CN106745586A - A kind of preparation method and application of cysteine-modifying ferric iron silica mlcrogels flocculant - Google Patents
A kind of preparation method and application of cysteine-modifying ferric iron silica mlcrogels flocculant Download PDFInfo
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- CN106745586A CN106745586A CN201611071331.XA CN201611071331A CN106745586A CN 106745586 A CN106745586 A CN 106745586A CN 201611071331 A CN201611071331 A CN 201611071331A CN 106745586 A CN106745586 A CN 106745586A
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- flocculant
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The present invention relates to a kind of preparation method and application of cysteine-modifying ferric iron silica mlcrogels flocculant;Water intaking glass is simultaneously dissolved in distilled water, obtains the mixed solution of waterglass and water, and this mixed solution reclaimed water glass content is 5.3~10.7wt%;To configure in the dilution heat of sulfuric acid addition mixed solution of 1~3mol/L, pH value of solution will be adjusted to 8~10 scopes;The concentrated sulfuric acid is added to adjust to 2~2.2 scopes pH value of solution;Then ferric sulfate solid and cysteine solid are sequentially added, the mass fraction of ferric sulfate and cysteine in solution is followed successively by 2.5~9.4% and 0.2~0.9%, stirred and fully dissolve, obtain cysteine-modifying ferric iron silica mlcrogels flocculant.Iron silicon substrate flocculant of the present invention is used for dye wastewater treatment.Possess the double effectses of cysteine-modifying class Fenton catalysis and flocculation.Its COD clearance can reach more than 84.7%.
Description
Technical field
The present invention relates to a kind of preparation method of the silicon substrate flocculant for thering is class Fenton to act on, belong to high concentrations of organic dye dirty
Water-treatment technology field.
Technical background
In recent years, the dye wastewater of dye industry discharge has become the subject matter in modern industry, these dyestuffs master
Be used to weaving, print and dye, papermaking, process hides, in the industrial sector such as paint.Based on dye wastewater complicated component, toxicity is high, colourity
Greatly, it is anti-oxidant, the characteristics of antibiont degradation capability is strong, and a large amount of situations about using of dyestuff cause dye wastewater discharge capacity big
So as to cause serious problem of environmental pollution.In traditional Fenton oxidation course of reaction, ferrous ion attacks hydrogen peroxide point
Son hydroxyl radical free radical of the generation with strong oxidizing property realizes organic pollution oxidation Decomposition, ferrous ion be oxidized to form iron from
Son.Fast with reaction speed, oxidation rate is high, simple to operate, easy realization, to the organic pollution degraded substantially without selection
The advantage of property.Its shortcoming is that effective degraded scope of pH is narrower, and iron ion is reduced into the speed of ferrous ion less than ferrous iron
Ion is oxidized the speed of iron ion, and the circulation between the ion of the different valence state of obstruction iron causes the utilization rate of hydrogen peroxide
It is not high, while hydrogen peroxide is extremely easy in decomposition, and then reduce reaction rate.At the same time, the ferric iron that reaction is produced is with the hydrogen of iron
The form of oxide residue is present, and can weaken or block the generation of hydroxyl radical free radical.Using light help Fenton's reaction, flocculation and
During microbial technology combination treatment phenolic waste water, its COD clearance can reach 98.9%, it is shown that very strong synergy
(Chinese patent;Inventor:Liu Guangming, Kong Lingren, Zhong Ping, Zhou Xia, Ren Xuechang, Shi Zaifeng;The patent No.:
CN200410065398.3).But need high light to can be only achieved preferable effect in this method.At using light electrolysis joint Fenton
During reason fracturing wastewater, first there is micro-electrolysis reaction, make substantial amounts of molecular scission in persistent organic pollutants, and produce a large amount of
Fe2+;It is subsequently added hydrogen peroxide and Fenton's reaction occurs, is CO by most of oxidation operation2And H2O;It is subsequently added into polypropylene
Acid amides carries out flocculation sediment, not oxidized pollutant can be separated into (Chinese patent with water;Inventor:Sun Tiegang;Patent
Number:CN201420640558.1).Complex operation in this method, cost is larger, higher to reaction condition requirement.In Fenton reagent
During addition organic additive treatment waste water, the Fe of solubility can be produced in course of reaction3+Part, while effective pH scopes are widened,
Have the disadvantage that the organic additive for adding does not have reducing power, it is impossible to strengthen Fe2+With Fe3+Between circular response, it is possible to decrease reaction
Efficiency (Abida O, Mailhot G, Litter M, Bolte M;Impact of iron‐complex(Fe(III)‐NTA)
on photoinduced degradation of 4‐chlorophenol in aqueous solution).In order to overcome with
Upper shortcoming, class Fenton oxidation reaction receives extensive concern as effective and efficient technology.
