CN103143330B - Functionalized polyvinyl alcohol adsorbent for managing heavy metal pollution in water and preparation method thereof - Google Patents
Functionalized polyvinyl alcohol adsorbent for managing heavy metal pollution in water and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a functionalized polyvinyl alcohol adsorbent for managing heavy metal pollution in water. The functionalized polyvinyl alcohol adsorbent is a polymer granule which is prepared from a polyvinyl alcohol-maleic anhydride polymer in modes of swelling and carbonization treatment, wherein the polyvinyl alcohol-maleic anhydride polymer is prepared from polyvinyl alcohol, maleic anhydride and butyl acetate as raw materials. The invention further discloses a preparation method of the functionalized polyvinyl alcohol adsorbent. The absorbing material disclosed by the invention is large in heavy metal absorption capacity, rapid in absorption speed, wide in application range, free of secondary pollution, simple in use method, remarkable in effect, safe and reliable, simple and convenient in preparation process, high in production efficiency and good in product quality, can be recycled and reused and can be produced in large scale.
Description
Technical field
The present invention relates to water body processing technology field, particularly relate to a kind of functionalized polyvinyl alcohol adsorbent and preparation method thereof administered Heavy Metals in Waters and pollute.
Background technology
The migration of heavy metal in water environment determines its existence form, enrichment situation and potential ecological hazard degree in water body.Heavy metal ion is with the form of solubilised state or particulate form by current mechanical handing, and this transition process obeys hydraulic principle.Heavy metal is realized migration and is transformed by series of physical chemical action (hydrolysis, oxidation, reduction, precipitation, dissolving, complexing, huge legendary turtle conjunction, suction-operated etc.) with simple ion, complex ion or shla molecule in the environment.In addition heavy metal can be passed through hydrolysis and generates hydroxide in water, also can generate sulfide or carbonate with corresponding anion.The solubility product of these compounds is all very little, easy generation sediment, the diffusion velocity of heavy metal contaminants in water body and scope are restricted, from the viewpoint of water self-cleaning, this is favourable, but plurality of heavy metal is deposited in water body deposit, likely again discharge when environmental condition changes, thus potential hazard is caused to water pollution.
Progressively go deep into research along with to the understanding of environmental problem, it is found that the change due to nature and human society factors, environmental quality presents " disturbance " phenomenon departing from stable state, i.e. so-called " transient state pollution " (transient pollution), Sudden Pollution Accident is wherein violent one, the disaster accident of domestic and international generation has shown to bring serious harm and loss to the Health and Living of people, especially sudden water pollution accident betides major river valley, has had a strong impact on production and the life of local resident.The modal heavy metal pollution of water body is cadmium, lead, nickel ion pollute, as 2009 occur in the lead contamination event of Fengxiang, China Shaanxi, Wugang, Hunan, and the cadmium pollution event of liuyang hunan; Guangxi in 2012 Longjiang cadmium pollution accident etc.These abrupt polluting accident give us the warning of many sternnesses from different visual angles: risk assessment and early warning, the ecology influence of carrying out sudden water pollution accident are assessed, emergency disposal, and from the generation of prevention of water contamination accident source, be that we tackle the top priority of sudden water pollution event at present.
Generally, water pollution accident occur after, can make full use of receiving water body from net capacity, pollutant is progressively diluted in migration, thus rely on water body self-purification ability pollutant is processed.But the self-purification capacity of water body is limited, in the face of some burst Pollution, the dilution of single dependence water body is produced effects very slow, needs to adopt manpower intervention to fall the oligosaprobic extent of injury and scope.At present, answer heavy metal current water contamination accident, the most frequently used emergency plan of prior art is " alkalescent chemical precipitation meet an urgent need scrubbing technology ", it is the amplification of water factory's water purification technology, mode of operation first throws in alkali and flocculant (poly-aluminium, Polyferric Sulfate) in a large number, when heavy metal concentration drops to water transfer dilution again to a certain degree.Although the method can separate the matter of great urgency, but the final result of process is heavy metal along with flocculant enters Sediments jointly, cause bed mud content of beary metal too high, if content of beary metal is higher than stripping threshold value in bed mud, or flocculant depolymerization, weathering, transition, or water environment changes (under fierce disturbance, ionic strength increase, pH value degradation), these heavy metals jointly entering bed mud with flocculant can enter in water body again, thus cause the secondary pollution of water body.
