CN106732444A - A kind of method processed stibium-containing wastewater except antimony sorbing material and preparation method thereof and using it - Google Patents
A kind of method processed stibium-containing wastewater except antimony sorbing material and preparation method thereof and using it Download PDFInfo
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- CN106732444A CN106732444A CN201611066138.7A CN201611066138A CN106732444A CN 106732444 A CN106732444 A CN 106732444A CN 201611066138 A CN201611066138 A CN 201611066138A CN 106732444 A CN106732444 A CN 106732444A
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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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- 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
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Abstract
The invention belongs to the process field of stibium-containing wastewater, and in particular to one kind is except antimony sorbing material and preparation method thereof and application method.This comprises the following steps except the preparation method of antimony sorbing material:S1. KMnO is used4And H2SO4Mixed solution immersion polyamide, polyamide is swelling and and KMnO4With generation redox reaction, the hydration MnO for fully being generated after reaction2Be attached to it is swelling after polyamide on;S2. the polyamide input FeSO after being processed through S14Fully soaked in solution, MnO is hydrated in immersion process2With FeSO4Reaction, the Fe (OH) of generation3It is doped in hydration MnO2In, filter off solution and cleaned with water, must be loaded with being hydrated MnO2With Fe (OH)3Polyamide, it is as described except antimony sorbing material.Its application method is simple, on request wet method dress post, and post is crossed after waste water is adjusted into pH.Advantages of the present invention is that the material that uses and reagent safety are nontoxic, except the preparation method of antimony sorbing material is simple and easy to apply;Except antimony sorbing material is high to the removal efficiency of antimony in water and is easy to regeneration and Reusability.
Description
Technical field
The invention belongs to the process field of stibium-containing wastewater, and in particular to one kind is except antimony sorbing material and preparation method thereof and makes
Use method
Background technology
Antimony is a kind of important non-ferrous metal, and antimony and its compound are widely used in ceramics, enamel, rubber, pigment, partly lead
The fields such as body, plastics, medicine, glass, battery, paint, pyrotechnic material, alloy and fire retardant.Antimony is not organism indispensable element,
With accumulation toxicity and carcinogenicity.Antimony and its compound are classified as preferential thing of preventing and remedying pollution by EPA and European Union.In China,
The health hazard that antimony pollution brings increasingly is paid close attention to by government and the public, and the effectively treatment of stibium-containing wastewater is extremely urgent.
China is antimony reserves country the abundantest in the world, is also to produce the big country of antimony first.Antimony and other non-ferrous metals
Adopt, select, a large amount of stibium-containing wastewaters of the process such as smelting discharge be antimony pollution major source, this also means that China is just carry seriously
Antimony pollution environmental risk.In recent years, it is domestic due to the way such as the Weathering And Leaching of Tailings Dam containing antimony, non-ferrous metal selecting and purchasing smelting discharge of wastewater
The event of water body antimony pollution is caused to happen occasionally in footpath.The valence state of antimony is usually+3 or+5 valencys, and the toxicity of trivalent antimony is than quinquevalence antimony
High ten times of toxicity, based on the research to antimony toxicity, the maximum acceptable concentration that some scholars have obtained Antimony In The Soils is 3.5-5mg/
kg.The limit value of antimony in drinking water is set to 6 μ g/L, China by EPA《Surface water environment quality mark》(GB3838-2002)
With《Drinking Water hygienic practice》The limit value of antimony is set to 5 μ g/L in (Ministry of Public Health, 2001).Antimony into water body passes through
Food chain enrichment is serious to threaten health, particularly causes high risks safely to drinking water supply, effectively prevention, control and
Antimony is administered to be of great significance the pollution tool of water environment.
Presence valence state and form of the antimony in water environment are extremely complex, and effective administering method of antimony pollution water body is few, especially
Its effective technology for lacking advanced treating.At present both at home and abroad for its water pollution treatment main method have chemical precipitation method, from
Sub- exchange process, membrane separation process, absorption method etc., these methods are each advantageous, but practical application all has obvious limitation.Chemistry is heavy
Shallow lake method is main with Polyferric Sulfate or poly-aluminium coagulating sedimentation, the method process is simple, after effect stability, but treatment in water antimony content still compared with
Height, is only suitable for as pretreatment.Ion-exchange is larger due to the calcium in water, magnesium plasma background concn, and competition exchange is caused
Efficiency declines, and antimony often exists, it is necessary to use anion and sun simultaneously with anion and cation form simultaneously in water
Ion exchange resin;Additionally, part antimony may be with uncharged Sb (OH)3Form is present, and ion-exchange cannot be removed.Film
Partition method has separative efficiency high, is taken seriously in heavy metal containing wastewater treatment field, but because film device invests larger, running cost
With higher, easily contaminated etc. reason of film, its practical application there are problems that many.Absorption method be water removal in micro heavy most
One of method of practical value, but, due to antimony, valence state and form are extremely complex in water, and existing sorbing material is difficult to reach
Absorption completely to various form antimony.The material that developing has selection characterization of adsorption to various existing forms antimony has important reality
Border meaning.
