CN106277478A - Sulfur acid sodium waste water treatment process in precipitated silica production process - Google Patents
Sulfur acid sodium waste water treatment process in precipitated silica production process Download PDFInfo
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- CN106277478A CN106277478A CN201610643670.4A CN201610643670A CN106277478A CN 106277478 A CN106277478 A CN 106277478A CN 201610643670 A CN201610643670 A CN 201610643670A CN 106277478 A CN106277478 A CN 106277478A
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- calcium
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- prodan
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- 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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
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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
-
- 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
- C02F2101/101—Sulfur compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Geology (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention provides sulfur acid sodium waste water treatment process in a kind of precipitated silica production process, particularly as follows: waste water is sent in reaction tank, it is continuously added into silicate fluoride solution while stirring, precipitation prodan in the first sedimentation tank sent into by material, filter pressing, filter cake washs, i.e. prepares prodan after drying;Solution after precipitation prodan is sent in neutralization pond standby together with the filtrate of solid-liquid separation;Add lime cream or precipitated calcium carbonate powder, send into sulfate precipitate calcium in the second sedimentation tank;Calcium sulfate slip filter pressing, Cake Wash the most i.e. prepares calcium sulfate;Regulating reservoir adds oxalic acid, sends into and the 3rd sedimentation tank precipitates calcium oxalate;Calcium oxalate slip filter pressing, Cake Wash the most i.e. prepares calcium oxalate.Solving the deficiency in background technology, this technique can process by waste water be applicable to the precipitated silica production process of different component, it is possible to reclaims the salinity in waste water, and recycle-water resource is reused.
Description
Technical field
The present invention relates to the technique processing method of wastewater zero discharge in a kind of precipitated silica production process, specifically provide
A kind of salinity reclaimed in waste water and reusable for water technique can be belonged to environmental technology field.
Background technology
White carbon refers to that precipitated silica, main component are silicon dioxide, the available mSiO of its composition2·nH2O represents.It
Being one of a kind of important fine inorganic chemicals product, its performance is similar to white carbon black, and outward appearance is the amorphous of white high degree of dispersion
Powder or cotton-shaped powder, also have and be processed into graininess as commodity.Light weight, below initial size 0.3 μm, relative density
2.319~2.653, fusing point 1750 DEG C, water insoluble and most acid, there is water absorption, can become after absorbing moisture in atmosphere
For the particulate assembled.Caustic soda and Fluohydric acid. can be dissolved in.Stable to other chemical drugs, high temperature resistant do not decompose, do not burn.To base
Matter and active component and additive demonstrate chemical inertness, to vitamin, hormone, fluoride, antibiotic, enzyme preparation and cosmetics
In conventional many active component have the good compatibility.There is the highest electrical insulating property.Owing to having porous and big
Specific surface area, has bigger dispersion force in rubber, be filled in rubber demonstrate high reinforcing.Surface-modified process
Hydrophobicity white carbon is soluble in oil, for rubber and plastics etc. as reinforcing filler, all can make the mechanical strength of its product
Significantly improve with anti-tear index.Owing to manufacture method is different, the physico-chemical property of white carbon, microstructure all have different,
Therefore its application and application effect are the most different.Precipitated silica is divided into again tradition precipitated silica and special precipitation white
White carbon black.The former refers to sulphuric acid, hydrochloric acid, CO2Being the white carbon that base stock produces with waterglass, the latter refers to use hypergravity
The Linesless charcoal that the specific process such as technology, sol-gel process, chemical crystal method, second-crystallized method or reverse micelle microemulsion liquid method produce
Black.
Precipitated silica is to prepare for raw material through chemical reaction with liquid sodium silicate with sulphuric acid mostly in the art
White carbon, its chemical equation respectively:
Na2O·mSiO2+H2SO4+nH2O=mSiO2·(n+1)H2O↓+Na2SO4
China is engaged in the history producing existing more than 50 year of precipitated silica, and the knowhow of more than 50 year shows, produces
The maximum consumption of precipitated silica is at two aspects: one is that the energy consumption of product is big, and white carbon black product per ton needs 750-880 degree
Electricity, 12-16 cube of steam and 2-4 ton coal;Two is that water consumption is big, and white carbon black product per ton needs the tap water of 65-80 ton, one
Producing 10000 tons of white carbon black production enterprises per year, the water consumption of a year is 65-80 ten thousand tons, and its water consumption is the most surprising!If white carbon
Manufacturing enterprise can not process these waste water containing sulfate effectively so that it is is scientificlly and effectively recycled, it will give
Local environment brings serious pollution;Also the wretched insufficiency that local water resource is brought can be given;Therefore, energy-saving and cost-reducing, green
Environmental protection is two big bottleneck and key factors of restriction China white carbon industry survival and development;At energy-conservation aspect, we can be in order to
The enterprise of afterheat steam more than needed and waste heat flue gas is had to solve big the asking of its energy consumption with local steel mill, power plant, coke-oven plant etc.
