CN105561933A - Preparation method of modified magnetic hydrogel heavy metal ion adsorbent - Google Patents
Preparation method of modified magnetic hydrogel heavy metal ion adsorbent Download PDFInfo
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Abstract
The invention relates to a preparation method of a modified magnetic hydrogel heavy metal ion adsorbent, belonging to the adsorbent preparation field. A magnetic heavy metal ion adsorbent prepared by purified lignosulfonate modified hydrogel and ferric salt through compounding is provided. According to the prepared adsorbent, the physical crosslinking property of the modified lignosulfonate is used to replace the use of a chemical crosslinking agent, the phenolic hydroxyl group, the carboxyl group and the sulfonic acid group of the lignosulfonate also can improve the water swelling property of hydrogel and thus the adsorptive property of the material is improved; and the adsorbent can be recovered conveniently due to existence of magnetic iron, and thus secondary pollution is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of modified magnetic hydrogel adsorbent for heavy metal, belong to absorbent preparation field.
Background technology
Lignosulfonates are one of topmost accessory substances of paper industry, only China just has millions of tons lignosulfonates to produce every year, a little part is only had to be utilized at present, therefore, active development lignin sulfonic acid product salt, constantly widen its range of application, be both conducive to environmental protection, be also conducive to the utilization of resource.Macromolecule hydrogel is that a class can be swelling in water, but water insoluble, and have the functional material of three-dimensional netted molecular structure, macromolecule hydrogel has important application in agricultural, building industry, pharmaceuticals industry, biotechnology etc.Macromolecule hydrogel is by sources divided into synthesis macromolecule hydrogel and natural polymer hydrogel; the raw material manufacturing synthesis macromolecule hydrogel is mainly derived from petroleum industry; non-renewable resources; and the biodegradability of this kind of hydrogel is mostly poor; at scarcity of resources; today that environmental protection is extremely urgent, the R&D work of natural polymer hydrogel has long-range strategic importance.Lignosulfonates have tridimensional network, and being rich in the hydrophilic radicals such as hydroxyl, carboxyl, sulfonic group in molecule, is a kind of raw material preparing hydrogel preferably in theory.
No matter be traditional sorbing material (such as active carbon, zeolite molecular sieve, resin), still the novel absorption material hydrogel received much concern in recent years, all faces same problem, exactly after absorption completes, how to reclaim from environment and be separated these materials, reduce the secondary pollution to environment.This problem is solved well to the research of magnetic adsorptive material.According to the preparation method of magnetic material, roughly can be divided three classes.One class is shitosan, alginic acid, PEF acids etc. by the modified compound modifying certain specific functional group upper conventional to magnetic-particle modifying surface; Also have with magnetic-particle be core or with it for shell, combine with organic polymer (as osmanthus glue, hydrogel) magnetic material forming a kind of nucleocapsid structure; The third is exactly with large pore material (as zeolite, multi-walled carbon nano-tubes) for patterned substrate, carried magnetic particle.
Summary of the invention
The technical problem that the present invention mainly solves: all will add chemical cross-linking agent in current conventional hydrogels preparation process, and the expensive price of crosslinking agent improves production cost virtually, and the adsorption effect of hydrogel adsorbent is excellent, but be difficult to be separated to obtain defect from pending pollutant after absorption, provide and a kind ofly utilize the lignin sulfonate modified hydrogel of purifying and the composite rear obtained magnetic adsorbent for heavy metal of molysite.The adsorbent that the present invention obtains utilizes the physical crosslinking of modified sodium lignosulfonate to instead of the use of chemical cross-linking agent, simultaneously sodium lignin sulfonate itself with phenolic hydroxyl group, carboxyl and sulfonic group also improve the water-swellable of hydrogel, improve the absorption property of material, and ferromagnetic existence makes the recovery of the present invention after being used to complete obtain splendid solution, decreases the generation of secondary pollution.