The content of the invention
The present invention is intended to provide a kind of preparation method of cysteine-modifying ferric iron silica mlcrogels flocculant.
It is exactly that make use of cysteine to be modified the reaction of class Fenton oxidation in this method, functional group's sulfydryl key of cysteine can
So as to accelerate ferrous iron and ferric circulation, the divalence concentration of iron relatively stablized can be kept to produce more hydroxyl radical free radical,
The utilization rate of hydrogen peroxide is improved, and weakens the decomposition of hydrogen peroxide itself.This catalysis oxidation can also have been widened simultaneously
The pH scopes of reaction degraded mixed dye wastewater.The class Fenton oxidation reaction of cysteine-modifying mistake and the flocculation of flocculant are imitated
Fruit is combined, it will be apparent that improve the treatment effect of sewage.
Technical scheme is as follows:
A kind of preparation method of cysteine-modifying ferric iron silica mlcrogels flocculant;Step is as follows:
1) dilution heat of sulfuric acid of 1~3mol/L is configured;
2) water intaking and is dissolved in distilled water glass, obtains the mixed solution of waterglass and water, this mixed solution reclaimed water glass
Glass content is 5.3~10.7wt%, 5~10min of mechanical agitation;
3) by step 1) dilution heat of sulfuric acid of 1~3mol/L that has configured adds step 2) mixed solution in, by solution
PH is adjusted in the range of 8~10 and keeping lasting stirring;
4) to step 3) add in solution the concentrated sulfuric acid to adjust to 2~2.2 scopes pH value of solution;Then ferric sulfate is sequentially added
Solid and cysteine solid, the mass fraction for making ferric sulfate and cysteine in solution is followed successively by 2.5~9.4% and 0.2~
0.9%, stir and fully dissolve, obtain cysteine-modifying ferric iron silica mlcrogels flocculant.
Microgel flocculant of the invention is applied to dye wastewater treatment.Iron of the iron silicon substrate flocculant when sewage is processed
Ion consumption is 50~500ppm.
It is preferred that the present invention includes to methylene blue, A Li Xinlan 8GX, coomassie brilliant blue R_250 and work for waste water from dyestuff
The wastewater degradation of the dyestuff of property indigo plant 19.
The dilution heat of sulfuric acid of 1~3mol/L is first configured, can be used when pH value is adjusted.Water intaking glass is simultaneously dissolved in distilled water
In, obtain the mixed solution of waterglass and water, this mixed solution reclaimed water glass content be 5.3~10.7wt%, mechanical agitation 5~
10min;The dilution heat of sulfuric acid of the 1~3mol/L that will be configured in advance is added in the mixed solution of above-mentioned waterglass and water, will be molten
Liquid pH is adjusted in the range of 8~10 and keeping lasting stirring;Then pH value of solution is adjusted to 2 to the addition concentrated sulfuric acid in above-mentioned solution
In the range of~2.2;And then to ferric sulfate solid and cysteine solid is sequentially added in above-mentioned reaction solution, sulphur in solution is made
The mass fraction of sour iron and cysteine is followed successively by 2.5~9.4%, 0.2~0.9%, stirs and fully dissolves, you can obtain half
The modified ferric iron silica mlcrogels flocculant of cystine, referred to as iron silicon substrate flocculant.
The beneficial effects of the invention are as follows:It is provided simultaneously with the double effectses of cysteine-modifying class Fenton catalysis and flocculation.