The content of the invention
The technical problems to be solved by the invention are to provide one kind except antimony sorbing material and preparation method thereof and application method,
It can effectively be adsorbed to the antimony in water, antimony content is down to below the limit value of Standard.
The technical scheme that the present invention solves above-mentioned technical problem is as follows:It is a kind of except the preparation method of antimony sorbing material, its bag
Include following steps:
S1. KMnO is used4And H2SO4Mixed solution immersion polyamide, polyamide is swelling and and KMnO4With aoxidize
The hydration MnO generated after reduction reaction, fully reaction2Be attached to it is swelling after polyamide on;
S2. the polyamide input FeSO after being processed through S14Fully soaked in solution, MnO is hydrated in immersion process2With
FeSO4Reaction, the Fe (OH) of generation3It is doped in hydration MnO2In, filter off solution and cleaned with water, must be loaded with being hydrated MnO2With
Fe(OH)3Polyamide, it is as described except antimony sorbing material.Obtain except antimony sorbing material moisture content generally in 20-40%
Between, and should keep in dark place.
Specifically, polyamide and the mass ratio of mixed solution are 0.5-1.5 in S1:30, KMnO in mixed solution4Quality
Fraction is 3-7%, H2SO4Mass fraction be 0.1-0.5%.
Specifically, the abundant reaction in S1 refers to reaction to the purple of mixed solution taking off.
Specifically, polyamide and FeSO in S24The mass ratio of solution is 0.5-1.5:30, FeSO4FeSO in solution4's
Mass fraction is 1-5%.
Specifically, the abundant immersion in S2 refers to immersion more than 24h.
Specifically, the polyamide is polyamide granules or Fypro.
The present invention also provides a kind of except antimony sorbing material, and it is prepared by above-mentioned method.
The present invention still further provides using the above-mentioned method processed stibium-containing wastewater except antimony sorbing material, its bag
Include following steps:By it is described fully soaked except antimony sorbing material water after wet method dress post obtain adsorption column, the blade diameter length ratio of adsorption column
It is 1:8-10;The pH of stibium-containing wastewater is adjusted to 5-8, adsorption column is then crossed with the flow velocity of 2-4BV/h, that is, completed to stibium-containing wastewater
Treatment.BV/h is typically the expression of space flow speed, and the volume for referring to the liquid that the unit interval (h) flows through pillar in post is tree in post
The multiple of fat volume.
In above-mentioned processing method, when antimony content is in more than 1mg/L in stibium-containing wastewater, stibium-containing wastewater crosses the advance of adsorption column
Row reduces the pretreatment of antimony content:It is 2-5g that bodied ferric sulfate is added in every liter of stibium-containing wastewater, stirs 15-30min, is added afterwards
Milk of lime to pH value of solution is 7-8, continues to stir 15-30min, finally adds polyacrylamide to carry out flocculation under slow stirring heavy
Shallow lake, separation of solid and liquid, the amount that polyacrylamide is added in every liter of stibium-containing wastewater are 2-10g.
In above-mentioned processing method, in adsorption column water outlet is caused close to adsorption saturation except antimony sorbing material in adsorption column
When antimony content exceedes limit value, sorbing material is regenerated:With 1~2%NaOH solution soak adsorption column in except antimony adsorption material
Material more than 6h, then crosses adsorption column to being that 7-8 stops wash-out, adsorption material to water outlet pH except antimony sorbing material is eluted with water
Material is regenerated.
The beneficial effects of the invention are as follows:The material and reagent safety for using are nontoxic, and the preparation method of sorbing material is simply easy
OK;Sorbing material it is high to the removal efficiency of antimony in water and be easy to regeneration, can Reusability, by equipped with sorbing material of the invention
Adsorption column treatment after, the content of antimony can be dropped to below the limit value of Standard in water;The system of the sorbing material that the present invention is provided
Preparation Method uses KMnO first4The method for aoxidizing polyamide makes hydrated manganese dioxide be firmly bonded on polyamide, makes polyamide
As a kind of carrier material of stabilization, it has good combination property, including mechanical property, heat resistance, wear resistance, resistance toization
Medicine etc. is learned, therefore making carrier with it can be effectively increased the service life of sorbing material;Additionally, the hydration MnO in sorbing material2
Trivalent antimony in water can be oxidized to quinquevalence antimony, to make it easier to removal, the Fe (OH) in sorbing material3Have to antimony in water
Adsorption capacity higher;Fe(OH)3It is few to calcium, magnesium, sulfate radical, chlorine plasma absorption, therefore the sorbing material that the present invention is provided exists
Influenceed small by other coexisting ions during to the absorption of antimony, therefore method is practical, it is easy to implement.