For this reason, the feature easily stabilized according to the heavy metal in solution, also develops heavy metal stabilization treatment technology method, at present as chemical precipitation method, membrane separation process, biosorption process, electrolysis, ferrite process and Exchange Resin by Adsorption.But, due to easily by pH value change impact (when pH value is lower, heavy metal ion can again stripping and bring secondary pollution), heavy metal waste long term stabilization be realized and still require further study and explore.At present, absorption method is respond well containing heavy metal water body for process, key is to need to prepare that displacement volume is large, environment compatibility is superior, cost performance is high, be beneficial to the sorbent material of recovery, non-secondary pollution, thus effectively controls and prevent the pollution of heavy metal in water cadmium, lead, nickel ion.
At present, there is not yet about functionalized polyvinyl alcohol adsorbent is at the report administering current water heavy metal cadmium, lead, nickel ion pollution.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide that a kind of heavy metal adsorption capacity is large, adsorption rate is fast, recoverys can be utilized, the functionalized polyvinyl alcohol adsorbent of the improvement Heavy Metals in Waters pollution of applied widely, non-secondary pollution.Another object of the present invention is to the preparation method that above-mentioned functions polyvinyl alcohol adsorbent is provided.
Object of the present invention is achieved by the following technical programs:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute provided by the invention, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment.Further, in polymer beads of the present invention, the content of hydroxyl and carboxyl is respectively 0.5 ~ 1.5mmol/g, 0.3 ~ 1.0mmol/g.In such scheme, raw materials by weight portion polyvinyl alcohol of the present invention: maleic anhydride: butyl acetate=1 ~ 1.5: 1 ~ 2: 4 ~ 6.
Sorbent material of the present invention is the polymer that polyvinyl alcohol and maleic anhydride are cross-linked to form, after swelling and carbonization treatment, change the swelling behavior of the water-soluble of polyvinyl alcohol and intermediate product polyvinyl alcohol-maleic anhydride polymer, thus increase the adsorption capacity of material, improve the mechanics mechanical performance of material.And adsorbent contains a large amount of active function group-COOH ,-OH, thus improves the absorption property of material heavy metal, reduces the adsorptive selectivity of material heavy metal.
Another object of the present invention is achieved by the following technical programs:
The preparation method of the functionalized polyvinyl alcohol adsorbent that above-mentioned improvement Heavy Metals in Waters provided by the invention pollutes, comprises the following steps:
(1) polyvinyl alcohol by weight: maleic anhydride: butyl acetate=1 ~ 1.5: 1 ~ 2: 4 ~ 6 take mixing after, at 75 ~ 90 DEG C of temperature, react 3 ~ 6h, filter; Precipitation is poured in the NaOH ethanolic solution containing NaOH 3wt% and react 2 ~ 10min at 80 ~ 100 DEG C of temperature, filter; Polyvinyl alcohol-maleic anhydride polymer is obtained after washing of precipitate, drying;
(2) polyvinyl alcohol-maleic anhydride polymer is fully swollen in dichloroethanes;
(3) add the concentrated sulfuric acid in fluoropolymer resin after swelling and carry out carbonization treatment;
(4) resin that obtains after filtering is carried out wash, dry, obtain functionalized polyvinyl alcohol adsorbent.
Further, polyvinyl alcohol-maleic anhydride polymer in mass ratio in step of the present invention (2): dichloroethanes=1: 3 ~ 5, stirs swelling 4 ~ 15h.
Further, the fluoropolymer resin after swelling in mass ratio in step of the present invention (3): the concentrated sulfuric acid=1: 2 ~ 4, reacts 4 ~ 10h at 60 ~ 100 DEG C of temperature.
Further, resin described in step of the present invention (4), first with the dilute sulfuric acid drip washing that concentration reduces gradually, then with 3%HCl, deionized water, 3%NaOH, deionized water, 3%HCl alternately washing, is finally washed till neutrality by deionized water.
The present invention has following beneficial effect:
(1) adsorption capacity is large
Sorbent material of the present invention is through swelling treatment and surface has duct or crack, is conducive to the raising of physical absorption capacity; Meanwhile, also containing a large amount of active function group-COOH ,-OH, ion-exchange can be passed through, dipolar bond effect improves chemisorption capacity.
(2) rate of adsorption is fast, and adsorptive selectivity is low, applied widely
Adsorber material adsorbs speed of the present invention is fast, is conducive to carrying out the pollution control of heavy metal circulating water.The present invention is applicable in heavy metal, the repairing and treating of slightly polluted wastewater and current water, also has significant effect for the combined pollution caused by multiple toxic heavy metal elements such as cadmium, lead, nickel.