By cysteine-modifying ferric iron silica mlcrogels, the pH models of this catalytic oxidation degradation of dye sewage have been widened
Enclose.The treatment effect of the system is more apparent in acid condition, and preferable treatment effect can be also reached under weak basic condition.When
When being degraded to high concentration mixed dye sewage, can realize that the catalysis of class Fenton and flocculation change by changing pH value
Become, reach more excellent dye wastewater treatment effect, the silicon substrate flocculant for for example being obtained in the present invention is to methylene blue, A Li Xinlan
The percent of decolourization that 8GX, coomassie brilliant blue R_250, active blue 19 these four dyestuffs are obtained when being degraded is followed successively by 96.5%,
95.7%th, 94.4%, 90.1%, its COD clearance can reach 84.7%.
Specific implementation method
The preparation of flocculant
The dilution heat of sulfuric acid of 1~3mol/L is first configured, can be used when pH value is adjusted.Take appropriate waterglass and be dissolved in steaming
In distilled water, the mixed solution of waterglass and water is obtained, this mixed solution reclaimed water glass content is 5.3~10.7wt%, machinery is stirred
Mix 5~10min.The dilution heat of sulfuric acid of the 1~3mol/L that will be configured in advance is added in the mixed solution of above-mentioned waterglass and water,
PH value of solution is adjusted in the range of 8~10 and keeping lasting stirring;Then pH value of solution is adjusted to the addition concentrated sulfuric acid in above-mentioned solution
Save in the range of 2~2.2.And then to ferric sulfate solid and cysteine solid is sequentially added in above-mentioned reaction solution, make molten
The mass fraction of ferric sulfate and cysteine is followed successively by 2.5~9.4%, 0.2~0.9% in liquid, stirs and fully dissolves, you can
Obtain cysteine-modifying ferric iron silica mlcrogels flocculant, referred to as iron silicon substrate flocculant.(the iron silicon substrate is flocculated
Iron ion consumption of the agent when sewage is processed is 50~500ppm)
The application method of catalyst in the present invention:
Methylene blue, A Li Xinlan 8GX, coomassie brilliant blue R_250, four kinds of dyes of active blue 19 are added in 1L running water altogether
Material, every kind of dyestuff addition is 250mg.The mixed solution of these four dyestuffs as need degrade mixed dye sewage solution.Often
The secondary 50mL sewage that takes is degraded.Watery hydrochloric acid is added in sewage, it is therefore an objective to adjust in the range of the pH to 2~6.2 of solution.Successively
The iron silicon substrate flocculant of 50~500 μ L of addition and the H that 0.1~0.5g mass fractions are 30%2O2Solution, reacts 10~120min.
10% calcium oxide is added to adjust in the range of 7.5~9.5 the pH value of solution afterwards.All of above process is required to be stirred with magnetic force
Mix device and keep quick stirring.Then it is millesimal polyacrylamide to mass fraction is added in above-mentioned pending solution
The μ L of solution 100~1000, slow down mixing speed and stir 2~5min.The solution left standstill 30 that will be obtained after the completion of degradation reaction~
180min.It is absorbance to be detected at 664nm, 610nm, 590nm, 554nm and is counted that supernatant is taken in ultraviolet specrophotometer wavelength
Calculate the removal efficiency of colourity.
The beneficial effects of the invention are as follows:It is provided simultaneously with the double effectses of cysteine-modifying class Fenton catalysis and flocculation.
By cysteine-modifying ferric iron silica mlcrogels, this catalytic oxidation degraded mixed dye sewage has been widened
PH scopes.The treatment effect of the system is more apparent in acid condition, and preferably treatment effect can be also reached under weak basic condition
Really.When being degraded to high concentration mixed dye sewage, can realize that the catalysis of class Fenton and flocculation are made by changing pH value
Change, reaches more excellent dye wastewater treatment effect.For example in the present invention silicon substrate flocculant that obtains to methylene blue, Ah
The percent of decolourization that sharp Xinlan 8GX, coomassie brilliant blue R_250, active blue 19 these four dyestuffs are obtained when being degraded is followed successively by
96.5%th, 95.7%, 94.4%, 90.1%, its COD clearance can reach 84.7%.
Embodiment 1:
Bifunctional material flocculant:Waterglass content is 5.3wt%, and it is 8 to adjust its pH with dilution heat of sulfuric acid, then uses dense sulphur
It is 2 that acid adjusts its pH, adds ferric sulfate 1.2g, cysteine 0.1g simultaneously fully to dissolve.
