CN108176352A - A kind of inorganic agent of treated sewage and its preparation method and application - Google Patents

A kind of inorganic agent of treated sewage and its preparation method and application Download PDF

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Publication number
CN108176352A
CN108176352A CN201810010157.0A CN201810010157A CN108176352A CN 108176352 A CN108176352 A CN 108176352A CN 201810010157 A CN201810010157 A CN 201810010157A CN 108176352 A CN108176352 A CN 108176352A
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parts
inorganic agent
temperature
hexamethylenetetramine
treated sewage
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成伟
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Shangrao Normal University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/42Treatment of water, waste water, or sewage by ion-exchange
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/103Arsenic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Dispersion Chemistry (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of inorganic agent of treated sewage and its preparation method and application, which includes according to the raw material of parts by weight:18 26 parts of vermiculite, 11 19 parts of hexamethylenetetramine, 7 15 parts of polyoxyethylene ether, 48 parts of ethyl cellulose.By vermiculite, ethyl cellulose co-grinding, hexamethylenetetramine solution is then added in, first heating stirring processing after sealing;Then polyoxyethylene ethereal solution is added in, heating stirring is handled after sealing, washs drying;5h is calcined at a temperature of 260 DEG C to obtain the final product.Energy effective Adsorption of Mercury, arsenic, nickel ion of the invention, there is very strong adsorption capacity and ion-exchange capacity to heavy metal ion, in should being handled to heavy metal ions in wastewater, adsorption capacity is big, adsorption capacity is strong, efficient, and processed waste water reaches the discharge standard of country.Properties of product of the present invention are stablized, and repeat and utilize, and the secondary effective percentage used can reach the 95% of first time using effect, and performance is still very stable after calcining again, suitable for industrialized production.

Description

A kind of inorganic agent of treated sewage and its preparation method and application
Technical field
The present invention relates to technical field of sewage, inorganic agent of specifically a kind of treated sewage and preparation method thereof and should With.
Background technology
Water pollution caused by heavy metal ion is the severe environmental problem that the whole world faces, and chromium, cadmium and lead are to draw The Heavy Metals ion of water pollution is played, wherein, the content of cadmium and lead is generally up to, maximum to human health risk.According to generation Boundary's Health Organization criterion, the highest content of cadmium and lead is not above 0.003 and 0.01mg/g in drinking water.Currently used for removal weight The method of metal ion mainly includes UF membrane, and the methods of acid-base neutralization, sedimentation, but cost is higher, and periodically long and reaction is difficult Its extensive commercial application is limited with control.
Heavymetal Wastewater Treatment by Adsorption has efficient, easy and good selective.Common sorbing material is active Charcoal, humic acid, sepiolite, polysaccharide resins etc..But the sorbing material industrially used at present is expensive, and extensive use is limited System.And although vermiculite is that raw material is commonly used in sorbing material field, but itself poor processing effect, need supersonic high temperature calcining etc. It handles or the compounding side of being made is mixed with other raw materials with suction-operated with significant effect, expanded after high-temperature calcination Make its structural instability, performance is unstable.
Invention content
It is above-mentioned to solve the purpose of the present invention is to provide a kind of inorganic agent of treated sewage and its preparation method and application The problem of being proposed in background technology.
To achieve the above object, the present invention provides following technical solution:
A kind of inorganic agent of treated sewage, includes according to the raw material of parts by weight:18-26 parts of vermiculite, hexamethylenetetramine 11- 19 parts, 7-15 parts of polyoxyethylene ether, 4-8 parts of ethyl cellulose.
As further embodiment of the present invention:The inorganic agent of the treated sewage includes according to the raw material of parts by weight:Vermiculite 20-24 parts, 13-17 parts of hexamethylenetetramine, 9-13 parts of polyoxyethylene ether, 5-7 parts of ethyl cellulose.
As further embodiment of the present invention:The inorganic agent of the treated sewage includes according to the raw material of parts by weight:Vermiculite 22 parts, 15 parts of hexamethylenetetramine, 11 parts of polyoxyethylene ether, 6 parts of ethyl cellulose.