(3) non-toxic
Analyze through cytotoxicity experiment and small white mouse acute toxicity testing, the extract of sorbent material water of the present invention does not have bio-toxicity, application has security in water body treating aspect, new pollution can not be caused, be conducive to promoting the coordination of environment and'economy, stable, healthy, sustainable development.
(4) mechanics satisfactory mechanical property, water insoluble, recoverable
Sorbent material of the present invention can carry out absorption-desorption repeatedly, and keep larger adsorption capacity, reduce costs simultaneously further, the enriching and recovering of heavy metal has good effect, when carrying out circulating water Heavy Metal Pollution Control, achieve a heavy metal " to pick up " from circulating water, avoid secondary pollution.
(5) using method is simple, and successful, is conducive to large-scale promotion and application
Sorbent material of the present invention can obtain good effect when dosage is less, and cost is low, can not produce secondary pollution, is easy to be accepted by society, is conducive to large-scale promotion and application.
(6) preparation technology is easy, production efficiency is high, good product quality, is produced on a large scale.
Accompanying drawing explanation
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail:
Fig. 1 is transmission/scanning electron microscope (SEM) photograph (a, b: transmission electron microscope picture of embodiment of the present invention functionalized polyvinyl alcohol adsorbent; C, d: scanning electron microscope (SEM) photograph).
Detailed description of the invention
Embodiment one:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method is as follows:
(1) take maleic anhydride 40g to be dissolved in the butyl acetate of 180g, and at 90 DEG C of temperature, react 6h together with 30g polyvinyl alcohol is in flask, filter; Precipitation is poured into 300mL containing in the NaOH ethanolic solution of NaOH 3wt%, at 90 DEG C of temperature, react 3min, filter; Dry at 50 DEG C of temperature after precipitation absolute ethanol washing and obtain polyvinyl alcohol-maleic anhydride polymer;
(2) weighing polyvinyl alcohol-maleic anhydride polymer 50g, is placed in 150g dichloroethanes and stirs swelling 15h;
(3) add the 600g concentrated sulfuric acid in fluoropolymer resin after swelling, at 90 DEG C of temperature, react 6h carry out carbonization treatment;
(4) resin obtained after filtering is first with the dilute sulfuric acid drip washing that concentration reduces gradually, then with 3%HCl, deionized water, 3%NaOH, deionized water, 3%HCl alternately washing, finally be washed till neutrality by deionized water, dry after filtering, obtain functionalized polyvinyl alcohol adsorbent.
In the present embodiment functionalized polyvinyl alcohol adsorbent, the content of hydroxyl and carboxyl is respectively 0.7932mmol/g and 0.9003mmol/g.
Embodiment two:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method and embodiment one difference are:
The consumption of step (1) maleic anhydride is 60g.
In the functionalized polyvinyl alcohol adsorbent obtained, the content of hydroxyl and carboxyl is respectively 0.6595mmol/g and 0.9590mmol/g.
Embodiment three:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method and embodiment one difference are:
The consumption of step (1) maleic anhydride is 30g.
In the functionalized polyvinyl alcohol adsorbent obtained, the content of hydroxyl and carboxyl is respectively 1.4790mmol/g and 0.4022mmol/g.
Embodiment four:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method and embodiment one difference are:
The consumption of step (1) polyvinyl alcohol is 60g.
Step (1) precipitation is 10min with the reaction time of NaOH ethanolic solution.
In the functionalized polyvinyl alcohol adsorbent obtained, the content of hydroxyl and carboxyl is respectively 0.8562mmol/g and 0.8591mmol/g.
Embodiment five:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method and embodiment one difference are:
The consumption of step (1) butyl acetate is 150g.
Step (2) weighing polyvinyl alcohol-maleic anhydride polymer 40g, is placed in 160g dichloroethanes and stirs swelling 8h.
In the functionalized polyvinyl alcohol adsorbent obtained, the content of hydroxyl and carboxyl is respectively 0.8056mmol/g and 0.9839mmol/g.
Embodiment six:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method and embodiment one difference are:
Step (1) maleic anhydride is dissolved in butyl acetate and at 80 DEG C of temperature, reacts 4h with polyvinyl alcohol.