Specific embodiment
Principle of the invention and feature are described below in conjunction with specific embodiment, example is served only for explaining this hair
It is bright, it is not intended to limit the scope of the present invention.
Embodiment 1
One kind removes antimony sorbing material, and its preparation method is as follows:
S1. KMnO is used4And H2SO4Mixed solution soak polyamide granules (column chromatography polyamide granules), polyamide
Particle is 0.5 with the mass ratio of mixed solution:30, KMnO in mixed solution4Mass fraction be 3%, H2SO4Mass fraction
It is 0.1%, polyamide granules are swelling and and KMnO4With generation redox reaction, the hydration MnO for fully being generated after reaction2Attachment
On polyamide granules after swelling;
S2. the polyamide granules input FeSO after being processed through S14Fully soaked in solution, the polyamide in S2 with
FeSO4The mass ratio of solution is 0.5:30, FeSO4FeSO in solution4Mass fraction be 1%, MnO is hydrated in immersion process2With
FeSO4Reaction, the Fe (OH) of generation3It is doped in hydration MnO2In, filter off solution and cleaned with water, must be loaded with being hydrated MnO2With
Fe(OH)3Polyamide, it is as described except antimony sorbing material.
Using obtained above except antimony sorbing material is processed the waste water containing antimony 0.8mg/L, specific method is:By institute
State fully soaked except antimony sorbing material water after wet method dress post obtain adsorption column, the blade diameter length ratio of adsorption column is 1:8;By stibium-containing wastewater
PH adjust to 5, adsorption column is then crossed with the flow velocity of 2BV/h, amount containing antimony in the water collected after post of crossing is 3.5 μ g/L.
Using obtained above except antimony sorbing material is processed the waste water containing antimony 2mg/L, specific method is:Will be described
Fully soaked except antimony sorbing material water after wet method dress post obtain adsorption column, the blade diameter length ratio of adsorption column is 1:8;Stibium-containing wastewater is entered
Row reduces the pretreatment of antimony content:It is 2g that bodied ferric sulfate is added in every liter of stibium-containing wastewater, stirs 15min, and lime is added afterwards
Breast to pH value of solution is 7, continues to stir 15min, finally adds polyacrylamide to carry out flocculation sediment, solid-liquid point under slow stirring
From the low waste water of amount containing antimony is obtained, the amount that polyacrylamide is added in every liter of stibium-containing wastewater is 2g, and the pH of the low waste water of amount containing antimony is adjusted
To 5, adsorption column is then crossed with the flow velocity of 2BV/h, amount containing antimony in the water collected after post of crossing is 4.1 μ g/L.
Embodiment 2
One kind removes antimony sorbing material, and its preparation method is as follows:
S1. KMnO is used4And H2SO4Mixed solution immersion Fypro, the quality of Fypro and mixed solution
Than being 1:30, KMnO in mixed solution4Mass fraction be 5%, H2SO4Mass fraction be 0.3%, Fypro is swelling
And and KMnO4With generation redox reaction, the hydration MnO for fully being generated after reaction2Be attached to it is swelling after Fypro
On;
S2. the Fypro input FeSO after being processed through S14Fully soaked in solution, the polyamide in S2 with
FeSO4The mass ratio of solution is 1:30, FeSO4FeSO in solution4Mass fraction be 3%, MnO is hydrated in immersion process2With
FeSO4Reaction, the Fe (OH) of generation3It is doped in hydration MnO2In, filter off solution and cleaned with water, must be loaded with being hydrated MnO2With
Fe(OH)3Fypro, it is as described except antimony sorbing material.
Using obtained above except antimony sorbing material is processed the waste water containing antimony 0.5mg/L, specific method is:By institute
State fully soaked except antimony sorbing material water after wet method dress post obtain adsorption column, the blade diameter length ratio of adsorption column is 1:9;By stibium-containing wastewater
PH adjust to 6.5, adsorption column is then crossed with the flow velocity of 3BV/h, amount containing antimony in the water collected after post of crossing is 2.1 μ g/L.
