CN108607504A - Phosphatic method in water removal is gone with the waste acetic acid containing rare earth - Google Patents
Phosphatic method in water removal is gone with the waste acetic acid containing rare earth Download PDFInfo
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- CN108607504A CN108607504A CN201810269617.1A CN201810269617A CN108607504A CN 108607504 A CN108607504 A CN 108607504A CN 201810269617 A CN201810269617 A CN 201810269617A CN 108607504 A CN108607504 A CN 108607504A
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- acetic acid
- water
- waste acetic
- rare earth
- waste
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres
-
- 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
- C02F2101/105—Phosphorus compounds
Abstract
The present invention goes phosphatic method in water removal with the waste acetic acid containing rare earth, includes the following steps:(1) the waste acetic acid containing rare earth is selected:It selects in rice white, powdered, average grain diameter is 68.65 μm, specific surface area 211.92m2/ g, the waste acetic acid containing rare-earth elements of lanthanum and cerium are as raw material;(2) roast:In Muffle furnace 100~180min is roasted in 500~800 DEG C;(3) cool down:It is cooled to room temperature in drier;(4) the pH of phosphorous water is adjusted;(5) adsorption reaction is carried out;(6) it is separated by solid-liquid separation and is measured, is tested under 700nm wavelength with ammonium molybdate spectrophotometric method, using spectrophotometer;The present invention is to phosphatic removal rate in water up to 90% or more, and whole process is generated without waste liquid, waste residue, and secondary pollution is not present;And it is easy to operate, it is cheap, it is a technology benefited the nation and the people.
Description
Technical field
The present invention relates to dead catalyst recycling and water-treatment technology fields, relate to the use of waste acetic acid processing
The technology of water particularly goes phosphatic method in water removal with the waste acetic acid containing rare earth.
Background technology
Catalytic cracking catalyst (FCC) is the maximum catalyst of petroleum refining industry's usage amount and catalytic cracking process application
Most commonly used catalyst.In catalytic cracking process, vanadium, nickel, iron, arsenic, lead, copper in the crude oil of heavy oil catalytic cracking etc.
Heavy metal can be accumulated on useless catalytic cracking catalyst, causing the selectivity of the catalyst to decline, and activity reduces, can not
Continue the requirement for meeting oil refining process.Therefore, the industries such as petroleum refining industry of China can all generate a large amount of useless catalytic cracking every year
Catalyst.
Currently, being mainly to being mainly that recycling recycles with the processing method of useless catalytic cracking catalyst in the industry
It is regenerated using useless catalytic cracking catalyst using magnetic method and medicament method of reproduction, selectively recycling activity is higher with useless
Catalytic cracking catalyst, or repeat to use using useless catalytic cracking catalyst recovered part activity.In addition, also one
A little researchs and report, such as:Valuable metal is recycled from useless catalytic cracking catalyst;As construction timber;As production
The raw material of cement, exquisite carclazyte.
Phosphorus is one of main matter of body eutrophication.The too high levels of phosphorus can be such that oxygen in water (DO) drops in water body
Low, algae overgrowing can cause a large amount of aquatiles dead, and water body becomes mixed, smelly, not only pollutes environment, but also more influence the mankind
Existence and health --- directly affect the drinking water source of the mankind.According to investigations, there are the lake of 30%-40%, reservoir in the current whole world
There are eutrophications.Therefore, the dephosphorization agent for researching and developing economical and efficient has become the task of top priority of protection environment for human survival.
Contain larger specific surface area with useless catalytic cracking catalyst, contain about 20% zeolite component, thus has
Preferable absorption property.Zeolite is a kind of aqueous porous silicoaluminate mineral with rack-like structure, and skeleton is mainly by silicon
The three-dimensional framework cyclic structure that oxygen tetrahedron is composed by bridging oxygen rule.It gives up currently, zeolite has been widely used for removal
The pollutants such as ammonia nitrogen, phosphate radical, heavy metal ion in water.Experimental configuration shows:Natural zeolite to the removal effect of ammonia nitrogen very
It is good, but it is bad to the removal effect of phosphorus.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of with the waste acetic acid containing rare earth
Go phosphatic method in water removal.Phosphorus is gone the study found that being modified to natural zeolite with rare earth element and can improve zeolite
Except efficiency, and the rare earth element that 2%~4% (wt) is typically contained with useless catalytic cracking catalyst that China is common, if energy
The phosphorus in water removal enough is removed using it, can not only be turned waste into wealth --- make full use of the industries such as petroleum refining industry to generate a large amount of with useless
Catalytic cracking catalyst, support the development of the industries such as petroleum refining industry, and the phosphorus in water removal can be removed, prevent lake, reservoir
Eutrophication administers the lake of eutrophication and reservoir, reaches the positive social effect benefited the nation and the people.
