CN108031441A - There is the modified activated carbon absorbent of absorption property to the orthophosphates in water body - Google Patents

There is the modified activated carbon absorbent of absorption property to the orthophosphates in water body Download PDF

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CN108031441A
CN108031441A CN201711414289.1A CN201711414289A CN108031441A CN 108031441 A CN108031441 A CN 108031441A CN 201711414289 A CN201711414289 A CN 201711414289A CN 108031441 A CN108031441 A CN 108031441A
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mixed liquor
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不公告发明人
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Beijing Qingyuan Environmental Protection Technology Co Ltd
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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
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0222—Compounds of Mn, Re
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0233—Compounds of Cu, Ag, Au
    • B01J20/0237—Compounds of Cu
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0248—Compounds of B, Al, Ga, In, Tl
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0251—Compounds of Si, Ge, Sn, Pb
    • B01J20/0255—Compounds of Pb
    • 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
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • 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
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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 invention discloses the modified activated carbon absorbent to the orthophosphates in water body with absorption property.The mixed liquor through 3 bromine, 4 fluoronitrobenzene and the preparation of 5 chlorine, 2 fluorine pyridine is modified after activated carbon cleans is prepared into substance C；Substance C is through NbCl4、InCl3、Sr(NO3)2、Mn(NO3)2The mixed liquor of preparation is modified to be prepared into material D；The mixed liquor that material D is prepared through 3 bromine, 2 toluene fluoride, 1 bromine, 2 iodine tetrafluoroethane, 3 chlorothiophene, 2 carboxylate methyl ester, 2 hydroxyl, 3 pyrazine carboxylic acid methyl esters modified is prepared into material F；Material F is through PbCl2、CuCl2、Co(NO3)2With Mg (NO3)2The modified obtained material of the mixed liquor of preparation is the modified activated carbon absorbent for having absorption property to the orthophosphates in water body.