A kind of preparation method of the inorganic agent of treated sewage, includes the following steps:
1) deionized water of 4-5 times of hexamethylenetetramine and its quality is mixed, hexamethylenetetramine solution is made;It will be poly- The ethyl alcohol of 6-7 times of ethylene oxide ether and its quality mixes, and polyoxyethylene ethereal solution is made;
2) by vermiculite, excessively ethyl cellulose co-grinding, 150-200 mesh sieve, hexamethylenetetramine solution is then added in, it is close It is honored as a queen and is first warming up to 83-85 DEG C and at such a temperature stir process 1.4-1.5h, then heat to 116-120 DEG C and in the temperature Lower stir process 85-90min, is cooled to room temperature;Then polyoxyethylene ethereal solution is added in, 68-71 DEG C is first warming up to after sealing simultaneously Stir process 55-60min at such a temperature then heats to 133-135 DEG C and at such a temperature stir process 48-53min, so After be warming up to 150-155 DEG C and at such a temperature stir process 40-45min, be down to room temperature, filtering removal filtrate, taking precipitate, Wash drying;Mixture A is made;
3) mixture A is calcined into 5h at a temperature of 260 DEG C to obtain the final product.
As further embodiment of the present invention:Washing, drying are to be washed with water, 100 DEG C of oven dryings.
As further embodiment of the present invention:In step 2), the speed of agitator added in after hexamethylenetetramine solution is 100r/min。
As further embodiment of the present invention:In step 2), the speed of agitator added in after polyoxyethylene ethereal solution is 220r/ min。
Another object of the present invention is to provide application of the inorganic agent in heavy metal-polluted water process.
Compared with prior art, the beneficial effects of the invention are as follows:
The present invention is handled vermiculite using hexamethylenetetramine, polyoxyethylene ether etc., through different temperatures stir process Inorganic agent obtained, energy effective Adsorption of Mercury, arsenic, nickel ion, has heavy metal ion very strong adsorption capacity and ion to hand over Transducing power, in should being handled to heavy metal ions in wastewater, adsorption capacity is big, adsorption capacity is strong, efficient, and processed waste water reaches The discharge standard of country.Properties of product of the present invention are stablized, and repeat and utilize, and the secondary effective percentage used can reach after calcining again The 95% of first time using effect, and performance is still very stable, suitable for industrialized production.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical solution in the embodiment of the present invention is clearly and completely described, Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based in the present invention Embodiment, those of ordinary skill in the art's all other embodiments obtained without making creative work, all Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of inorganic agent of treated sewage, including following raw material:Vermiculite 18kg, six methines four Amine 11kg, polyoxyethylene ether 7kg, ethyl cellulose 4kg.
4 times of deionized water of hexamethylenetetramine and its quality is mixed, hexamethylenetetramine solution is made;By polyoxy second The ethyl alcohol of 6 times of alkene ether and its quality mixes, and polyoxyethylene ethereal solution is made.By vermiculite, ethyl cellulose co-grinding, cross 150 Mesh sieves, and then adds in hexamethylenetetramine solution, 83 DEG C and at such a temperature stir process 1.4h is first warming up to after sealing, then It is warming up to 116 DEG C and at such a temperature stir process 85min, speed of agitator 100r/min.It is cooled to room temperature;Then it adds in poly- Ethylene oxide ethereal solution is first warming up to 68 DEG C and at such a temperature stir process 55min after sealing, then heat to 133 DEG C and Stir process 48min at this temperature then heats to 150 DEG C and stir process 40min, speed of agitator is at such a temperature 220r/min.Room temperature, filtering removal filtrate are down to, taking precipitate is washed with water, 100 DEG C of oven dryings;Mixture A is made.It will Mixture A calcines 5h at a temperature of 260 DEG C to obtain the final product.
Embodiment 2
In the embodiment of the present invention, a kind of inorganic agent of treated sewage, including following raw material:Vermiculite 26kg, six methines four Amine 19kg, polyoxyethylene ether 15kg, ethyl cellulose 8kg.