To achieve the above object, this invention takes following technical schemes.
It is a kind of with the waste acetic acid containing rare earth go water removal in phosphatic method, which is characterized in that including with
Lower step:
(1) waste acetic acid containing rare earth is selected
It selects in rice white, powdered, average grain diameter is 68.65 μm, specific surface area 211.92m2/ g, contain rare earth element
The waste acetic acid of lanthanum (La) and cerium (Ce) is as raw material;
(2) it roasts
By the selected waste acetic acid raw material of step (1) in Muffle furnace in 500~800 DEG C roast 100~
180min makes remaining organic matter in waste acetic acid decompose and volatilize, also makes toxic heavy metal substance therein solid
It is melted into inert substance, reduces its toxicity and migration in the environment;
(3) cooling
Waste acetic acid after step (2) is roasted, which is placed in drier, to be cooled to room temperature, standby as adsorbent
With;
(4) pH of phosphorous water is adjusted
The phosphorous water of 100mL is added in reaction bulb, the pH of the phosphorous water is adjusted to 2 using acid solution or aqueous slkali
~10, then add 2~12g/L of adsorbent of step (3);
(5) adsorption reaction is carried out
The reaction bulb of step (4) is jumped a queue and is placed in water bath with thermostatic control oscillation case, in 10~40 DEG C of reaction temperature, rotating speed
Adsorption reaction is carried out under 100~200r/min, takes out reaction bulb after 30~600min of adsorption reaction;
(6) it is separated by solid-liquid separation and is measured
Step (5) reaction bulb is stood, so that the liquid in reaction bulb is urged with useless catalytic cracking using the method for gravitational settling
Agent realize be separated by solid-liquid separation, taken after supernatant liquid is centrifuged supernatant or filtering after take filtrate, with ammonium molybdate spectrophotometric method into
The measurement of row phosphate concn:The phosphate content adsorbed in front and back solution is tested under 700nm wavelength using spectrophotometer,
Calculate phosphatic removal rate.
Further, the content point of the waste acetic acid rare earth elements lanthanum (La) and cerium (Ce) of step (1) selection
It Wei not 1.01% (wt) and 2.08% (wt).
Further, step (4) the phosphorous water is that potassium dihydrogen phosphate is formulated with deionized water or actual contains
Phosphorus waste water, phosphatic a concentration of 0.5~10.0mg/L in phosphorous water.
The present invention goes the good effect of phosphatic method in water removal to be with the waste acetic acid containing rare earth:
(1) it is used for waste acetic acid to remove the phosphate in water removal, not only realizes waste acetic acid
Harmlessness disposing, and can become and give up as a kind of new resource, support the development of the industries such as petroleum refining industry, meet clean manufacturing
With the theory of sustainable development.
(2) phosphate in water removal is removed with the waste acetic acid containing rare earth, it is reachable to phosphatic removal rate in water
90% or more, highest to can reach 99%, phosphatic concentration is less than 0.5mg/L in water outlet, and whole process is without waste liquid, waste residue
It generates, secondary pollution is not present.
(3) phosphor-removing effect of the invention is good, easy to operate, cheap;The industries such as petroleum refining industry generate a large amount of useless
Catalytic cracking catalyst can meet improvement of the large area containing phosphorus water, be a positive technology success benefited the nation and the people.
Description of the drawings
Fig. 1 is the flow diagram that the present invention goes phosphatic method in water removal with the waste acetic acid containing rare earth.
Specific implementation mode
The present invention presented below goes the specific reality of phosphatic method in water removal with the waste acetic acid containing rare earth
Mode is applied, 5 embodiments are provided, it should be noted that the implementation embodiment not limited to the following of the present invention.
Embodiment 1
It is a kind of to go phosphatic method in water removal with the waste acetic acid containing rare earth, include the following steps:
(1) waste acetic acid containing rare earth is selected
It selects in rice white, powdered, average grain diameter is 68.65 μm, specific surface area 211.92m2/ g, rare-earth elements of lanthanum
(La) and the content of cerium (Ce) is respectively the waste acetic acid of 1.01% (wt) and 2.08% (wt) as raw material.