Topic;In terms of water saving, we must develop a kind of sulfur acid sodium cycling utilization of wastewater and accomplish the green of low cost, zero-emission
The process of environmental protection solves this problem, to promote the sound development of China's white carbon industry.
Summary of the invention
The invention provides sulfur acid sodium waste water treatment process in a kind of precipitated silica production process, solve background skill
Deficiency in art, this technique can process by waste water be applicable to the precipitated silica production process of different component, it is possible to returns
Receive the salinity in waste water, and recycle-water resource is reused.
Realizing the technical scheme that above-mentioned purpose of the present invention used is:
Sulfur acid sodium waste water treatment process in precipitated silica production process, comprises the following steps:
(1) content of the sodium sulfate, in first sample analysis sodium sulfate wastewater pond, is then re-fed in reaction tank, add with
The hexafluosilicic acid of sodium sulfate equimolar amounts, makes the sodium ion in waste water react generation prodan precipitation with hexafluosilicic acid, adds fluorine silicon
After acid, stir 30~45 minutes;It is re-fed in the first sedimentation tank precipitating prodan;
(2), the prodan slip solid-liquid separating equipment after precipitation is separated, isolated filtering residue tap water
Or deionized water wash, the most i.e. prepare prodan;The solution after precipitation prodan and the filtrate of solid-liquid separation
Merging is sent in neutralization pond standby together;
(3), continue in neutralization pond, add lime cream or precipitated calcium carbonate powder under conditions of stirring, be stirred for after adding
After 30~45 minutes, send into sulfate precipitate calcium in the second sedimentation tank;Clear water after sulfate precipitate calcium is re-fed in regulating reservoir standby;
Calcium sulfate slip after precipitation is with being pumped into filter pressing in pressure filter, and filter pressing gained filtrate is sent in regulating reservoir equally, filter pressing gained
Filter cake tap water or deionized water wash, to after neutrality, the most i.e. prepare calcium sulfate;
(4), under conditions of stirring, in regulating reservoir, add oxalic acid, stir 30~45 minutes, stop stirring, then it is sent
Enter precipitation calcium oxalate in the 3rd sedimentation tank;Clear water after precipitation calcium oxalate the most directly stores standby;Oxalic acid after precipitation
Calcium slip with being pumped into filter pressing in pressure filter, filter pressing gained filter cake tap water or deionized water wash, the most i.e. prepare grass
Acid calcium.
The waste water of sulfur acid sodium is first concentrated in (1) by step, and after concentration, isolated clear water directly stores standby, dense
Concentrated solution after contracting detects sodium sulphate content therein again.
Use plural serial stage electrodialysis or multistage nanofiltration or multi-stage reverse osmosis device to concentrate, or by series electrical dialysis,
Nanofiltration and reverse osmosis unit carry out concentration to waste water after being combined.
In step (4) first after the calcium ion concentration in sample analysis regulating reservoir, then according to calcium ion concentration to regulation
Pond adds the oxalic acid of equimolar quality.
In technical scheme provided by the present invention, as follows for the sodium sulfate reaction principle in waste water:
Na2SO4+H2SiF6=Na2SiF6↓+H2SO4
H2SO4+Ca(OH)2=CaSO4↓+2H2O
Or H2SO4+CaCO3=CaSO4↓+H2O+CO2↑
Ca(OH)2+H2C2O4=CaC2O4↓+2H2O
Or CaCO3+H2C2O4=CaC2O4↓+H2O+CO2↑
Above-mentioned technique provided by the present invention has the advantage that 1, the salinity in waste water can be carried out back by the present invention
Receive, prepare prodan, calcium sulfate, calcium oxalate.2, the clear water obtained after processing in the present invention can directly return to workshop to be carried out
Use, really realize zero-emission.
Detailed description of the invention
With example, process of the present invention is described below, should not be understood as limiting the technological parameter do not invented.
Embodiment 1
As a example by the sodium sulfate wastewater that the present embodiment produces in the precipitated silica production process of Fujian company, illustrate
The process of the present invention:
In the first sample analysis sodium sulfate wastewater pond of step 1 standby after sodium sulphate content and pH value;
Step 2 with in the reaction tank being pumped into, after measuring its volume, opens stirring the sodium sulfate wastewater in step 1, then
It is slowly added into and the industrial by-product silicate fluoride solution of the sodium sulfate equimolar quality in waste water.After adding silicate fluoride solution, stirring
After mixing 30 minutes, stop stirring, add flocculant while material being sent into the first sedimentation tank with pump with rapid precipitation hexafluosilicic acid
Sodium.Prodan slip bottom sedimentation tank with being pumped into filter pressing in pressure filter, filter cake tap water or deionized water wash three
After secondary, drying plant is sent to sell as commodity prodan after drying;The clear water containing sulphuric acid after precipitation prodan and pressure
Vitriolated clear water in filter separation process is standby with being pumped in neutralization pond again.
