Background technology
Along with the increase of world population, the quickening of urbanization process and developing rapidly of industrial or agricultural, various waste water, the sharp increase of waste quantity, the living environment of the severe contamination mankind, environment protection and environmental improvement problem more and more receive publicity.Many natural materialss have absorption, filtrations, separation, ion-exchange, the physical and chemical performance of the excellence such as catalysis because it has unique composition and constitutional features, and have good environment attribute, environmental pollution improvement has special effect.Loess is a kind of wide material sources, nontoxic, non-secondary pollution, Green Water process natural materials cheap and easy to get.Nearly 1,300 ten thousand square kilometres of the total area of whole world loess distribution, accounts for 1/10th of Global land area.In China, loess area about 640,000 square kilometres, and also loess landform is grown the most perfect in China, and scale is also grand.Loess being used for sewage disposal had both allowed natural materials obtain reasonable employment, solved again water environment pollution problem.
Patent of invention (ZL 201210011518.6) with vinylformic acid and β-hydroxyethyl methacrylate for function monomer, prepare loess based high molecular sorbent material (LS/PAAHM), its adsorption effect is good, but its preparation process is comparatively loaded down with trivial details, and after absorption not free settling be separated.
summary of the invention
The object of the invention is for problems of the prior art, a kind of preparation method of loess base polyacrylamide amine absorber is provided.
One, the preparation of loess base polyacrylamide amine absorber
In the aqueous dispersion of loess, adding acrylamide is polymerization single polymerization monomer, and N,N methylene bis acrylamide is linking agent, and ammonium persulphate is initiator, adopts situ aggregation method to carry out polyreaction, obtains loess base polyacrylamide amine absorber.Its concrete preparation technology is: be well-dispersed in by loess in water, adds polymerization single polymerization monomer acrylamide and linking agent, and heating makes it dissolve; Add initiator again, in 65 ~ 85 DEG C of isothermal reaction 2 ~ 4 h, obtain loess based polyalcohol; Finally loess based polyalcohol distilled water wash is removed unreacted monomer, then slough water wherein by washing with alcohol, dry, grinding, obtains loess base polyacrylamide amine absorber, is designated as LS/PAM.
The add-on of acrylamide is 1/5 ~ 1/2 of loess quality; The add-on of linking agent is 0.1 ~ 0.5% of loess quality; The add-on of initiator is loess quality 0.1 ~ 3%.
Two, structure, the morphology characterization of loess base polyacrylamide amine absorber
Below by the characterization method such as FT-IR, TG and sem analysis, the surface functional group type of loess base polyacrylamide amine absorber prepared by the present invention, structure and morphology are analyzed.
1, sem analysis
The loess that Fig. 1 (a) is amplification 5,000 times SEM figure.As can be seen from the figure, there is a lot of irregular small-particle on loess surface, and shape is different, and structure of loess more complicated is described.B SEM that () is the loess base polyacrylamide of amplification 80,000 times schemes.As can be seen from the figure, loess (i.e. LS/PAM) surface after acrylic amide modified is more uneven, forms one layer of polymeric film and is wrapped up by loess, loess surface crack is disappeared, and occurs laminated structure; And particles after polymerization shape has similarity.This is conducive to solution and penetrates in polymer network structure, is namely conducive to the absorption to metal ion and dyestuff.
2, FT-IR analyzes
Fig. 2 is the infrared spectrogram (FT-IR) of the loess base polyacrylamide (LS/PAM) prepared of the present invention and loess (LS).1037 cm in LS
-1near be the stretching vibration absorption peak of Si-O-Si, 538 cm
-1, 470 cm
-1near be the flexural vibration absorption peak of Si-O-Si, 1471 cm
-1for-CH
3stretching vibration absorption peak; 797 cm
-1for the charateristic avsorption band of quartz, and peak is comparatively strong, illustrates that unformed silicon oxide is more.Compared with LS, loess base polyacrylamide maintains the structure of loess substantially, at 3450 cm
-1there is the charateristic avsorption band of acid amides C=O in place, at 1685 cm
-1there is the stretching vibration of stronger-C=O in place, at 1645 cm
-1there is stronger-NH in place
2formation vibration, 3184 cm
-1for-NH
2charateristic avsorption band, this show polyacrylamide and loess compound success.