5 times of deionized water of hexamethylenetetramine and its quality is mixed, hexamethylenetetramine solution is made;By polyoxy second The ethyl alcohol of 7 times of alkene ether and its quality mixes, and polyoxyethylene ethereal solution is made.By vermiculite, ethyl cellulose co-grinding, cross 200 Mesh sieves, and then adds in hexamethylenetetramine solution, 85 DEG C and at such a temperature stir process 1.5h is first warming up to after sealing, then It is warming up to 120 DEG C and at such a temperature stir process 90min, speed of agitator 100r/min.It is cooled to room temperature;Then it adds in poly- Ethylene oxide ethereal solution is first warming up to 71 DEG C and at such a temperature stir process 60min after sealing, then heat to 135 DEG C and Stir process 53min at this temperature then heats to 155 DEG C and stir process 45min, speed of agitator is at such a temperature 220r/min.Room temperature, filtering removal filtrate are down to, taking precipitate is washed with water, 100 DEG C of oven dryings;Mixture A is made.It will Mixture A calcines 5h at a temperature of 260 DEG C to obtain the final product.
Embodiment 3
In the embodiment of the present invention, a kind of inorganic agent of treated sewage, including following raw material:Vermiculite 20kg, six methines four Amine 13kg, polyoxyethylene ether 9kg, ethyl cellulose 5kg.
5 times of deionized water of hexamethylenetetramine and its quality is mixed, hexamethylenetetramine solution is made;By polyoxy second The ethyl alcohol of 7 times of alkene ether and its quality mixes, and polyoxyethylene ethereal solution is made.By vermiculite, ethyl cellulose co-grinding, cross 200 Mesh sieves, and then adds in hexamethylenetetramine solution, 84 DEG C and at such a temperature stir process 1.5h is first warming up to after sealing, then It is warming up to 118 DEG C and at such a temperature stir process 90min, speed of agitator 100r/min.It is cooled to room temperature;Then it adds in poly- Ethylene oxide ethereal solution is first warming up to 70 DEG C and at such a temperature stir process 58min after sealing, then heat to 134 DEG C and Stir process 50min at this temperature then heats to 152 DEG C and stir process 45min, speed of agitator is at such a temperature 220r/min.Room temperature, filtering removal filtrate are down to, taking precipitate is washed with water, 100 DEG C of oven dryings;Mixture A is made.It will Mixture A calcines 5h at a temperature of 260 DEG C to obtain the final product.
Embodiment 4
In the embodiment of the present invention, a kind of inorganic agent of treated sewage, including following raw material:Vermiculite 24kg, six methines four Amine 17kg, polyoxyethylene ether 13kg, ethyl cellulose 7kg.
5 times of deionized water of hexamethylenetetramine and its quality is mixed, hexamethylenetetramine solution is made;By polyoxy second The ethyl alcohol of 7 times of alkene ether and its quality mixes, and polyoxyethylene ethereal solution is made.By vermiculite, ethyl cellulose co-grinding, cross 200 Mesh sieves, and then adds in hexamethylenetetramine solution, 84 DEG C and at such a temperature stir process 1.5h is first warming up to after sealing, then It is warming up to 118 DEG C and at such a temperature stir process 90min, speed of agitator 100r/min.It is cooled to room temperature;Then it adds in poly- Ethylene oxide ethereal solution is first warming up to 70 DEG C and at such a temperature stir process 58min after sealing, then heat to 134 DEG C and Stir process 50min at this temperature then heats to 152 DEG C and stir process 45min, speed of agitator is at such a temperature 220r/min.Room temperature, filtering removal filtrate are down to, taking precipitate is washed with water, 100 DEG C of oven dryings;Mixture A is made.It will Mixture A calcines 5h at a temperature of 260 DEG C to obtain the final product.
Embodiment 5
In the embodiment of the present invention, a kind of inorganic agent of treated sewage, including following raw material:Vermiculite 22kg, six methines four Amine 15kg, polyoxyethylene ether 11kg, ethyl cellulose 6kg.
