CN106925236B - A kind of gelatin-manganese dioxide composites preparation method and applications for adsorbing heavy metal - Google Patents
A kind of gelatin-manganese dioxide composites preparation method and applications for adsorbing heavy metal Download PDFInfo
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- CN106925236B CN106925236B CN201710190002.5A CN201710190002A CN106925236B CN 106925236 B CN106925236 B CN 106925236B CN 201710190002 A CN201710190002 A CN 201710190002A CN 106925236 B CN106925236 B CN 106925236B
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- gelatin
- manganese dioxide
- dioxide composites
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- manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0222—Compounds of Mn, Re
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The present invention provides a kind of gelatin-manganese dioxide composites preparation method and applications for adsorbing heavy metal.Gelatin-the manganese dioxide composites are after the manganese sulfate solution for being 1-50mmol/L by the aqueous gelatin solution and concentration of mass concentration≤10% is mixed according to the ratio that volume ratio is 6:1-10, potassium permanganate is added to stir evenly, potassium permanganate concentration is 5-30mmol/L in mixed solution after stirring, finally mixed solution is poured into ptfe autoclave, it is reacted 8-24 hours under 150-200 DEG C of hot conditions, obtain tan precipitate, and after being cleaned the tan precipitate of collection to unreacting reagent with clear water and completely removing repeatedly, drying obtains brown powder.Gelatin-manganese dioxide composites of the present invention are directly appended in leaded and cadmium sewage after oscillation absorption 4-10 hours, centrifugation removal gelatin-manganese dioxide composites, lead in sewage and cadmium are purified, good purification, can be used for efficient absorption/purification of lead and cadmium ion in environment.
Description
Technical field
The present invention relates to heavy metal adsorptions, and in particular to a kind of gelatin-manganese dioxide for lead, cadmium heavy metal ion is multiple
Close the preparation method and applications of adsorbent material.
Background technique
Heavy metal pollution is the serious problems of environmental pollution, and heavy metal pollution integrated control has become China's environmental improvement
Great demand.In numerous heavy metals, lead and cadmium have very strong bio-toxicity, and can be enriched with by food chain, to people
Class nervous system, digestive system, hematological system and endocrine system cause larger damage.
Currently, the minimizing technology of heavy metal in waste water mainly includes chemical precipitation method, ion-exchange, electrolysis method, film point
From method, absorption method etc..Chemical precipitation method and electrolysis method effluent quality are poor, easily cause secondary pollution；Ion-exchange and UF membrane
Method higher cost.Absorption method is one of removing heavy metals effect the best way, has easy, flexible, selection with other methods
The advantages that property is good.But conventional absorbtion material price is expensive, largely limits the extensive use of absorption method, therefore, exploitation
The adsorbent material of high efficiency low cost becomes firstly the need of solving the problems, such as.Mn oxide is cheap, resourceful, inhales with others
Enclosure material, which is compared, has biggish cost advantage.
Summary of the invention
For the problems of prior art, the present invention provides a kind of gelatin-manganese dioxide for adsorbing heavy metal is multiple
Object preparation method and applications are closed, the present invention is prepared using the manganese of gelatine reduction high-valence state can adsorb the bright of heavy metal ion
Glue-manganese dioxide composite material, due to the various active group and special construction of gelatin, this material shows lead, cadmium ion
Quickly absorption power and extremely strong adsorption capacity.
Technical solution provided by the invention: a kind of 1. gelatin-manganese dioxide composites preparation methods for adsorbing heavy metal,
It is characterized in that including the following steps:
(1) gelatin is added to the water, stand 30 minutes or more, it is then heated to 40-60 DEG C, is made it dissolve, matter is configured to
Measure the aqueous gelatin solution of concentration≤10%；
(2) manganese sulfate is dissolved in the water, ultrasonic disperse is uniform, and compound concentration is that the manganese sulfate of 1-50mmol/L is water-soluble
Liquid；
(3) it will be prepared in step (2) according to the ratio that the volume ratio of aqueous gelatin solution and manganese sulfate solution is 6:1-10
Manganese sulfate solution be added in the aqueous gelatin solution prepared in step (1), and potassium permanganate is added into mixed solution and stirs
It mixes uniformly, potassium permanganate concentration is 5-30mmol/L in mixed solution after stirring；
(4) mixed solution that step (3) obtains is poured into ptfe autoclave, in 150-200 DEG C of hot conditions
Lower reaction 8-24 hours obtains tan precipitate, and the tan precipitate of collection is cleaned with clear water repeatedly complete to unreacting reagent
After removal, drying obtains the i.e. described gelatin-manganese dioxide composites of brown powder.
The present invention preferably technical solution: the gelatin mass ratio in the step (1) in aqueous gelatin solution is 4-6%.
The present invention preferably technical solution: the supersonic frequency of ultrasonic disperse is 40KHz, jitter time in the step (2)
It is 10-30 minutes.
The present invention preferably technical solution: the concentration for the manganese sulfate solution prepared in the step (2) is 20-
The manganese sulfate solution of 30mmol/L.