3, TG-DTA analyzes
Fig. 3 is the thermogram (TG-DTA) of loess base polyacrylamide amine absorber of the present invention and loess (LS).Can find out from TG curve, there is a little weightless district at 123 DEG C in LS, and this is losing due to free water and planar water.Substantially reach weightless balance at 550 DEG C, rate of weight loss is about 7%, mainly organic pyrolysis.Loess base polyacrylamide planar water 100 DEG C time removes, the pyrolysis of 300 DEG C of generation polymkeric substance, and 800 DEG C do not reach weightless balance yet, and rate of weight loss is about 30%.Illustrate that LS and PAM is approximately polymerized with mol ratio 4:1.Can find out from DTA curve, there is a little water endotherm(ic)peak at 40 DEG C in LS, have a unconspicuous exothermic peak at 350 DEG C, this is consistent with organic thermolysis.Loess base polyacrylamide amine absorber is in the endotherm(ic)peak of 50 DEG C of appearance one with the free water of LS overlap.
Three, the absorption property of loess base polyacrylamide
1, loess base polyacrylamide is to containing MB(methylene blue) absorption of simulated wastewater: getting containing MB is simulated wastewater 25 mL of 50 mg/L, pH=6 ~ 7.Add loess base polyacrylamide of the present invention (initial amount is 0.02 g/L) wherein, constant temperature oscillation mixed solution 10 min, leave standstill, centrifugal, supernatant liquor visible spectrophotometry measures the concentration of remaining MB, and calculating percent of decolourization can reach 98.4%, and loading capacity reaches as high as 127.6 mg/g.
2, loess base polyacrylamide is to the absorption of Pb (II): getting containing Pb (II) concentration is simulated wastewater 25 mL of 50 mg/L, pH=5.Add loess base polyacrylamide of the present invention agent (initial amount is 0.05 g/L) wherein, constant temperature oscillation mixed solution 20 min, leave standstill, suction filtration, filtrate is by the concentration of aas determination remaining plumbous (II), calculate Pb (II) clearance and can reach 98.5%, loading capacity reaches as high as 121.4 mg/g.
In sum, the present invention take loess as matrix, acrylamide is chelating type function monomer, situ aggregation method is adopted to carry out copolyreaction, the loess base polyacrylamide amine absorber of preparation has very strong sequestering power and adsorptive power, to the Pb (II) in waste water and MB, there is good absorption property, and be easy to after Adsorption of Heavy Metal Ions with cationic dyestuff from sedimentation water be separated, thus there is obvious application advantage in the treatment of waste water.
Accompanying drawing explanation
Fig. 1 is the SEM of loess base polyacrylamide amine absorber (LS/PAM) of the present invention and raw material loess (LS) thereof.
Fig. 2 is the FT-IR of loess base polyacrylamide amine absorber (LS/PAM) of the present invention and raw material loess (LS) thereof.
Fig. 3 is the TG-DTA of loess base polyacrylamide amine absorber (LS/PAM) of the present invention and raw material loess (LS) thereof.
Embodiment
Below by specific embodiment, the preparation of loess base polyacrylamide amine absorber of the present invention and heavy metal ion absorption property that is plumbous and methylene blue are described further.
Embodiment one
1, the preparation of loess base polyacrylamide amine absorber
In 250 mL three-necked flasks, add loess (LS) and the 30 mL distilled water of 12 g, mechanical stirring makes it be uniformly dispersed, then add the acrylamide (AM) of 4 g, 0.03g N,N methylene bis acrylamide (MBA), stir 30 min at normal temperatures after be warming up to 45 DEG C acrylamide dissolved; Add 0.06 g ammonium persulphate (APS), continue to be warming up to 75 DEG C and stir 1 h, obtain gelatinous solid polymkeric substance; By polymkeric substance distilled water wash 3 ~ 5 times, remove unreacted monomer, then with the water that washing with alcohol is sloughed wherein for 2 ~ 4 times, be cut into small pieces; Vacuum-drying, grind into powder, obtains 14.8 g loess base polyacrylamide amine absorbers.