Step 3 the most slowly adds equimolar quality or slight excess of lightweight carbonic acid under conditions of stirring in neutralization pond
Calcium powder, after being stirred for 30 minutes after adding.Again be pumped into while the second sedimentation tank precipitates add flocculant with quickly
Sulfate precipitate calcium.Clear water after sulfate precipitate calcium is re-fed in regulating reservoir standby;Calcium sulfate slip bottom second sedimentation tank is used
Being pumped into filter pressing in pressure filter, filtrate is sent in regulating reservoir, after filter cake tap water or deionized water wash to neutrality, send dry
Workshop is sold as commodity calcium sulfate after drying.
After calcium ion concentration in step 4 sample analysis regulating reservoir, under conditions of stirring, in regulating reservoir, addition etc. rubs
The oxalic acid of your quality, stirs 30 minutes, stops stirring.Pump is sent to add flocculant with soon while it is sent into the 3rd sedimentation tank again
Speed precipitation calcium oxalate.Precipitation calcium oxalate after clear water be re-fed into after filtering from the beginning pond for workshop.Oxalic acid after precipitation
Calcium slip, with being pumped into filter pressing in pressure filter, after filter cake tap water or deionized water wash three times, send drying plant dried
Sell as commodity calcium oxalate.
Embodiment 2
For as a example by the waste water of the sulfur acid sodium that the present embodiment produces in Hubei company precipitated silica production process
Bright process of the present invention
Step 1 is concentrating in the wastewater collection of sulfur acid sodium to wastewater disposal basin, and after concentration, isolated clear water directly stores standby
With, the concentrated solution after concentration is sent in special reserve pool standby, the sodium sulphate content in sample analysis concentrated solution and pH value standby
With;
Step 2 with in the reaction tank being pumped into, after measuring its volume, is opened the waste water in step 1 stirring, is more slowly added
Enter and the industrial by-product silicate fluoride solution of the sodium ion equimolar quality in waste water.After adding silicate fluoride solution, stirring 30 points
Zhong Hou, stops stirring, adds flocculant with rapid precipitation prodan while material being sent into the first sedimentation tank with pump.Precipitation
Prodan slip bottom pond, with being pumped into filter pressing in pressure filter, after filter cake tap water or deionized water wash three times, send
Drying plant is sold as commodity prodan after drying;The clear water containing sulphuric acid after precipitation prodan is again with in being pumped into
Standby with in pond.
Step 3 the most slowly adds equimolar quality or slight excess of lime cream under conditions of stirring in neutralization pond,
45 minutes it are stirred for after adding.Again be pumped into while the second sedimentation tank precipitates add flocculant with rapid precipitation sulphuric acid
Calcium.Clear water after sulfate precipitate calcium is re-fed in regulating reservoir standby;Calcium sulfate slip bottom second sedimentation tank is with being pumped into pressure
Filter pressing in filter, filtrate sends in regulating reservoir, after filter cake tap water or deionized water wash to neutrality, send drying plant to be dried
Sell as commodity calcium sulfate afterwards.
After calcium ion concentration in step 4 sample analysis regulating reservoir, under conditions of stirring, in regulating reservoir, addition etc. rubs
The oxalic acid of your quality, stirs 45 minutes, stops stirring.Pump is sent to add flocculant with soon while it is sent into the 3rd sedimentation tank again
Speed precipitation calcium oxalate.Precipitation calcium oxalate after clear water be re-fed into after filtering from the beginning pond for workshop.Oxalic acid after precipitation
Calcium slip, with being pumped into filter pressing in pressure filter, after filter cake tap water or deionized water wash three times, send drying plant dried
Sell as commodity calcium oxalate.