The 400g concentrated sulfuric acid is added in step (3) fluoropolymer resin after swelling.
In the functionalized polyvinyl alcohol adsorbent obtained, the content of hydroxyl and carboxyl is respectively 0.8436mmol/g and 0.8119mmol/g.
Embodiment seven:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method and embodiment one difference are:
The 800g concentrated sulfuric acid is added in step (3) fluoropolymer resin after swelling.
In the functionalized polyvinyl alcohol adsorbent obtained, the content of hydroxyl and carboxyl is respectively 0.8001mmol/g and 0.9013mmol/g.
Embodiment eight:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method and embodiment one difference are:
Fluoropolymer resin after step (3) is swelling and the concentrated sulfuric acid react 3h at 100 DEG C of temperature.
In the functionalized polyvinyl alcohol adsorbent obtained, the content of hydroxyl and carboxyl is respectively 0.8023mmol/g and 0.9002mmol/g.
Embodiment nine:
A kind of functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute of the present embodiment, for the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after swelling, carbonization treatment, its preparation method and embodiment one difference are:
Fluoropolymer resin after step (3) is swelling and the concentrated sulfuric acid react 10h at 60 DEG C of temperature.
In the functionalized polyvinyl alcohol adsorbent obtained, the content of hydroxyl and carboxyl is respectively 0.7986mmol/g and 0.9095mmol/g.
The above embodiment of the present invention, visible by Fig. 1 (a, b, c, d), under high-resolution-ration transmission electric-lens, obviously can find out the structure of functionalized polyvinyl alcohol adsorbent.Obviously can see that adsorbent surface has a lot of gap and duct from the scanning electron microscope (SEM) photograph of functionalized polyvinyl alcohol adsorbent, and cut open from stratiform section on, obviously can observe adsorbent and have a lot of recessed nest, thus increase specific area, increase physical absorption capacity.
The Performance Detection situation of the above embodiment of the present invention functionalized polyvinyl alcohol adsorbent is as follows:
(1) saturated extent of adsorption
Detect through Static Adsorption, according to langmuir models fitting, adsorbent is to Cd
2+, Pb
2+, Ni
2+saturated extent of adsorption reach 134.89mg/g, 308.19mg/g, 100.95mg/g respectively.
(2) regeneration is resolved
Use 3%(volume ratio) aqueous solution of nitric acid (solid-to-liquid ratio is 1:250) resolve, filter, be washed till neutrality with distilled water, dry recycle.In the process of continuous 6 absorption-parsings, the surperficial duct of adsorbent or crack are increased, and improve physical absorption amount, and adsorbance slowly rises and tends towards stability, and it is to Cd
2+adsorbance bring up to 158.72mg/g by 134.89mg/g, to Pb
2+adsorbance bring up to 399.90mg/g by 308.19mg/g, to Ni
2+adsorbance bring up to 112.88mg/g by 100.95mg/g; The desorption rate of adsorbent keeps stable and is greater than 90%, shows good desorption performance.This characteristic of adsorbent makes to reduce costs further recovery enriching heavy metal simultaneously becomes possibility, when carrying out circulating water Heavy Metal Pollution Control, achieving a heavy metal and " picking up " from circulating water, avoiding secondary pollution.
(3) rate of adsorption
Employing static adsorptive method detects, and takes the adsorbent of some parts of 0.200g, when pH=5, measures the Cd that 50mL concentration is respectively 400mg/L
2+rong Ye ∕ Pb
2+rong Ye ∕ Ni
2+solution, after 2min, to Cd
2+, Pb
2+, Ni
2+clearance reach 67.95%, 60.28%, 65.71% respectively; Reach balance gradually after 20 min, to Cd
2+, Pb
2+, Ni
2+clearance reach 97.91%, 99.98%, 97.76% respectively.The rate of adsorption is fast, is conducive to carrying out the pollution control of heavy metal circulating water.
On the other hand, to the heavy metal of low concentration, also there is excellent adsorption effect.Detect through Static Adsorption, these some parts of 0.200g adsorbents taken, when pH=5, measure the Cd that 50mL concentration is respectively 5ug/L
2+rong Ye ∕ Pb
2+rong Ye ∕ Ni
2+solution, absorption 30min reaches adsorption equilibrium, records remaining Cd
2+, Pb
2+, Ni
2+concentration is respectively 0.0296ug/L, 0.779ug/L, 0.0605ug/L, and clearance is respectively 99.41%, 84.42%, 98.79%.