2, absorption property measures
(1) to the absorption containing MB simulated wastewater: in waste water, MB concentration is 20 mg/L, pH=6 ~ 7; Adsorbent amount is 0.5 g/L, and after room temperature (25 DEG C) vibration absorption 10 min, percent of decolourization reaches 98.1%, and loading capacity is 61.4 mg/g.
(2) to the absorption containing Pb (II) simulated wastewater: [Pb (II)]: 50 mg/L; PH=5, adsorbent amount 0.1 g/L, room temperature (25 DEG C) vibration absorption vibration 30 min, Pb (II) clearance is 96.5%, and loading capacity reaches 48.2 mg/g.
Embodiment two
1, the preparation of loess base polyacrylamide amine absorber
In 250 mL three-necked flasks, add loess (LS) and the 30 mL distilled water of 8 g, mechanical stirring 30 min makes it be uniformly dispersed, then add the acrylamide (AM) of 4 g, 0.04 g N,N methylene bis acrylamide (MBA), stir 30 min at normal temperatures after be warming up to 45 DEG C acrylamide dissolved; Add 0.24 g ammonium persulphate (APS), continue to be warming up to 65 DEG C and continue stirring 2.5 h, obtain gelatinous solid polymkeric substance.Polymkeric substance distilled water wash 3 ~ 5 times to remove unreacted monomer, then with the water that washing with alcohol is sloughed in gel for 2 ~ 4 times, is cut into small pieces, and vacuum-drying, grind into powder, obtains 10.7 g loess base polyacrylamide amine absorbers.
2, absorption property measures
Experiment condition is with embodiment one.The percent of decolourization of MB reaches 94.1%, and loading capacity is 72.9 mg/g.Pb (II) clearance reaches 94.9%, and loading capacity is 42.3 mg/g.
Embodiment three
1, the preparation of loess base polyacrylamide amine absorber
In 250 mL three-necked flasks, add loess (LS) and the 30 mL distilled water of 16 g, mechanical stirring 30 min makes it be uniformly dispersed, then add the acrylamide (AM) of 4 g, 0.064 g N,N methylene bis acrylamide (MBA), stir 30 min at normal temperatures after be warming up to 45 DEG C acrylamide dissolved; Add 0.16 g ammonium persulphate (APS), continue to be warming up to 85 DEG C, stir 3 h, obtain gelatinous solid polymkeric substance; Polymkeric substance distilled water wash 3 ~ 5 times to remove unreacted monomer, then with the water that washing with alcohol is sloughed wherein for 2 ~ 4 times, is cut into small pieces, and vacuum-drying, grind into powder, obtains 18.1 g loess base polyacrylamide amine absorbers.
2, the mensuration of absorption property
Experiment condition is with embodiment one.The percent of decolourization of MB reaches 97.4%, and loading capacity is 127.6 mg/g.Pb (II) clearance reaches 93.2%, and loading capacity is 119.7 mg/g.
Embodiment four
1, the preparation of loess base polyacrylamide amine absorber
In 250 mL three-necked flasks, add loess (LS) and the 30 mL distilled water of 12 g, mechanical stirring 30 min makes it be uniformly dispersed, then add the acrylamide (AM) of 4 g, 0.01 g N,N methylene bis acrylamide (MBA), stir 30 min at normal temperatures after be warming up to 45 DEG C acrylamide dissolved; Add 0.24 g ammonium persulphate (APS), continue to be warming up to 75 DEG C, stir 4 h, obtain gelatinous solid polymkeric substance; Polymkeric substance distilled water wash 3 ~ 5 times to remove unreacted monomer, then with the water that washing with alcohol is sloughed wherein for 2 ~ 4 times, is cut into small pieces, and vacuum-drying, grind into powder, obtains 15.1 g loess base polyacrylamide amine absorbers.