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) taking 50 ~ 100g sodium lignin sulfonate pours in 1L beaker, add 500 ~ 600mL deionized water, be placed on magnetic stirrer, move into Buchner funnel after stirring 20 ~ 30min with the rotating speed of 300 ~ 400r/min and carry out suction filtration, obtain filtrate, in filtrate, continue dropping 20 ~ 30mL mass concentration is the sulfuric acid solution of 80%;
(2) pour in 200mL volumetric flask by dripping the mixed liquor after sulfuric acid, and connect condensation reflux unit, volumetric flask is moved in oil bath pan, be warming up to 100 ~ 120 DEG C, collect refluxer after backflow 1 ~ 2h, in condensate liquid, add 5 ~ 10g sodium chloride, until deposit-free is separated out, the sediment obtained saltouing carries out putting into baking oven dry 1 ~ 2h at 50 ~ 60 DEG C after suction filtration obtains solids, obtains desugar purifying sodium lignin sulfonate;
(3) get in the there-necked flask of 3 ~ 5mg polyacrylamide loading with agitator, dropping funel and thermometer, add 3 ~ 5g carboxymethyl cellulose, 1 ~ 3g agar and 2 ~ 4g collagen, in there-necked flask, add 200 ~ 300mL deionized water by dropping funel, start agitator and stir 10 ~ 20min with the rotating speed of 300 ~ 400r/min;
(4) take the above-mentioned obtained purifying sodium lignin sulfonate of 5 ~ 10g and put into 250mL beaker, add 150 ~ 200mL distilled water, after stirring with glass bar, add 10 ~ 15g sodium peroxydisulfate, continue stirring 5 ~ 10min, obtained modification liquid;
(5) in above-mentioned there-necked flask, nitrogen is passed into the speed of 10mL/min, remove air in bottle, oil bath is warming up to 70 ~ 80 DEG C, start agitator while stirring above-mentioned obtained modification liquid dropwise to be instilled in flask, control rate of addition to make to dropwise in its 10 ~ 20min, then add the sodium peroxide solid of mixed liquor gross mass 5 ~ 8%, arranging speed of agitator is 900 ~ 1000r/min vigorous stirring, 30 ~ 40min, form a large amount of bubble, make hydrogel surface produce a large amount of evenly pore;
(6) in the there-necked flask of 1L, the above-mentioned obtained microporous of 200 ~ 300g is loaded, add 400 ~ 500mL distilled water, after passing into nitrogen 30 ~ 40min with the speed of 5mL/min in flask, add 2 ~ 3g ferrous sulfate and 1 ~ 3g iron chloride powder more wherein, start agitator and stir 1 ~ 2h with the rotating speed of 300 ~ 400r/min, put into sonic oscillation instrument ultrasonic reaction 20 ~ 30min again, adding 10 ~ 20mL mass concentration is that the ammoniacal liquor of 5% is until mixture pH is 7 ~ 8, move into water-bath, be heated to 60 ~ 70 DEG C, after insulation reaction 3 ~ 4h, filter to obtain filter residue, at 40 ~ 50 DEG C, a kind of modified magnetic hydrogel adsorbent for heavy metal is drying to obtain with vacuum desiccator.
Embody rule method of the present invention: get the modified magnetic hydrogel adsorbent for heavy metal that the present invention obtains, be 10 ~ 15g/L to containing the adsorbent adding the present invention in the wastewater disposal basin of heavy metal cadmium ion and obtain by dosage, afterwards aeration absorption 10 ~ 12h is carried out to pending wastewater disposal basin, around pond, uniform magnetic field is applied after absorption terminates, under the effect of magnetic force, collect the adsorbent after having adsorbed, with flame atomic absorption spectrometry adsorbent, 80 ~ 90% are reached to metal biosorption rate, there is splendid adsorption effect.
Beneficial effect of the present invention: the adsorbent that the present invention obtains utilizes the physical crosslinking of modified sodium lignosulfonate to instead of the use of chemical cross-linking agent, simultaneously sodium lignin sulfonate itself with phenolic hydroxyl group, carboxyl and sulfonic group also improve the water-swellable of hydrogel, improve the absorption property of material, and ferromagnetic existence makes the recovery of the present invention after being used to complete obtain splendid solution, decreases the generation of secondary pollution.