The dilution heat of sulfuric acid of 1mol/L is first configured, can be used when pH value is adjusted.Water intaking glass 2.5g is simultaneously dissolved in 45g steamings
In distilled water, this mixed solution reclaimed water glass content is 5.3wt%, mechanical agitation 5min.The 1mol/L's that will be configured in advance is dilute
Sulfuric acid solution is added in the mixed solution of above-mentioned waterglass and water, and pH value of solution is adjusted to 8 and lasting stirring is kept;Then it is upward
State and add in solution the slow concentrated sulfuric acid successively and pH value of solution is adjusted to 2.And then to sequentially adding 1.2g in above-mentioned reaction solution
Ferric sulfate solid and 0.1g cysteine solids, the mass fraction for making ferric sulfate and cysteine in solution is followed successively by 2.5%,
0.2%, stir and fully dissolve, you can obtain cysteine-modifying ferric iron silica mlcrogels flocculant, referred to as
Iron silicon substrate flocculant.(iron ion content of the iron silicon substrate flocculant when sewage is processed is 50ppm).
Use bifunctional material flocculant process mixed dye sewage of the present invention:Take 50mL sewage to be degraded, in sewage
It is middle to add appropriate watery hydrochloric acid regulation pH=2,50 μ L iron silicon substrate flocculants are added, it is 30% that 0.1g mass fractions are added under agitation
H2O2Solution stirs 10min, and it is millesimal polyacrylamide solution 100 μ L, stirring at low speed 2min to add mass fraction.
The solution left standstill 30min that will be obtained after the completion of degradation reaction.It is at 664nm, 610nm, 590nm, 554nm that supernatant is taken in wavelength
Detection absorbance.Be followed successively by 52.2% by the chroma removal rate that each dyestuff is obtained after calculating, 42.3%, 22.1%,
8.3%.Thus visible its degraded flocculation resultant effect under this condition of result is preferable.
Embodiment 2:
Bifunctional material flocculant:Waterglass content is 6.6wt%, and it is 9 to adjust its pH with dilution heat of sulfuric acid, then uses dense sulphur
It is 2.1 that acid adjusts its pH, adds ferric sulfate 2.4g, cysteine 0.25g simultaneously fully to dissolve.
The dilution heat of sulfuric acid of 2mol/L is first configured, can be used when pH value is adjusted.Water intaking glass 3.2g is simultaneously dissolved in 45g steamings
In distilled water, this mixed solution reclaimed water glass content is 6.6wt%, mechanical agitation 7min.The 2mol/L's that will be configured in advance is dilute
Sulfuric acid solution is added in the mixed solution of above-mentioned waterglass and water, pH is adjusted to 9 and lasting stirring is kept, then to above-mentioned molten
Being slowly added to the concentrated sulfuric acid in liquid successively will adjust pH value of solution to 2.1.And then to sequentially adding 2.4g sulphur in above-mentioned reaction solution
Sour iron solid and 0.25g cysteine solids, the mass fraction for making ferric sulfate and cysteine in solution is followed successively by 5%,
0.5%, stir and fully dissolve, that is, obtain cysteine-modifying ferric iron silica mlcrogels flocculant, referred to as iron
Silicon substrate flocculant.(iron ion content of the iron silicon substrate flocculant when sewage is processed is 150ppm).
Use bifunctional material flocculant process mixed dye sewage of the present invention:Take 50mL sewage to be degraded, in sewage
It is middle to add appropriate watery hydrochloric acid regulation pH=4,375 μ L iron silicon substrate flocculants are added, addition 0.3g mass fractions are under agitation
30% H2O2Solution stirs 30min, and addition mass fraction is the μ L of millesimal polyacrylamide solution 500, stirring at low speed
3min.The solution left standstill 60min that will be obtained after the completion of degradation reaction.Take supernatant ultraviolet specrophotometer wavelength be 664nm,
Absorbance is detected at 610nm, 590nm, 554nm.Be followed successively by 96.5% by the chroma removal rate that each dyestuff is obtained after calculating,
95.7%th, 94.4%, 90.1%.Thus visible its degraded flocculating effect under this condition of result is optimal.