Claims (4)
1. sulfur acid sodium waste water treatment process in precipitated silica production process, it is characterised in that comprise the following steps:
(1) content of the sodium sulfate, in first sample analysis sodium sulfate wastewater pond, is then re-fed in reaction tank, adds and sulphuric acid
The hexafluosilicic acid of sodium equimolar amounts, makes the sodium ion in waste water react generation prodan precipitation with hexafluosilicic acid, after adding hexafluosilicic acid,
Stir 30~45 minutes;It is re-fed in the first sedimentation tank precipitating prodan;
(2), the prodan slip solid-liquid separating equipment after precipitation is separated, isolated filtering residue tap water or go
Ionized water washs, and the most i.e. prepares prodan;Solution after precipitation prodan and during isolated filtrate sends in the lump
Standby with in pond;
(3), continue in neutralization pond, add lime cream or precipitated calcium carbonate powder under conditions of stirring, be stirred for after adding 30~
After 45 minutes, send into sulfate precipitate calcium in the second sedimentation tank;Clear water after sulfate precipitate calcium is re-fed in regulating reservoir standby;Precipitation
After calcium sulfate slip with being pumped into filter pressing in pressure filter, filter pressing gained filtrate is sent in regulating reservoir equally, filter pressing gained filter cake
After tap water or deionized water wash to neutrality, the most i.e. prepare calcium sulfate;
(4), under conditions of stirring, in regulating reservoir, add oxalic acid, stir 30~45 minutes, stop stirring, then its feeding the
Three sedimentation tanks precipitate calcium oxalate;Clear water after precipitation calcium oxalate the most directly stores standby;Calcium oxalate material after precipitation
Starch with being pumped into filter pressing in pressure filter, filter pressing gained filter cake tap water or deionized water wash, the most i.e. prepare calcium oxalate.
Waste water treatment process the most according to claim 1, it is characterised in that: first by the waste water of sulfur acid sodium in step (1)
Concentrating, after concentration, isolated clear water directly stores standby, and the concentrated solution after concentration detects sodium sulphate content therein again.
Waste water treatment process the most according to claim 2, it is characterised in that: use plural serial stage electrodialysis or multistage nanofiltration
Or multi-stage reverse osmosis device concentrates, or waste water is entered after series electrical dialysis, nanofiltration and reverse osmosis unit are combined
Row concentration.
Waste water treatment process the most according to claim 1, it is characterised in that: first sample analysis regulating reservoir in step (4)
In calcium ion concentration after, in regulating reservoir, then add the oxalic acid of equimolar quality according to calcium ion concentration.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106976945A (en) * | 2017-04-11 | 2017-07-25 | 天津理工大学 | Removing sodium containing sodium-salt aqueous solution under a kind of sour environment |
CN108439647A (en) * | 2018-04-18 | 2018-08-24 | 浙江森友环保成套设备有限公司 | A kind for the treatment of process of concrete mixing plant waste water |
CN114394712A (en) * | 2022-01-27 | 2022-04-26 | 安徽中科莘阳膜科技有限公司 | Integrated device and method for extracting high-purity mirabilite from white carbon black production wastewater |
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CN102020281A (en) * | 2010-12-30 | 2011-04-20 | 甘肃锦世化工有限责任公司 | Method for producing sodium fluosilicate by utilizing waste water containing sodium sulfate |
CN201882936U (en) * | 2010-12-09 | 2011-06-29 | 河南煤业化工集团有限责任公司 | ADC foamer condensation mother liquor and washes recycle device |
CN102492994A (en) * | 2011-12-23 | 2012-06-13 | 吉林大学 | Method for preparing calcium sulfate whiskers by using white carbon black industrial wastewater |
CN102602946A (en) * | 2012-03-21 | 2012-07-25 | 陈君华 | Method for preparing high-specific-surface white carbon black by circularly utilizing waste water including sodium sulfate |
-
2016
- 2016-08-08 CN CN201610643670.4A patent/CN106277478A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN201882936U (en) * | 2010-12-09 | 2011-06-29 | 河南煤业化工集团有限责任公司 | ADC foamer condensation mother liquor and washes recycle device |
CN102020281A (en) * | 2010-12-30 | 2011-04-20 | 甘肃锦世化工有限责任公司 | Method for producing sodium fluosilicate by utilizing waste water containing sodium sulfate |
CN102492994A (en) * | 2011-12-23 | 2012-06-13 | 吉林大学 | Method for preparing calcium sulfate whiskers by using white carbon black industrial wastewater |
CN102602946A (en) * | 2012-03-21 | 2012-07-25 | 陈君华 | Method for preparing high-specific-surface white carbon black by circularly utilizing waste water including sodium sulfate |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106976945A (en) * | 2017-04-11 | 2017-07-25 | 天津理工大学 | Removing sodium containing sodium-salt aqueous solution under a kind of sour environment |
CN108439647A (en) * | 2018-04-18 | 2018-08-24 | 浙江森友环保成套设备有限公司 | A kind for the treatment of process of concrete mixing plant waste water |
CN114394712A (en) * | 2022-01-27 | 2022-04-26 | 安徽中科莘阳膜科技有限公司 | Integrated device and method for extracting high-purity mirabilite from white carbon black production wastewater |
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