Using obtained above except antimony sorbing material is processed the waste water containing antimony 5mg/L, specific method is:Will be described
Fully soaked except antimony sorbing material water after wet method dress post obtain adsorption column, the blade diameter length ratio of adsorption column is 1:9;Stibium-containing wastewater is entered
Row reduces the pretreatment of antimony content:It is 4g that bodied ferric sulfate is added in every liter of stibium-containing wastewater, stirs 20min, and lime is added afterwards
Breast to pH value of solution is 8, continues to stir 20min, finally adds polyacrylamide to carry out flocculation sediment, solid-liquid point under slow stirring
From the low waste water of amount containing antimony is obtained, the amount that polyacrylamide is added in every liter of stibium-containing wastewater is 5g, and the pH of the low waste water of amount containing antimony is adjusted
To 7, adsorption column is then crossed with the flow velocity of 3BV/h, amount containing antimony in the water collected after post of crossing is 2.6 μ g/L.
Embodiment 3
One kind removes antimony sorbing material, and its preparation method is as follows:
S1. KMnO is used4And H2SO4Mixed solution soak polyamide granules (column chromatography polyamide granules), polyamide
Particle is 1.5 with the mass ratio of mixed solution:30, KMnO in mixed solution4Mass fraction be 7%, H2SO4Mass fraction
It is 0.5%, polyamide granules are swelling and and KMnO4With generation redox reaction, the hydration MnO for fully being generated after reaction2Attachment
On polyamide granules after swelling;
S2. the polyamide granules input FeSO after being processed through S14Fully soaked in solution, the polyamide granules in S2
With FeSO4The mass ratio of solution is 1.5:30, FeSO4FeSO in solution4Mass fraction be 5%, MnO is hydrated in immersion process2
With FeSO4Reaction, the Fe (OH) of generation3It is doped in hydration MnO2In, filter off solution and cleaned with water, must be loaded with being hydrated MnO2
With Fe (OH)3Polyamide granules, it is as described except antimony sorbing material.
Using obtained above except antimony sorbing material is processed the waste water containing antimony 0.9mg/L, specific method is:By institute
State fully soaked except antimony sorbing material water after wet method dress post obtain adsorption column, the blade diameter length ratio of adsorption column is 1:10;Antimony will be contained to give up
The pH of water is adjusted to 8, then crosses adsorption column with the flow velocity of 4BV/h, and amount containing antimony in the water collected after post of crossing is 3.4 μ g/L.
Using obtained above except antimony sorbing material is processed the waste water containing antimony 10mg/L, specific method is:By institute
State fully soaked except antimony sorbing material water after wet method dress post obtain adsorption column, the blade diameter length ratio of adsorption column is 1:10;To useless containing antimony
Water reduce the pretreatment of antimony content:It is 5g that bodied ferric sulfate is added in every liter of stibium-containing wastewater, stirs 30min, is added afterwards
Milk of lime to pH value of solution is 8, continues to stir 30min, finally adds polyacrylamide to carry out flocculation sediment, solid under slow stirring
Liquid separates to obtain the low waste water of amount containing antimony, and the amount that polyacrylamide is added in every liter of stibium-containing wastewater is 10g, by the pH of the low waste water of amount containing antimony
Regulation then crosses adsorption column to 8 with the flow velocity of 4BV/h, and amount containing antimony in the water collected after post of crossing is 4.7 μ g/L.
Embodiment 4
When being prepared using embodiment 1 except antimony sorbing material is processed into adsorption column the waste water containing antimony 0.8mg/L
Except antimony sorbing material is caused close to adsorption saturation antimony content is higher than 5 μ g/L of national standard limit in adsorption column water outlet when, to adsorption column
In sorbing material regenerated:With 1~2%NaOH solution soak adsorption column in except more than antimony sorbing material 6h, then use
Water crosses adsorption column to being that 7-8 stops wash-out to water outlet pH, except antimony sorbing material is to obtain again except antimony sorbing material is eluted
It is raw.
After regeneration, use device has adsorption column of the regeneration except antimony sorbing material in method same in embodiment 1 to containing antimony
The waste water of 0.8mg/L is processed, cross post after collect water in amount containing antimony be 3.7 μ g/L, after regeneration except antimony sorbing material pair
Antimony in stibium-containing wastewater still has preferable adsorption effect.