The present invention preferably technical solution: the volume ratio of aqueous gelatin solution and manganese sulfate solution is 6:3- in step (3)
5, potassium permanganate concentration is 10-25mmol/L.
Gelatin-manganese dioxide composites application of a kind of above method preparation provided by the invention, it is characterised in that: will
Gelatin-manganese dioxide composites of preparation are directly appended in leaded and cadmium sewage after oscillation absorption 4-10 hours, and centrifugation is gone
Except gelatin-manganese dioxide composites, lead in sewage and cadmium are purified；Its gelatin-manganese dioxide composites additive amount is 5-
20g/20L sewage.
The present invention preferably technical solution: the gelatin-manganese dioxide composites are respectively to the adsorption capacity of lead, cadmium
165.7mg/g、155.8mg/g。
Due to Mn oxide large specific surface area, surface active groups are more, charge changeability is strong, have strongly to heavy metal
Chemical activity, and gelatin is rich in functional group abundant, wherein amino has reproducibility, and has water phase compatibility and green
Environmental protection characteristic, the present invention prepare the gelatin-manganese dioxide that can adsorb heavy metal ion using the manganese of gelatine reduction high-valence state
Composite material, compared with traditional Mn oxide, gelatin-manganese dioxide prepared by the present invention is rich in functional group (ammonia abundant
Base, carboxyl, imino group, sulfydryl, imidazoles etc.), there is water phase compatibility and environmentally protective characteristic, and prepare simply, it is at low cost
It is honest and clean, it can be used for efficient absorption/purification of lead and cadmium ion in environment.
Detailed description of the invention
Fig. 1, Fig. 2 are the scanning nuclear microprobe figures of gelatin-manganese dioxide composites of the present invention.
Fig. 3 is adsorption effect of the gelatin-manganese dioxide composites to lead, cadmium ion.
Fig. 4 is adsorption dynamics adsorption kinetics of the gelatin-manganese dioxide composites to lead, cadmium ion.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1, a kind of preparation of gelatin-manganese dioxide composites, the specific steps are as follows:
(1) 1.5g gelatin is impregnated 40 minutes in 30mL aqueous solution, is then heated to 50 DEG C and makes it dissolve, stirring makes it
It is uniformly dispersed, is configured to aqueous gelatin solution；
(2) 25mg manganese sulfate is dissolved in 25ml aqueous solution, disperses 10- under conditions of ultrasonic frequency is 40KHz
30 minutes, manganese sulfate solution was configured to until being uniformly dispersed；
(3) take the manganese sulfate for being added in the aqueous gelatin solution prepared in 30ml step (1) and preparing in 25ml step (2) molten
Liquid, and 158mg potassium permanganate is added, it stirs evenly, pours into ptfe autoclave, 160 DEG C are reacted 12 hours, are obtained brown
Color precipitating；And cleaned repeatedly with water, unreacted reagent is removed, and dry and obtain the i.e. described gelatin-manganese dioxide of brown powder
Compound.
Gelatin-the manganese dioxide composites prepared in embodiment 1 are passed through into scanning electron microscope transmissioning electric mirror test respectively, are swept
Electron microscope is retouched as shown in Figure 1, transmission electron microscope picture is as shown in Figure 2.Electromicroscopic photograph shows that gelatin-manganese dioxide particle is dumbbell shaped
Structure, is about 4 μm, about 2 μm wide；A large amount of fine particle is contained on dumbbell structure surface, illustrates that gelatin molecule is centered around dioxy
Change around manganese, forms adsorption site one by one.
Embodiment 2, a kind of preparation of gelatin-manganese dioxide composites, the specific steps are as follows:
(1) 0.3g gelatin is impregnated 50 minutes in 30mL aqueous solution, is then heated to 40 DEG C of dissolutions, stirring makes its dispersion
Uniformly, it is configured to aqueous gelatin solution；
(2) 4.23mg manganese sulfate is dissolved in 25ml aqueous solution, disperses 10 under conditions of ultrasonic frequency is 40KHz
Minute, manganese sulfate solution is configured to until being uniformly dispersed；
(3) manganese sulfate solution for being added in the aqueous gelatin solution prepared in 30ml step (1) and preparing in 5ml step (2) is taken,
And 27.7mg potassium permanganate is added, it stirs evenly, pours into ptfe autoclave, 150 DEG C are reacted 8 hours, and brown is obtained
Precipitating；And cleaned repeatedly with water, remove unreacted reagent, and dry that obtain the i.e. described gelatin-manganese dioxide of brown powder multiple
Close object.
Embodiment 3, a kind of preparation of gelatin-manganese dioxide composites, the specific steps are as follows:
(1) 3g gelatin is impregnated 50 minutes in 30mL aqueous solution, is then heated to 60 DEG C of dissolutions, stirring keeps its dispersion equal
It is even, it is configured to aqueous gelatin solution；
(2) 42mg manganese sulfate is dissolved in 25ml aqueous solution, 30 points is dispersed under conditions of ultrasonic frequency is 40KHz
Clock is configured to manganese sulfate solution until being uniformly dispersed；
(3) take the manganese sulfate for being added in the aqueous gelatin solution prepared in 30ml step (1) and preparing in 50ml step (2) molten
Liquid, and 379mg potassium permanganate is added, it stirs evenly, pours into ptfe autoclave, 200 DEG C are reacted 24 hours, are obtained brown
Color precipitating；And cleaned repeatedly with water, unreacted reagent is removed, and dry and obtain the i.e. described gelatin-manganese dioxide of brown powder
Compound.