Embodiment 3:
Bifunctional material flocculant:Waterglass content is 10.7wt%, and it is 10 to adjust its pH with dilute sulfuric acid, then uses the concentrated sulfuric acid
It is 2.2 to adjust its pH, adds ferric sulfate 4.2g, cysteine 0.5g simultaneously fully to dissolve.
The dilution heat of sulfuric acid of 3mol/L is first configured, can be used when pH value is adjusted.Take 5.4g waterglass and be dissolved in 45g steamings
In distilled water, this mixed solution reclaimed water glass content is 10.7wt%, mechanical agitation 10min.The 3mol/L's that will be configured in advance
Dilution heat of sulfuric acid is added in the mixed solution of above-mentioned waterglass and water, and pH is adjusted to 10 and lasting stirring is kept;Then it is upward
State and be slowly added to the concentrated sulfuric acid successively in solution and adjust to 2.2 the pH of solution.And then to being sequentially added in above-mentioned reaction solution
4.2g ferric sulfate solid and 0.5g cysteine solids, are followed successively by the mass fraction of ferric sulfate and cysteine in solution
9.4%th, 0.9%, stir and fully dissolve, that is, cysteine-modifying ferric iron silica mlcrogels flocculant is obtained, letter
Referred to as iron silicon substrate flocculant.(iron ion content of the iron silicon substrate flocculant when sewage is processed is 500ppm).
Using bifunctional material flocculant process mixed dye sewage of the present invention, take 50mL sewage and degraded, in sewage
It is middle to add appropriate watery hydrochloric acid regulation pH=6.2,1250 μ L iron silicon substrate flocculants are added, addition 0.5g mass fractions are under agitation
30% H2O2Solution stirs 10min, and addition mass fraction is the μ L of millesimal polyacrylamide solution 1000, stirring at low speed
5min.The solution left standstill 180min that will be obtained after the completion of degradation reaction.Take supernatant is in ultraviolet specrophotometer wavelength
Absorbance is detected at 664nm, 610nm, 590nm, 554nm.It is followed successively by by the chroma removal rate that each dyestuff is obtained after calculating
81.7%th, 79.1%, 71.4%, 50.1%.Thus visible its degraded flocculating effect under this condition of result is preferable.
Claims (4)
1. a kind of preparation method of cysteine-modifying ferric iron silica mlcrogels flocculant;It is characterized in that step is such as
Under:
1) dilution heat of sulfuric acid of 1~3mol/L is configured;
2) water intaking and is dissolved in distilled water glass, obtains the mixed solution of waterglass and water, and waterglass contains in this mixed solution
It is 5.3~10.7wt% to measure, 5~10min of mechanical agitation;
3) by step 1) dilution heat of sulfuric acid of 1~3mol/L that has configured adds step 2) mixed solution in, pH value of solution is adjusted
Section is in the range of 8~10 and keeping persistently stirring;
4) to step 3) add in solution the concentrated sulfuric acid to adjust to 2~2.2 scopes pH value of solution;Then ferric sulfate solid is sequentially added
With cysteine solid, the mass fraction for making ferric sulfate and cysteine in solution is followed successively by 2.5~9.4% and 0.2~
0.9%, stir and fully dissolve, obtain cysteine-modifying ferric iron silica mlcrogels flocculant.
2. the application of the microgel flocculant of claim 1, it is characterized in that being used for dye wastewater treatment.
3. application as claimed in claim 2, it is characterized in that iron ion consumption of the iron silicon substrate flocculant when sewage is processed is 50
~500ppm.
4. application as claimed in claim 2, it is characterized in that waste water from dyestuff is included to methylene blue, A Li Xinlan 8GX, coomassie
The wastewater degradation of the dyestuff of light blue R-250 and active blue 19.
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CN113231104A (en) * | 2021-05-31 | 2021-08-10 | 华中科技大学 | Amino acid modified nano zero-valent iron material and preparation method thereof |
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CN113231104A (en) * | 2021-05-31 | 2021-08-10 | 华中科技大学 | Amino acid modified nano zero-valent iron material and preparation method thereof |
CN113231104B (en) * | 2021-05-31 | 2022-06-14 | 华中科技大学 | Amino acid modified nano zero-valent iron material and preparation method thereof |
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