(4) oxicity analysis
Oxicity analysis comprises cytotoxicity and animal toxicity experiment.Adsorbent use water concussion lixiviate 5 days, 1g sample leachate contains the extract of 1g given the test agent.Cell experiment finds that concentration is the extract of the every 100mL nutrient solution of 8%(containing 8g sample) and following, the activity of sample on K562 cell, human umbilical cord mesenchymal stem cells and human liver cell affects without conspicuousness; Acute toxicity zoopery take mouse as reference, and mouse stomach amount is 0.2g.10g
-1body weight, is equivalent to 20,000mg.kg
-1, have no dead, then LD
50> 15,000mg.kg
-1, tested sample reaches 1 grade, actual non-toxic.Illustrate that this materials application has security in water body treating aspect, new pollution can not be caused.Carry out environmental safety evaluation to using material and be conducive to promoting the coordination of environment and'economy, stable, healthy, sustainable development.
Claims (6)
1. the functionalized polyvinyl alcohol adsorbent administered Heavy Metals in Waters and pollute, it is characterized in that: be the polyvinyl alcohol-maleic anhydride polymer prepared for raw material with polyvinyl alcohol, maleic anhydride, butyl acetate, the polymer beads obtained after, concentrated sulfuric acid carbonization treatment swelling through dichloroethanes; In described polymer beads, the content of hydroxyl and carboxyl is respectively 0.5 ~ 1.5mmol/g, 0.3 ~ 1.0mmol/g.
2. the functionalized polyvinyl alcohol adsorbent of improvement Heavy Metals in Waters pollution according to claim 1, is characterized in that: described raw materials by weight portion polyvinyl alcohol: maleic anhydride: butyl acetate=1 ~ 1.5: 1 ~ 2: 4 ~ 6.
3. the preparation method of the functionalized polyvinyl alcohol adsorbent of the described improvement Heavy Metals in Waters pollution of one of claim 1-2, is characterized in that comprising the following steps:
(1) polyvinyl alcohol by weight: maleic anhydride: butyl acetate=1 ~ 1.5: 1 ~ 2: 4 ~ 6 take mixing after, at 75 ~ 90 DEG C of temperature, react 3 ~ 6h, filter; Precipitation is poured in the NaOH ethanolic solution containing NaOH 3wt% and react 2 ~ 10min at 80 ~ 100 DEG C of temperature, filter; Polyvinyl alcohol-maleic anhydride polymer is obtained after washing of precipitate, drying;
(2) polyvinyl alcohol-maleic anhydride polymer is fully swollen in dichloroethanes;
(3) add the concentrated sulfuric acid in fluoropolymer resin after swelling and carry out carbonization treatment;
(4) resin that obtains after filtering is carried out wash, dry, obtain functionalized polyvinyl alcohol adsorbent.
4. the preparation method of the functionalized polyvinyl alcohol adsorbent of improvement Heavy Metals in Waters pollution according to claim 3, it is characterized in that: polyvinyl alcohol-maleic anhydride polymer in mass ratio in described step (2): dichloroethanes=1: 3 ~ 5, stir swelling 4 ~ 15h.
5. the preparation method of the functionalized polyvinyl alcohol adsorbent of improvement Heavy Metals in Waters pollution according to claim 3, it is characterized in that: the fluoropolymer resin after swelling in mass ratio in described step (3): the concentrated sulfuric acid=1: 2 ~ 4, at 60 ~ 100 DEG C of temperature, react 4 ~ 10h.
6. the preparation method of the functionalized polyvinyl alcohol adsorbent of improvement Heavy Metals in Waters pollution according to claim 3, it is characterized in that: resin described in described step (4) is first with the dilute sulfuric acid drip washing that concentration reduces gradually, then with 3%HCl, deionized water, 3%NaOH, deionized water, 3%HCl alternately washing, finally neutrality is washed till by deionized water.
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| CN104069782B (en) * | 2014-06-20 | 2016-05-25 | 河海大学 | A kind of preparation method of functionalized polyvinyl alcohol microballoon and application |
| CN105304864A (en) * | 2014-07-15 | 2016-02-03 | 北京当升材料科技股份有限公司 | Preparation and treatment method for low-sulfur manganese cobalt nickel hydroxide |
| CN111359581B (en) * | 2020-02-19 | 2021-08-17 | 东华大学 | Method for preparing heavy metal adsorbent by using waste polyvinyl chloride plastic |
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