Detailed description of the invention
Taking 50 ~ 100g sodium lignin sulfonate pours in 1L beaker, add 500 ~ 600mL deionized water, be placed on magnetic stirrer, move into Buchner funnel after stirring 20 ~ 30min with the rotating speed of 300 ~ 400r/min and carry out suction filtration, obtain filtrate, in filtrate, continue dropping 20 ~ 30mL mass concentration is the sulfuric acid solution of 80%, pour in 200mL volumetric flask by dripping the mixed liquor after sulfuric acid, and connect condensation reflux unit, volumetric flask is moved in oil bath pan, be warming up to 100 ~ 120 DEG C, collect refluxer after backflow 1 ~ 2h, in condensate liquid, add 5 ~ 10g sodium chloride, until deposit-free is separated out, the sediment obtained saltouing carries out putting into baking oven dry 1 ~ 2h at 50 ~ 60 DEG C after suction filtration obtains solids, obtains desugar purifying sodium lignin sulfonate, get in the there-necked flask of 3 ~ 5mg polyacrylamide loading with agitator, dropping funel and thermometer, add 3 ~ 5g carboxymethyl cellulose, 1 ~ 3g agar and 2 ~ 4g collagen, in there-necked flask, add 200 ~ 300mL deionized water by dropping funel, start agitator and stir 10 ~ 20min with the rotating speed of 300 ~ 400r/min, take the above-mentioned obtained purifying sodium lignin sulfonate of 5 ~ 10g and put into 250mL beaker, add 150 ~ 200mL distilled water, after stirring with glass bar, add 10 ~ 15g sodium peroxydisulfate, continue stirring 5 ~ 10min, obtained modification liquid, nitrogen is passed into the speed of 10mL/min in above-mentioned there-necked flask, remove air in bottle, oil bath is warming up to 70 ~ 80 DEG C, start agitator while stirring above-mentioned obtained modification liquid dropwise to be instilled in flask, control rate of addition to make to dropwise in its 10 ~ 20min, then add the sodium peroxide solid of mixed liquor gross mass 5 ~ 8%, arranging speed of agitator is 900 ~ 1000r/min vigorous stirring, 30 ~ 40min, form a large amount of bubble, make hydrogel surface produce a large amount of evenly pore, the above-mentioned obtained microporous of 200 ~ 300g is loaded in the there-necked flask of 1L, add 400 ~ 500mL distilled water, after passing into nitrogen 30 ~ 40min with the speed of 5mL/min in flask, add 2 ~ 3g ferrous sulfate and 1 ~ 3g iron chloride powder more wherein, start agitator and stir 1 ~ 2h with the rotating speed of 300 ~ 400r/min, put into sonic oscillation instrument ultrasonic reaction 20 ~ 30min again, adding 10 ~ 20mL mass concentration is that the ammoniacal liquor of 5% is until mixture pH is 7 ~ 8, move into water-bath, be heated to 60 ~ 70 DEG C, after insulation reaction 3 ~ 4h, filter to obtain filter residue, at 40 ~ 50 DEG C, a kind of modified magnetic hydrogel adsorbent for heavy metal is drying to obtain with vacuum desiccator.
Example 1
Taking 50g sodium lignin sulfonate pours in 1L beaker, add 500mL deionized water, be placed on magnetic stirrer, move into Buchner funnel after stirring 20min with the rotating speed of 300r/min and carry out suction filtration, obtain filtrate, continuing to drip 20mL mass concentration in filtrate is the sulfuric acid solution of 80%, pour in 200mL volumetric flask by dripping the mixed liquor after sulfuric acid, and connect condensation reflux unit, volumetric flask is moved in oil bath pan, be warming up to 100 DEG C, collect refluxer after backflow 1h, in condensate liquid, add 5g sodium chloride, until deposit-free is separated out, the sediment obtained saltouing carries out putting into baking oven dry 1h at 50 DEG C after suction filtration obtains solids, obtains desugar purifying sodium lignin sulfonate, get in the there-necked flask of 3mg polyacrylamide loading with agitator, dropping funel and thermometer, add 3g carboxymethyl cellulose, 1g agar and 2g collagen, in there-necked flask, add 200mL deionized water by dropping funel, start agitator and stir 10min with the rotating speed of 300r/min, take the above-mentioned obtained purifying sodium lignin sulfonate of 5g and put into 250mL beaker, add 150mL distilled water, after stirring with glass bar, add 10g sodium peroxydisulfate, continue to stir 5min, obtained modification liquid, nitrogen is passed into the speed of 10mL/min in above-mentioned there-necked flask, remove air in bottle, oil bath is warming up to 70 DEG C, start agitator while stirring above-mentioned obtained modification liquid dropwise to be instilled in flask, control rate of addition to make to dropwise in its 10min, then add the sodium peroxide solid of mixed liquor gross mass 5%, arranging speed of agitator is 900r/min vigorous stirring 30min, form a large amount of bubble, make hydrogel surface produce a large amount of evenly pore, the above-mentioned obtained microporous of 200g is loaded in the there-necked flask of 1L, add 400mL distilled water, after passing into nitrogen 30min with the speed of 5mL/min in flask, add 2g ferrous sulfate and 1g iron chloride powder more wherein, start agitator and stir 1h with the rotating speed of 300r/min, put into sonic oscillation instrument ultrasonic reaction 20min again, adding 10mL mass concentration is that the ammoniacal liquor of 5% is until mixture pH is 7, move into water-bath, be heated to 60 DEG C, after insulation reaction 3h, filter to obtain filter residue, at 40 DEG C, a kind of modified magnetic hydrogel adsorbent for heavy metal is drying to obtain with vacuum desiccator.