(2) it roasts
The selected waste acetic acid raw material of step (1) is roasted into 100min in 500 DEG C in Muffle furnace, makes to give up
Remaining organic matter is decomposed and is volatilized in catalytic cracking catalyst, and toxic heavy metal substance therein is also made to be solidified into inert material
Matter reduces its toxicity and migration in the environment.
(3) cooling
Waste acetic acid after step (2) is roasted, which is placed in drier, to be cooled to room temperature, standby as adsorbent
With.
(4) pH of phosphorous water is adjusted
The phosphorus that initial phosphate concentration made of 100mL is configured by potassium dihydrogen phosphate is 0.5mg/L is added in reaction bulb
The pH of the phosphorus solution is adjusted to 2 by solution using acid solution or aqueous slkali, then adds the adsorbent 2g/L of step (3).
(5) adsorption reaction is carried out
The reaction bulb of step (4) is jumped a queue and is placed in water bath with thermostatic control oscillation case, in 10 DEG C of reaction temperature, rotating speed 100r/
Adsorption reaction is carried out under min, takes out reaction bulb after adsorption reaction 600min.
(6) it is separated by solid-liquid separation and is measured
The reaction bulb of step (5) is stood, the liquid in reaction bulb and useless catalytic cracking are made using the method for gravitational settling
Catalyst, which is realized, to be separated by solid-liquid separation, and takes supernatant after supernatant liquid is centrifuged, phosphate concn is carried out with ammonium molybdate spectrophotometric method
Measurement:The phosphate content adsorbed in front and back solution is tested under 700nm wavelength using spectrophotometer, calculates phosphate
Removal rate.
The test result of embodiment 1 shows:Under the reaction condition of the phosphorus removing method of embodiment 1, the useless catalysis containing rare earth
Cracking catalyst reaches 90% to phosphatic removal rate in water, and phosphatic concentration is less than 0.1mg/L in water outlet.
Embodiment 2
It is a kind of to go phosphatic method in water removal with the waste acetic acid containing rare earth, include the following steps:
(1) select the waste acetic acid containing rare earth (with embodiment 1).
(2) it roasts
The selected waste acetic acid raw material of step (1) is roasted into 180min in Muffle furnace in 800 DEG C, other
With embodiment 1.
(3) cooling (with embodiment 1).
(4) pH of phosphorous water is adjusted
The phosphorus that initial phosphate concentration made of 100mL is configured by potassium dihydrogen phosphate is 5.0mg/L is added in reaction bulb
The pH of the phosphorus solution is adjusted to 10 by solution using acid solution or aqueous slkali, then adds the adsorbent 12g/L of step (3).
(5) adsorption reaction is carried out
The reaction bulb of step (4) is jumped a queue and is placed in water bath with thermostatic control oscillation case, in 40 DEG C of reaction temperature, rotating speed 200r/
Adsorption reaction is carried out under min, takes out reaction bulb after adsorption reaction 30min.
(6) it is separated by solid-liquid separation and is measured (with embodiment 1)
The test result of embodiment 2 shows:Under the reaction condition of the phosphorus removing method of embodiment 2, the useless catalysis containing rare earth
Cracking catalyst reaches 90% to phosphatic removal rate in water, and phosphatic concentration is less than 0.5mg/L in water outlet.
Embodiment 3
It is a kind of to go phosphatic method in water removal with the waste acetic acid containing rare earth, include the following steps:
(1) select the waste acetic acid containing rare earth (with embodiment 1).
(2) it roasts
The selected waste acetic acid raw material of step (1) is roasted into 120min in Muffle furnace in 600 DEG C, other
With embodiment 1.
(3) cooling (with embodiment 1).
(4) pH of phosphorous water is adjusted
The phosphorus that initial phosphate concentration made of 100mL is configured by potassium dihydrogen phosphate is 1.0mg/L is added in reaction bulb
The pH of the phosphorus solution is adjusted to 6 by solution using acid solution or aqueous slkali, then adds the adsorbent 5g/L of step (3).
(5) adsorption reaction is carried out
The reaction bulb of step (4) is jumped a queue and is placed in water bath with thermostatic control oscillation case, in 25 DEG C of reaction temperature, rotating speed 180r/
Adsorption reaction is carried out under min, takes out reaction bulb after adsorption reaction 120min.
(6) it is separated by solid-liquid separation and is measured (with embodiment 1)
The test result of embodiment 3 shows:Under the reaction condition of the phosphorus removing method of embodiment 3, the useless catalysis containing rare earth
Cracking catalyst reaches 99% to phosphatic removal rate in water, and phosphatic concentration is less than 0.1mg/L in water outlet.