The antimony content of the stibium-containing wastewater in embodiment 1 to 4 and the antimony content crossed in the water collected after adsorption column pass through
ICP-MS methods determine, from the point of view of the result that above-described embodiment is processed stibium-containing wastewater, the present invention provide except antimony adsorption material
Material has preferable adsorption effect and should adsorption effect is still except antimony sorbing material regenerating easily, after regeneration to the antimony in stibium-containing wastewater
So preferably.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all it is of the invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (10)
1. it is a kind of except the preparation method of antimony sorbing material, it is characterised in that to comprise the following steps:
S1. KMnO is used4And H2SO4Mixed solution immersion polyamide, polyamide is swelling and and KMnO4Redox is anti-with occurring
Should, the hydration MnO for fully being generated after reaction2Be attached to it is swelling after polyamide on;
S2. the polyamide input FeSO after being processed through S14Fully soaked in solution, MnO is hydrated in immersion process2With FeSO4
Reaction, the Fe (OH) of generation3It is doped in hydration MnO2In, filter off solution and cleaned with water, must be loaded with being hydrated MnO2And Fe
(OH)3Polyamide, it is as described except antimony sorbing material.
2. a kind of except the preparation method of antimony sorbing material according to claim 1, it is characterised in that in S1 polyamide with mix
The mass ratio of solution is 0.5-1.5:30, KMnO in mixed solution4Mass fraction be 3-7%, H2SO4Mass fraction be
0.1-0.5%.
3. it is a kind of except the preparation method of antimony sorbing material according to claim 1, it is characterised in that the abundant reaction in S1 is
Refer to that reaction to the purple of mixed solution takes off.
4. a kind of except the preparation method of antimony sorbing material according to claim 1, it is characterised in that polyamide in S2 with
FeSO4The mass ratio of solution is 0.5-1.5:30, FeSO4FeSO in solution4Mass fraction be 1-5%.
5. it is according to claim 1 a kind of except the preparation method of antimony sorbing material, it is characterised in that the abundant immersion in S2
Refer to immersion more than 24h.
6. it is a kind of except the preparation method of antimony sorbing material according to any one of Claims 1-4, it is characterised in that described
Polyamide is polyamide granules or Fypro.
7. it is a kind of to remove antimony sorbing material, it is characterised in that the method as described in any one of claim 1 to 5 is prepared.
8. the method processed stibium-containing wastewater except antimony sorbing material described in a kind of usage right requirement 7, it is characterised in that
Comprise the following steps:By it is described fully soaked except antimony sorbing material water after wet method dress post obtain adsorption column, the footpath of adsorption column is high
Than being 1:8-10;The pH of stibium-containing wastewater is adjusted to 5-8, adsorption column is then crossed with the flow velocity of 2-4BV/h, that is, completed to useless containing antimony
The treatment of water.
9. the method that a kind of use according to claim 8 is processed stibium-containing wastewater except antimony sorbing material, its feature
It is that, when antimony content is in more than 1mg/L in stibium-containing wastewater, stibium-containing wastewater carries out reducing the pre- place of antimony content before crossing adsorption column
Reason:To bodied ferric sulfate is added in stibium-containing wastewater, 15-30min is stirred, it is 7-8 that milk of lime to pH value of solution is added afterwards, continues to stir
15-30min is mixed, finally adds polyacrylamide to carry out flocculation sediment, separation of solid and liquid under slow stirring, in every liter of stibium-containing wastewater
Addition bodied ferric sulfate is 2-5g, and the amount that polyacrylamide is added in every liter of stibium-containing wastewater is 2-10g.
10. the method that a kind of use according to claim 8 or claim 9 is processed stibium-containing wastewater except antimony sorbing material, its
It is characterised by, antimony content exceedes limit value in adsorption column water outlet is caused close to adsorption saturation except antimony sorbing material in adsorption column
When, sorbing material is regenerated:With 1~2%NaOH solution soak adsorption column in except more than antimony sorbing material 6h, then use
Water crosses adsorption column to being that 7-8 stops wash-out to water outlet pH except antimony sorbing material is eluted, and sorbing material is to be regenerated.
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CN109453734A (en) * | 2018-11-14 | 2019-03-12 | 中国地质大学(北京) | A kind of MnO2Modified ferrihydrite adsorbing material and preparation method thereof |
CN110186830A (en) * | 2019-06-03 | 2019-08-30 | 上海理工大学 | Laboratory dyeing waste water removes antimony filtrate test device and method |
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CN111875091A (en) * | 2020-07-13 | 2020-11-03 | 旬阳领盛新材料科技有限公司 | Treatment method of antimony-containing wastewater |
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CN112774631A (en) * | 2021-01-11 | 2021-05-11 | 内蒙古牧星人新材料科技有限公司 | Method for preparing biochar-based composite adsorbing material by using aquatic product processing waste and application of biochar-based composite adsorbing material in antimony-containing wastewater treatment |
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