5 times of deionized water of hexamethylenetetramine and its quality is mixed, hexamethylenetetramine solution is made;By polyoxy second The ethyl alcohol of 7 times of alkene ether and its quality mixes, and polyoxyethylene ethereal solution is made.By vermiculite, ethyl cellulose co-grinding, cross 200 Mesh sieves, and then adds in hexamethylenetetramine solution, 84 DEG C and at such a temperature stir process 1.5h is first warming up to after sealing, then It is warming up to 118 DEG C and at such a temperature stir process 90min, speed of agitator 100r/min.It is cooled to room temperature;Then it adds in poly- Ethylene oxide ethereal solution is first warming up to 70 DEG C and at such a temperature stir process 58min after sealing, then heat to 134 DEG C and Stir process 50min at this temperature then heats to 152 DEG C and stir process 45min, speed of agitator is at such a temperature 220r/min.Room temperature, filtering removal filtrate are down to, taking precipitate is washed with water, 100 DEG C of oven dryings;Mixture A is made.It will Mixture A calcines 5h at a temperature of 260 DEG C to obtain the final product.
Comparative example 1
In addition to hexamethylenetetramine is not contained, formula and preparation process are consistent with embodiment 5.
Comparative example 2
In addition to polyoxyethylene ether is not contained, formula and preparation process are consistent with embodiment 5.
Comparative example 3
It does not contain hexamethylenetetramine and outside polyoxyethylene ether, formula and preparation process is consistent with embodiment 5.
Comparative example 4
Each raw material is mixed, adds in other raw materials in embodiment, 100 DEG C of oven dryings;It is calcined at a temperature of 260 DEG C 5h to obtain the final product.Its raw material component is consistent with embodiment 5.
Comparative example 5
After each raw material is mixed, it is ultrasonically treated 30min, 100 DEG C of oven dryings;5h is calcined at a temperature of 260 DEG C to obtain the final product. Its raw material component is consistent with embodiment 5.
Embodiment 6
Adsorption test of the present invention to mercurous ions mimic water:5 kinds of inorganic agents prepared by above-described embodiment are selected by following Waste water treatment process, experimental result are included in table 1.And it is compared with the product of comparative example 1-5.
(1) the simulated wastewater 1000mL that the initial concentration containing mercury ion is 550mg/L is taken;
(2) pH value is adjusted in the range of 2.0~8.5;
(3) present invention is added in into simulated water sample, inorganic agent dosage is 1.0g/L water samples, at room temperature stirring and adsorbing 20min;
(4) the static concentration for taking supernatant aas determination mercury ion calculates adsorption capacity.
Table 1
Inorganic agent Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Adsorption capacity (mg/g) 371.6 382.5 433.9 452.1 475.5
Inorganic agent Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5
Adsorption capacity (mg/g) 125.8 110.1 45.2 68.8 87.1
As seen from Table 1, the present invention is 475.5mg/g to the maximum adsorption capacity of mercury ion.
Embodiment 7
Adsorption test of the present invention to the simulation water containing arsenic ion:5 kinds of inorganic agents prepared by above-described embodiment are selected by implementation The waste water treatment process of example 6, the initial concentration of arsenic ion is 350mg/L, and experimental result is included in table 2.
Table 2
Inorganic agent Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Adsorption capacity (mg/g) 228.6 237.2 308.1 315.7 325.1
Inorganic agent Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5
Adsorption capacity (mg/g) 70.6 118.4 55.8 81.5 92.5
As seen from Table 2, the present invention is 325.1mg/g to the maximum adsorption capacity of arsenic ion.
Embodiment 8
Adsorption test of the present invention to nickeliferous ions mimic water:5 kinds of inorganic agents prepared by above-described embodiment are selected by implementation The waste water treatment process of example 6, the initial concentration of nickel ion is 280mg/L, and experimental result is included in table 3.
Table 3
Inorganic agent Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
Adsorption capacity (mg/g) 195.7 211.7 241.6 255.2 261.2
Inorganic agent Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5
Adsorption capacity (mg/g) 108.4 92.5 33.7 78.5 92.5
As seen from Table 3, the maximum adsorption capacity of the invention to nickel ion is 261.2mg/g.