Embodiment 4
It is a kind of to go phosphatic method in water removal with the waste acetic acid containing rare earth, include the following steps:
(1) select the waste acetic acid containing rare earth (with embodiment 1).
(2) it roasts
The selected waste acetic acid raw material of step (1) is roasted into 120min in Muffle furnace in 600 DEG C, other
With embodiment 1.
(3) cooling (with embodiment 1).
(4) pH of phosphorous water is adjusted
It is molten that the phosphorus that initial phosphate concentration is 10.0mg/L made of the configuration of 100mL potassium dihydrogen phosphates is added into reaction bulb
The pH of the phosphorus solution is adjusted to 6 by liquid using acid solution or aqueous slkali, then adds the adsorbent 12g/L of step (3).
(5) adsorption reaction is carried out
The reaction bulb of step (4) is jumped a queue and is placed in water bath with thermostatic control oscillation case, in 40 DEG C of reaction temperature, rotating speed 180r/
Adsorption reaction is carried out under min, takes out reaction bulb after adsorption reaction 120min.
(6) it is separated by solid-liquid separation and is measured
Step (5) reaction bulb is stood, so that the liquid in reaction bulb is urged with useless catalytic cracking using the method for gravitational settling
Agent, which is realized, to be separated by solid-liquid separation, and takes filtrate after supernatant liquid is filtered, the measurement of phosphorus concentration is carried out with ammonium molybdate spectrophotometric method:Make
The phosphate content adsorbed in front and back solution is tested under 700nm wavelength with spectrophotometer, calculates phosphatic removal rate.
The test result of embodiment 4 shows:Under the reaction condition of the phosphorus removing method of embodiment 4, the useless catalysis containing rare earth
Cracking catalyst reaches 90% to phosphatic removal rate in water, and phosphatic concentration is less than 0.5mg/L in water outlet.
Embodiment 5
A kind of phosphatic method in the waste acetic acid removal actual waste water containing rare earth, including following step
Suddenly:
(1) select the waste acetic acid containing rare earth (with embodiment 1).
(2) it roasts
The selected waste acetic acid raw material of step (1) is roasted into 120min in Muffle furnace in 600 DEG C, other
With embodiment 1.
(3) cooling (with embodiment 1).
(4) pH of phosphorous water is adjusted
The actual waste water that 100mL initial phosphate concentrations are 3.8mg/L is added into reaction bulb, uses acid solution or alkali
The pH of the phosphorus solution is adjusted to 6 by solution, then adds the adsorbent 8g/L of step (3).
(5) adsorption reaction is carried out
The reaction bulb of step (4) is jumped a queue and is placed in water bath with thermostatic control oscillation case, in 25 DEG C of reaction temperature, rotating speed 150r/
Adsorption reaction is carried out under min, takes out reaction bulb after adsorption reaction 120min.
(6) it is separated by solid-liquid separation and is measured
Step (5) reaction bulb is stood, so that the liquid in reaction bulb is urged with useless catalytic cracking using the method for gravitational settling
Agent, which is realized, to be separated by solid-liquid separation, and takes filtrate after supernatant liquid is filtered, the measurement of phosphorus concentration is carried out with ammonium molybdate spectrophotometric method:Make
The phosphate content adsorbed in front and back solution is tested under 700nm wavelength with spectrophotometer, calculates phosphatic removal rate.
The test result of embodiment 5 shows:Under the reaction condition of the phosphorus removing method of embodiment 5, the useless catalysis containing rare earth
Cracking catalyst reaches 90% to phosphatic removal rate in actual waste water, and phosphatic concentration is less than 0.5mg/L in water outlet.
When phosphatic initial concentration is 5mg/L in phosphorous water, the dosage of waste acetic acid is 5g/L, reaction
Temperature is 25 DEG C, and when the reaction time is 2h, the phosphor-removing effect of waste acetic acid is as shown in table 1 under different pH value.By table 1
As it can be seen that waste acetic acid can realize that good phosphor-removing effect, phosphatic removal rate reach in the range of pH is 2~10
To 92% or more.
The phosphor-removing effect of waste acetic acid under the different pH value of table 1.
When phosphatic initial concentration is 5mg/L in phosphorous water, the dosage of waste acetic acid is 5g/L, solution
Initial pH value be 7, the reaction time be 2h when, the phosphor-removing effect of waste acetic acid such as 2 institute of table at a temperature of differential responses
Show.As shown in Table 2, waste acetic acid can realize good phosphor-removing effect, phosphorus in the range of temperature is 10~40 DEG C
The removal rate of hydrochlorate reaches 92% or more.