Embody rule method of the present invention: get the modified magnetic hydrogel adsorbent for heavy metal that the present invention obtains, be 10g/L to containing the adsorbent adding the present invention in the wastewater disposal basin of heavy metal cadmium ion and obtain by dosage, afterwards aeration absorption 10h is carried out to pending wastewater disposal basin, around pond, uniform magnetic field is applied after absorption terminates, under the effect of magnetic force, collect the adsorbent after having adsorbed, with flame atomic absorption spectrometry adsorbent, 80% is reached to metal biosorption rate, there is splendid adsorption effect.
Example 2
Taking 80g sodium lignin sulfonate pours in 1L beaker, add 550mL deionized water, be placed on magnetic stirrer, move into Buchner funnel after stirring 25min with the rotating speed of 350r/min and carry out suction filtration, obtain filtrate, continuing to drip 25mL mass concentration in filtrate is the sulfuric acid solution of 80%, pour in 200mL volumetric flask by dripping the mixed liquor after sulfuric acid, and connect condensation reflux unit, volumetric flask is moved in oil bath pan, be warming up to 110 DEG C, collect refluxer after backflow 1h, in condensate liquid, add 8g sodium chloride, until deposit-free is separated out, the sediment obtained saltouing carries out putting into baking oven dry 1h at 55 DEG C after suction filtration obtains solids, obtains desugar purifying sodium lignin sulfonate, get in the there-necked flask of 4mg polyacrylamide loading with agitator, dropping funel and thermometer, add 4g carboxymethyl cellulose, 2g agar and 3g collagen, in there-necked flask, add 250mL deionized water by dropping funel, start agitator and stir 15min with the rotating speed of 350r/min, take the above-mentioned obtained purifying sodium lignin sulfonate of 8g and put into 250mL beaker, add 180mL distilled water, after stirring with glass bar, add 13g sodium peroxydisulfate, continue to stir 8min, obtained modification liquid, nitrogen is passed into the speed of 10mL/min in above-mentioned there-necked flask, remove air in bottle, oil bath is warming up to 75 DEG C, start agitator while stirring above-mentioned obtained modification liquid dropwise to be instilled in flask, control rate of addition to make to dropwise in its 15min, then add the sodium peroxide solid of mixed liquor gross mass 7%, arranging speed of agitator is 950r/min vigorous stirring 35min, form a large amount of bubble, make hydrogel surface produce a large amount of evenly pore, the above-mentioned obtained microporous of 250g is loaded in the there-necked flask of 1L, add 450mL distilled water, after passing into nitrogen 35min with the speed of 5mL/min in flask, add 2g ferrous sulfate and 2g iron chloride powder more wherein, start agitator and stir 1h with the rotating speed of 350r/min, put into sonic oscillation instrument ultrasonic reaction 25min again, adding 15mL mass concentration is that the ammoniacal liquor of 5% is until mixture pH is 7, move into water-bath, be heated to 65 DEG C, after insulation reaction 3h, filter to obtain filter residue, at 45 DEG C, a kind of modified magnetic hydrogel adsorbent for heavy metal is drying to obtain with vacuum desiccator.