When the content of heavy metal ion is less than the adsorption capacity of inorganic agent in wastewater sample, adsorption rate is up to 100% A kind of material of good absorption heavy metal ion.
It is obvious to a person skilled in the art that the present invention is not limited to the details of above-mentioned exemplary embodiment, Er Qie In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power Profit requirement rather than above description limit, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should It considers the specification as a whole, the technical solutions in each embodiment can also be properly combined, forms those skilled in the art The other embodiment being appreciated that.

Claims (8)

1. a kind of inorganic agent of treated sewage, which is characterized in that include according to the raw material of parts by weight:18-26 parts of vermiculite, six first 11-19 parts of urotropine, 7-15 parts of polyoxyethylene ether, 4-8 parts of ethyl cellulose.
2. the inorganic agent of treated sewage according to claim 1, which is characterized in that include according to the raw material of parts by weight:Leech 20-24 parts of stone, 13-17 parts of hexamethylenetetramine, 9-13 parts of polyoxyethylene ether, 5-7 parts of ethyl cellulose.
3. the inorganic agent of treated sewage according to claim 1, which is characterized in that include according to the raw material of parts by weight:Leech 22 parts of stone, 15 parts of hexamethylenetetramine, 11 parts of polyoxyethylene ether, 6 parts of ethyl cellulose.
4. a kind of preparation method of the inorganic agent of treated sewage as described in any one of claims 1-3, which is characterized in that including with Lower step:
1)4-5 times of deionized water of hexamethylenetetramine and its quality is mixed, hexamethylenetetramine solution is made;By polyoxy second The ethyl alcohol of 6-7 times of alkene ether and its quality mixes, and polyoxyethylene ethereal solution is made;
2)By vermiculite, ethyl cellulose co-grinding, 150-200 mesh sieve is crossed, hexamethylenetetramine solution is then added in, after sealing 83-85 DEG C and at such a temperature stir process 1.4-1.5h are first warming up to, 116-120 DEG C is then heated to and stirs at such a temperature Processing 85-90min is mixed, is cooled to room temperature;Then polyoxyethylene ethereal solution is added in, 68-71 DEG C is first warming up to after sealing and at this At a temperature of stir process 55-60min, then heat to 133-135 DEG C and at such a temperature stir process 48-53min, Ran Housheng Temperature to 150-155 DEG C and at such a temperature stir process 40-45min, is down to room temperature, filtering removal filtrate, taking precipitate, washing It is dry;Mixture A is made;
3)Mixture A is calcined into 5h at a temperature of 260 DEG C to obtain the final product.
5. the preparation method of the inorganic agent of treated sewage according to claim 4, which is characterized in that washing, drying are to use Water washing, 100 DEG C of oven dryings.
6. the preparation method of the inorganic agent of treated sewage according to claim 4, which is characterized in that step 2)In, it adds in Speed of agitator after hexamethylenetetramine solution is 100r/min.
7. the preparation method of the inorganic agent of treated sewage according to claim 4, which is characterized in that step 2)In, it adds in Speed of agitator after polyoxyethylene ethereal solution is 220r/min.
8. application of the inorganic agent as described in any one of claims 1-3 in heavy metal-polluted water process.
CN201810010157.0A 2018-01-05 2018-01-05 A kind of inorganic agent of treated sewage and its preparation method and application Pending CN108176352A (en)

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CN104117342A (en) * 2014-06-26 2014-10-29 安徽普源分离机械制造有限公司 Bentonite modified by surface active agent and preparation method of bentonite
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CN101049942A (en) * 2007-03-30 2007-10-10 东华大学 Hydrosol of vermiculite, preparation method, and application
CN102728325A (en) * 2012-06-11 2012-10-17 西南科技大学 Preparation method of modified ethyl cellulose adsorption material
CN104117342A (en) * 2014-06-26 2014-10-29 安徽普源分离机械制造有限公司 Bentonite modified by surface active agent and preparation method of bentonite
CN106390936A (en) * 2016-12-07 2017-02-15 郑州源冉生物技术有限公司 Illite adsorbent as well as preparation method and application thereof

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Title
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