The phosphor-removing effect of waste acetic acid at a temperature of 2. differential responses of table
Claims (3)
1. a kind of going phosphatic method in water removal with the waste acetic acid containing rare earth, which is characterized in that including following
Step:
(1) waste acetic acid containing rare earth is selected
It selects in rice white, powdered, average grain diameter is 68.65 μm, specific surface area 211.92m2/ g, containing rare-earth elements of lanthanum and
The waste acetic acid of cerium is as raw material;
(2) it roasts
By the selected waste acetic acid raw material of step (1) in Muffle furnace in 500~800 DEG C roast 100~
180min makes remaining organic matter in waste acetic acid decompose and volatilize, also makes toxic heavy metal substance therein solid
It is melted into inert substance, reduces its toxicity and migration in the environment;
(3) cooling
Waste acetic acid after step (2) is roasted, which is placed in drier, to be cooled to room temperature, spare as adsorbent;
(4) pH of phosphorous water is adjusted
The phosphorous water of 100mL is added in reaction bulb, the pH of the phosphorous water is adjusted to 2 using acid solution or aqueous slkali~
10, then add 2~12g/L of adsorbent of step (3);
(5) adsorption reaction is carried out
The reaction bulb of step (4) is jumped a queue be placed on water bath with thermostatic control oscillation case in, 10~40 DEG C of reaction temperature, rotating speed 100~
Adsorption reaction is carried out under 200r/min, takes out reaction bulb after 30~600min of adsorption reaction;
(6) it is separated by solid-liquid separation and is measured
Step (5) reaction bulb is stood, the liquid in reaction bulb and waste acetic acid are made using the method for gravitational settling
It realizes and is separated by solid-liquid separation, take filtrate after supernatant or filtering are taken after supernatant liquid is centrifuged, phosphorus is carried out with ammonium molybdate spectrophotometric method
The measurement of hydrochlorate concentration:The phosphate content adsorbed in front and back solution is tested under 700nm wavelength using spectrophotometer, is calculated
Go out phosphatic removal rate..
2. according to claim 1 go phosphatic method in water removal with the waste acetic acid containing rare earth, special
Sign is, the waste acetic acid rare earth elements lanthanum of step (1) selection and the content of cerium be respectively 1.01%wt and
2.08%wt.
3. according to claim 1 go phosphatic method in water removal with the waste acetic acid containing rare earth, special
Sign is that step (4) the phosphorous water is phosphorus-containing wastewater that potassium dihydrogen phosphate is formulated with deionized water or actual, is contained
Phosphatic a concentration of 0.5~10.0mg/L in phosphorus water.
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CN1817439A (en) * | 2006-01-17 | 2006-08-16 | 昆明理工大学 | Rare earth adsorbent and production thereof |
CN101607192A (en) * | 2009-07-14 | 2009-12-23 | 昆明理工大学 | A kind of method of molding rare earth absorbent |
CN102380343A (en) * | 2011-08-31 | 2012-03-21 | 环境保护部华南环境科学研究所 | Simultaneous nitrogen and phosphorus removal modified artificial zeolite for micro-polluted water, and preparation method thereof |
CN105921103A (en) * | 2016-05-19 | 2016-09-07 | 四川理工学院 | Preparation method of La(OH)3 modified kieselguhr and molecular sieve adsorption material for simultaneously fixing nitrogen and phosphorus |
CN106607006A (en) * | 2016-11-25 | 2017-05-03 | 环境保护部华南环境科学研究所 | Preparation method for adsorbent capable of removing nitrogen and phosphorus simultaneously |
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CN1817439A (en) * | 2006-01-17 | 2006-08-16 | 昆明理工大学 | Rare earth adsorbent and production thereof |
CN101607192A (en) * | 2009-07-14 | 2009-12-23 | 昆明理工大学 | A kind of method of molding rare earth absorbent |
CN102380343A (en) * | 2011-08-31 | 2012-03-21 | 环境保护部华南环境科学研究所 | Simultaneous nitrogen and phosphorus removal modified artificial zeolite for micro-polluted water, and preparation method thereof |
CN105921103A (en) * | 2016-05-19 | 2016-09-07 | 四川理工学院 | Preparation method of La(OH)3 modified kieselguhr and molecular sieve adsorption material for simultaneously fixing nitrogen and phosphorus |
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