Embody rule method of the present invention: get the modified magnetic hydrogel adsorbent for heavy metal that the present invention obtains, be 13g/L to containing the adsorbent adding the present invention in the wastewater disposal basin of heavy metal cadmium ion and obtain by dosage, afterwards aeration absorption 11h is carried out to pending wastewater disposal basin, around pond, uniform magnetic field is applied after absorption terminates, under the effect of magnetic force, collect the adsorbent after having adsorbed, with flame atomic absorption spectrometry adsorbent, 85% is reached to metal biosorption rate, there is splendid adsorption effect.
Example 3
Taking 100g sodium lignin sulfonate pours in 1L beaker, add 600mL deionized water, be placed on magnetic stirrer, move into Buchner funnel after stirring 30min with the rotating speed of 400r/min and carry out suction filtration, obtain filtrate, continuing to drip 30mL mass concentration in filtrate is the sulfuric acid solution of 80%, pour in 200mL volumetric flask by dripping the mixed liquor after sulfuric acid, and connect condensation reflux unit, volumetric flask is moved in oil bath pan, be warming up to 120 DEG C, collect refluxer after backflow 2h, in condensate liquid, add 10g sodium chloride, until deposit-free is separated out, the sediment obtained saltouing carries out putting into baking oven dry 2h at 60 DEG C after suction filtration obtains solids, obtains desugar purifying sodium lignin sulfonate, get in the there-necked flask of 5mg polyacrylamide loading with agitator, dropping funel and thermometer, add 5g carboxymethyl cellulose, 3g agar and 4g collagen, in there-necked flask, add 300mL deionized water by dropping funel, start agitator and stir 20min with the rotating speed of 400r/min, take the above-mentioned obtained purifying sodium lignin sulfonate of 10g and put into 250mL beaker, add 200mL distilled water, after stirring with glass bar, add 15g sodium peroxydisulfate, continue to stir 10min, obtained modification liquid, nitrogen is passed into the speed of 10mL/min in above-mentioned there-necked flask, remove air in bottle, oil bath is warming up to 80 DEG C, start agitator while stirring above-mentioned obtained modification liquid dropwise to be instilled in flask, control rate of addition to make to dropwise in its 20min, then add the sodium peroxide solid of mixed liquor gross mass 8%, arranging speed of agitator is 1000r/min vigorous stirring 40min, form a large amount of bubble, make hydrogel surface produce a large amount of evenly pore, the above-mentioned obtained microporous of 300g is loaded in the there-necked flask of 1L, add 500mL distilled water, after passing into nitrogen 40min with the speed of 5mL/min in flask, add 3g ferrous sulfate and 3g iron chloride powder more wherein, start agitator and stir 2h with the rotating speed of 400r/min, put into sonic oscillation instrument ultrasonic reaction 30min again, adding 20mL mass concentration is that the ammoniacal liquor of 5% is until mixture pH is 8, move into water-bath, be heated to 70 DEG C, after insulation reaction 4h, filter to obtain filter residue, at 50 DEG C, a kind of modified magnetic hydrogel adsorbent for heavy metal is drying to obtain with vacuum desiccator.
Embody rule method of the present invention: get the modified magnetic hydrogel adsorbent for heavy metal that the present invention obtains, be 15g/L to containing the adsorbent adding the present invention in the wastewater disposal basin of heavy metal cadmium ion and obtain by dosage, afterwards aeration absorption 12h is carried out to pending wastewater disposal basin, around pond, uniform magnetic field is applied after absorption terminates, under the effect of magnetic force, collect the adsorbent after having adsorbed, with flame atomic absorption spectrometry adsorbent, 90% is reached to metal biosorption rate, there is splendid adsorption effect.