2, the mensuration of absorption property
Experiment condition is with embodiment one.The percent of decolourization of MB reaches 93.2%, and loading capacity is 105.4 mg/g.Pb (II) clearance reaches 92.6%, and loading capacity is 98.9 mg/g.
Loess in the various embodiments described above all selects Longnan of Gansu Province loess.Other reagent obtains by market is bought.
Claims (5)
1. the preparation method of loess base polyacrylamide amine absorber is in the aqueous dispersion of loess, and adding acrylamide is polymerization single polymerization monomer, and N,N methylene bis acrylamide is linking agent, and ammonium persulphate is initiator, adopts situ aggregation method carry out polyreaction and obtain.
2. the preparation method of loess base polyacrylamide amine absorber as claimed in claim 1, is characterized in that: be well-dispersed in by loess in water, adds polymerization single polymerization monomer acrylamide and linking agent, and heating makes it dissolve; Add initiator again, in 65 ~ 85 DEG C of isothermal reaction 2 ~ 4 h, obtain loess based polyalcohol; Loess based polyalcohol distilled water wash removes unreacted monomer, then sloughs water wherein by washing with alcohol, dry, and grinding, obtains loess base polyacrylamide amine absorber.
3. the preparation method of loess base polyacrylamide amine absorber as claimed in claim 1 or 2, is characterized in that: the add-on of polymerization single polymerization monomer acrylamide is 1/5 ~ 1/2 of loess quality.
4. the preparation method of loess base polyacrylamide amine absorber as claimed in claim 1 or 2, is characterized in that: the add-on of linking agent N,N methylene bis acrylamide is 0.1 ~ 0.5% of loess quality.
5. the preparation method of loess base polyacrylamide amine absorber as claimed in claim 1 or 2, is characterized in that: the add-on of initiator ammonium persulfate is loess quality 0.1 ~ 3%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170120A (en) * | 2015-09-30 | 2015-12-23 | 西北师范大学 | Method for preparing functional loess-based adsorbent through surface graft polymerization |
| CN106117471A (en) * | 2016-07-01 | 2016-11-16 | 西北师范大学 | A kind of preparation of the loess grafted propylene acid copolymer adsorbent for Adsorption of Heavy Metal Ions |
| CN106905496A (en) * | 2017-03-18 | 2017-06-30 | 西北师范大学 | A kind of loess particle graft copolymer adsorbent and preparation method thereof |
| CN109603775A (en) * | 2018-11-30 | 2019-04-12 | 武汉理工大学 | A kind of carrying metal ion polyacrylamide magnetic bead and its preparation method and application |
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| KR100246004B1 (en) * | 1997-09-19 | 2000-03-15 | 김명곤 | Mortar containing loess, mineral or rocks |
| CN101914256A (en) * | 2010-08-06 | 2010-12-15 | 西北师范大学 | Method for preparing composite water-retaining agent by adopting plant straws |
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| KR100246004B1 (en) * | 1997-09-19 | 2000-03-15 | 김명곤 | Mortar containing loess, mineral or rocks |
| CN101914256A (en) * | 2010-08-06 | 2010-12-15 | 西北师范大学 | Method for preparing composite water-retaining agent by adopting plant straws |
| CN102580694A (en) * | 2012-01-13 | 2012-07-18 | 西北师范大学 | Method for preparing modified loess with high adsorption performance |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105170120A (en) * | 2015-09-30 | 2015-12-23 | 西北师范大学 | Method for preparing functional loess-based adsorbent through surface graft polymerization |
| CN106117471A (en) * | 2016-07-01 | 2016-11-16 | 西北师范大学 | A kind of preparation of the loess grafted propylene acid copolymer adsorbent for Adsorption of Heavy Metal Ions |
| CN106905496A (en) * | 2017-03-18 | 2017-06-30 | 西北师范大学 | A kind of loess particle graft copolymer adsorbent and preparation method thereof |
| CN109603775A (en) * | 2018-11-30 | 2019-04-12 | 武汉理工大学 | A kind of carrying metal ion polyacrylamide magnetic bead and its preparation method and application |
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