Gelatin-the manganese dioxide composites prepared in embodiment 1, embodiment 2 and embodiment 3 are passed through into scanning electron microscope respectively
Transmissioning electric mirror test, scanning electron microscope (SEM) photograph is as shown in Figure 1, transmission electron microscope picture is as shown in Figure 2.Electromicroscopic photograph shows, three
The gelatin prepared in embodiment-manganese dioxide particle is dumbbell structure, is about 4 μm, about 2 μm wide；Dumbbell structure surface
Containing a large amount of fine particle, illustrate that gelatin molecule is centered around around manganese dioxide, forms adsorption site one by one.
20mg gelatin-manganese dioxide composites prepared by embodiment 1, are added separately to that 20mL is leaded and cadmium by embodiment 4
Aqueous solution in, lead, cadmium concentration be respectively 0-150 μ g/mL.(200rpm) is vibrated after 10 hours, is then centrifuged for
(10000rpm) removes gelatin-manganese dioxide composites, using national standard method (GB/T 5750.6-2006 Drinking Water
Standard test method metal indicator) content of lead, cadmium in supernatant is measured, and then calculate gelatin-manganese dioxide composites pair
The adsorption capacity of lead and cadmium.Specific test results are shown in figure 2, and gelatin-manganese dioxide composites hold the absorption of lead, cadmium ion
Amount reach 165.7mg/g, 155.8mg/g, and compare manganese dioxide to the adsorption capacity of lead, cadmium ion be only 50.13mg/g,
48.82mg/g shows Adsorption of Lead, the site of cadmium ion has been formed.
Embodiment 5,20mg gelatin-manganese dioxide composites prepared by embodiment 1, which are added separately to 20mL concentration, is
In the lead of 10 μ g/mL, cadmium aqueous solution, while oscillation absorption, it is spaced different time point acquisition supernatants, is marked using country
Lead in quasi- method (GB/T 5750.6-2006 drinking water standard method of inspection metal indicator) measurement supernatant, cadmium contain
Amount, and then gelatin-manganese dioxide composites are calculated to the rate of adsorption of lead, cadmium.As a result as shown in figure 3, gelatin-manganese dioxide
Compound can reach adsorption equilibrium in 45 minutes, show preferable adsorption efficiency.
Claims (5)
1. a kind of gelatin-manganese dioxide composites preparation method for adsorbing heavy metal, it is characterised in that include the following steps:
(1) gelatin is added to the water, stand 30 minutes or more, it is then heated to 40-60 DEG C, is made it dissolve, it is dense to be configured to quality
The aqueous gelatin solution of degree≤10%；
(2) manganese sulfate is dissolved in the water, ultrasonic disperse is uniform, and compound concentration is the manganese sulfate solution of 20-30mmol/L；
(3) sulfuric acid that will be prepared in step (2) according to the ratio that the volume ratio of aqueous gelatin solution and manganese sulfate solution is 6:3-5
Manganese aqueous solution is added in the aqueous gelatin solution prepared in step (1), and potassium permanganate is added into mixed solution and stirs evenly,
Potassium permanganate concentration is 10-25mmol/L in mixed solution after stirring；
(4) mixed solution that step (3) obtains is poured into ptfe autoclave, it is anti-under 150-200 DEG C of hot conditions
It answers 8-24 hours, obtains tan precipitate, and the tan precipitate of collection is cleaned to unreacting reagent repeatedly with clear water and is completely removed
Afterwards, drying obtains the i.e. described gelatin-manganese dioxide composites of brown powder, and powder particle is in dumbbell structure under Electronic Speculum.
2. a kind of gelatin-manganese dioxide composites preparation method for adsorbing heavy metal according to claim 1, feature exist
In: the gelatin mass ratio in the step (1) in aqueous gelatin solution is 4-6%.
3. a kind of gelatin-manganese dioxide composites preparation method for adsorbing heavy metal according to claim 1, feature exist
In: the supersonic frequency of ultrasonic disperse is 40KHz in the step (2), and jitter time is 10-30 minutes.
4. a kind of gelatin-manganese dioxide composites application of method preparation according to claim 1, feature exist
In: gelatin-manganese dioxide composites of preparation are directly appended in leaded and cadmium sewage after oscillation absorption 4-10 hours, from
The heart removes gelatin-manganese dioxide composites, purifies to lead in sewage and cadmium；Its gelatin-manganese dioxide composites additive amount
For 5-20g/20L sewage.
5. a kind of application of gelatin-manganese dioxide composites according to claim 4, it is characterised in that: the gelatin-
Manganese dioxide composites are respectively 165.7mg/g, 155.8mg/g to the adsorption capacity of lead, cadmium.
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