Claims (1)
1. a preparation method for modified magnetic hydrogel adsorbent for heavy metal, is characterized in that concrete preparation process is:
(1) taking 50 ~ 100g sodium lignin sulfonate pours in 1L beaker, add 500 ~ 600mL deionized water, be placed on magnetic stirrer, move into Buchner funnel after stirring 20 ~ 30min with the rotating speed of 300 ~ 400r/min and carry out suction filtration, obtain filtrate, in filtrate, continue dropping 20 ~ 30mL mass concentration is the sulfuric acid solution of 80%;
(2) pour in 2L volumetric flask by dripping the mixed liquor after sulfuric acid, and connect condensation reflux unit, volumetric flask is moved in oil bath pan, be warming up to 100 ~ 120 DEG C, collect refluxer after backflow 1 ~ 2h, in condensate liquid, add 5 ~ 10g sodium chloride, until deposit-free is separated out, the sediment obtained saltouing carries out putting into baking oven dry 1 ~ 2h at 50 ~ 60 DEG C after suction filtration obtains solids, obtains desugar purifying sodium lignin sulfonate;
(3) get in the there-necked flask of 3 ~ 5mg polyacrylamide loading with agitator, dropping funel and thermometer, add 3 ~ 5g carboxymethyl cellulose, 1 ~ 3g agar and 2 ~ 4g collagen, in there-necked flask, add 200 ~ 300mL deionized water by dropping funel, start agitator and stir 10 ~ 20min with the rotating speed of 300 ~ 400r/min;
(4) take the above-mentioned obtained purifying sodium lignin sulfonate of 5 ~ 10g and put into 250mL beaker, add 150 ~ 200mL distilled water, after stirring with glass bar, add 10 ~ 15g sodium peroxydisulfate, continue stirring 5 ~ 10min, obtained modification liquid;
(5) in above-mentioned there-necked flask, nitrogen is passed into the speed of 10mL/min, remove air in bottle, oil bath is warming up to 70 ~ 80 DEG C, start agitator while stirring above-mentioned obtained modification liquid dropwise to be instilled in flask, control rate of addition to make to dropwise in its 10 ~ 20min, then add the sodium peroxide solid of mixed liquor gross mass 5 ~ 8%, arranging speed of agitator is 900 ~ 1000r/min vigorous stirring, 30 ~ 40min, form a large amount of bubble, make hydrogel surface produce a large amount of evenly pore;
(6) in the there-necked flask of 1L, the above-mentioned obtained microporous of 200 ~ 300g is loaded, add 400 ~ 500mL distilled water, after passing into nitrogen 30 ~ 40min with the speed of 5mL/min in flask, add 2 ~ 3g ferrous sulfate and 1 ~ 3g iron chloride powder more wherein, start agitator and stir 1 ~ 2h with the rotating speed of 300 ~ 400r/min, put into sonic oscillation instrument ultrasonic reaction 20 ~ 30min again, adding 10 ~ 20mL mass concentration is that the ammoniacal liquor of 5% is until mixture pH is 7 ~ 8, move into water-bath, be heated to 60 ~ 70 DEG C, after insulation reaction 3 ~ 4h, filter to obtain filter residue, at 40 ~ 50 DEG C, a kind of modified magnetic hydrogel adsorbent for heavy metal is drying to obtain with vacuum desiccator.
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Cited By (6)
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| CN106220866A (en) * | 2016-07-28 | 2016-12-14 | 东北林业大学 | A kind of preparation method that copper ion is had high adsorption magnetic hydrogel |
| CN106861642A (en) * | 2017-02-14 | 2017-06-20 | 华南理工大学 | A kind of preparation and application of the biomass-based hydrogel with high absorption capacity |
| CN110433777A (en) * | 2018-05-03 | 2019-11-12 | 南京大学 | A kind of environmental sensitivity gel of crosslink metallic albumen and its application |
| CN112480983A (en) * | 2020-11-30 | 2021-03-12 | 青岛科技大学 | Method for promoting efficient generation of methane hydrate by sulfonic acid-based hydrogel |
| CN113072198A (en) * | 2021-04-25 | 2021-07-06 | 陕西科技大学 | Preparation method and application of ultralong sustained-release solid scale inhibitor |
| CN114133462A (en) * | 2021-12-16 | 2022-03-04 | 江苏暨之阳环保科技有限公司 | Heavy metal treatment agent for petroleum-polluted soil and preparation method thereof |
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| CN102391603A (en) * | 2011-07-22 | 2012-03-28 | 西安交通大学 | Preparation method of novel magnetism macromolecule hydrogel |
| WO2015068837A1 (en) * | 2013-11-11 | 2015-05-14 | 日産化学工業株式会社 | Hydrogel-forming composition and hydrogel made therefrom |
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