Description

There is the modified activated carbon absorbent of absorption property to the orthophosphates in water body
Technical field
The invention belongs to wastewater treating technology field, more particularly to a kind of orthophosphates in water body has absorption property Modified activated carbon absorbent.
Background technology
With China's sustained economic development, problem of environmental pollution is but gradually serious.Industrial production and daily life generate Substantial amounts of waste water, causes water pollution all the more serious, brings no small pressure to water environment, body eutrophication pollution becomes mesh One of preceding main water pollution.The nutriments such as N, P that body eutrophication discharges in living mainly due to human being's production Into slow flow water bodies such as lake, river mouth, river bends, utilized by microorganism panning, cause planktonic organism to accelerate breeding, make organic matter Speed of production is more than depletion rate, and water quality is destroyed, and causes the phenomenon of other biological death.At present for how to effectively control with it is pre- The eutrophic state of waterproof body, is a most important thing for administering water environment.Phosphorus is the main battalion for causing body eutrophication Material is supported, phytoplankton will be caused to increase substantially when phosphorus content is in more than 0.018mg/L in water.When the phosphorus content in water During less than 0.1mg/L, the biomass of phytoplankton and the content proportional of phosphorus.Phosphate is broadly divided into orthophosphates (H2PO4 -、HPO4 2-、PO4 3-), Quadrafos (P2O7 4-、P3O10 5-、P3O9 3-).Wherein, orthophosphates is extensive in the river of lake The form of appearance, generally to be regarded as the biologically effective state of most critical.
The principle of absorption method dephosphorization is that have using between phosphate radical and specific surface area larger material or porous molecular screen There are affinity physically or chemically and then the method for removing Phosphateadsorption, and after absorption, desorption can be carried out and returned Phosphor resource is received, while realizes the effect of pollution administration and resource reclaim.The advantage of absorption method be few occupied space, simple flow, Can repeatedly utilize, will not to produce secondary pollution, suitable application region wide, be to apply most phosphorus removing methods at present.But general absorption Agent is expensive, regeneration rate is not high.Therefore, it is that absorption is ground to seek a kind of adsorbent efficient, that adsorption capacity is big, regeneration rate is high Study carefully the emphasis in field.Also lack efficient dephosphorization adsorbent at present, particularly there is efficient absorption to the orthophosphates in water body The adsorbent of performance.
The content of the invention
The object of the present invention is to provide the modified activated carbon absorption that a kind of orthophosphates in water body has absorption property Agent, its preparation method comprise the following steps that：
(1) activated carbon that 58.8 gram particle footpaths are 2~4cm is added to the nitric acid that 250mL mass percent concentrations are 10% In solution, stirred 10 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain substance A 0, substance A 0 is through 500mL deionizations Placed 35 minutes in 105 DEG C of drying box after water washing, obtain substance A；
(2) the bromo- 4- fluoronitrobenzenes of 8.2 grams of 3- are added in 400mL absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor H1；
(3) substance A is added in mixed liquor H1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains substance B 1, and substance B 1 is placed 40 minutes in 80 DEG C of drying box, obtains substance B 2；
(4) the chloro- 2- fluorine pyridines of 4.4 grams of 5- are added in 400mL absolute ethyl alcohols, 3 points is stirred under the conditions of 1000r/min Clock, obtains mixed liquor H1；
(5) substance B 2 is added in mixed liquor H2, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains substance B 3, and substance B 3 is placed 40 minutes in 80 DEG C of drying box, obtains substance C；
(6) by 10.29 grams of NbCl4With 8.53 grams of InCl3It is added in 1200mL deionized waters, under the conditions of 1000r/min Stirring 3 minutes, is divided into 4 parts of equivalent, obtains mixed liquor J1, mixed liquor J2, mixed liquor J3, mixed liquor J4 after shaking up；
(7) Sr (NO by 140mL molar concentrations for 0.24mol/L3)2Solution and 60mL molar concentrations are 0.46mol/L's Mn(NO3)2Solution is added in mixed liquor J1, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K1；
(8) substance C is added in mixed liquor K1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains substance C 1, and substance C 1 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material C2；
(9) Sr (NO by 140mL molar concentrations for 0.34mol/L3)2Solution and 60mL molar concentrations are 0.51mol/L's Mn(NO3)2Solution is added in mixed liquor J2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K2；
(10) substance C 2 is added in mixed liquor K2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains substance C 3, and substance C 3 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material C4；
(11) Sr (NO by 140mL molar concentrations for 0.44mol/L3)2Solution and 60mL molar concentrations are 0.56mol/L Mn (NO3)2Solution is added in mixed liquor J3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K3；
(12) substance C 4 is added in mixed liquor K3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains substance C 5, and substance C 5 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material C6；
(13) Sr (NO by 140mL molar concentrations for 0.54mol/L3)2Solution and 60mL molar concentrations are 0.61mol/L Mn (NO3)2Solution is added in mixed liquor J4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K4；
(14) substance C 6 is added in mixed liquor K4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains substance C 7, and substance C 7 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material D；
(15) the bromo- 2- toluene fluorides of 5.9 grams of 3- are added in 300mL absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor L1；
(16) material D is added in mixed liquor L1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains material D1, and material D1 is placed 40 minutes in 80 DEG C of drying box, obtains material E；
(17) by 16.9 grams of 1- bromo-2-iodotetrafluoroethanes and 9.8 grams of 3- chlorothiophene -2- carboxylate methyl esters be added to 1500mL without In water-ethanol, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, Mixed liquor M3, mixed liquor M4, mixed liquor M5；
(18) 8.8 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M1, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N1；
(19) material E is added in mixed liquor N1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains material E1, and material E1 is placed 40 minutes in 80 DEG C of drying box, obtains material E2；
(20) 8.2 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M2, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N2；
(21) material E2 is added in mixed liquor N2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains material E3, and material E3 is placed 40 minutes in 80 DEG C of drying box, obtains material E4；
(22) 7.6 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M3, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N3；
(23) material E4 is added in mixed liquor N3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains material E5, and material E5 is placed 40 minutes in 80 DEG C of drying box, obtains material E6；
(24) 7.0 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M4, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N4；
(25) material E6 is added in mixed liquor N4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains material E7, and material E7 is placed 40 minutes in 80 DEG C of drying box, obtains material E8；
(26) 6.4 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M5, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N5；
(27) material E8 is added in mixed liquor N5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains material E9, and material E9 is placed 40 minutes in 80 DEG C of drying box, obtains material F；
(28) by 4.22 grams of PbCl2With 2.19 grams of CuCl2It is added in 300mL deionized waters, under the conditions of 1000r/min Stirring 3 minutes, is divided into 2 parts of equivalent, obtains mixed liquor O after shaking up；
(29) Co (NO by 100mL molar concentrations for 0.65mol/L3)2Solution and 100mL molar concentrations are 0.42mol/L Mg (NO3)2Solution is added in mixed liquor O, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor P；
(30) material F is added in mixed liquor P, is shaken 45 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains material F1, and material F1 is placed 120 minutes in 80 DEG C of drying box, and obtained material is to the orthophosphoric acid in water body Salt has the modified activated carbon absorbent of absorption property.
The invention has the advantages that the modified activated carbon that the obtained orthophosphates in water body has absorption property is inhaled Attached dose has the characteristics that high to phosphorus adsorption efficiency, adsorption capacity is big, can be with regeneration.
Embodiment
The present invention provides a kind of orthophosphates in water body have absorption property modified activated carbon absorbent, below Illustrate to apply process in fact by an example.
Embodiment 1.
(1) activated carbon that 58.8 gram particle footpaths are 2~4cm is added to the nitric acid that 250mL mass percent concentrations are 10% In solution, stirred 10 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain substance A 0, substance A 0 is through 500mL deionizations Placed 35 minutes in 105 DEG C of drying box after water washing, obtain substance A；
(2) the bromo- 4- fluoronitrobenzenes of 8.2 grams of 3- are added in 400mL absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor H1；
(3) substance A is added in mixed liquor H1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains substance B 1, and substance B 1 is placed 40 minutes in 80 DEG C of drying box, obtains substance B 2；
(4) the chloro- 2- fluorine pyridines of 4.4 grams of 5- are added in 400mL absolute ethyl alcohols, 3 points is stirred under the conditions of 1000r/min Clock, obtains mixed liquor H1；
(5) substance B 2 is added in mixed liquor H2, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains substance B 3, and substance B 3 is placed 40 minutes in 80 DEG C of drying box, obtains substance C；
(6) by 10.29 grams of NbCl4With 8.53 grams of InCl3It is added in 1200mL deionized waters, under the conditions of 1000r/min Stirring 3 minutes, is divided into 4 parts of equivalent, obtains mixed liquor J1, mixed liquor J2, mixed liquor J3, mixed liquor J4 after shaking up；
(7) Sr (NO by 140mL molar concentrations for 0.24mol/L3)2Solution and 60mL molar concentrations are 0.46mol/L's Mn(NO3)2Solution is added in mixed liquor J1, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K1；
(8) substance C is added in mixed liquor K1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains substance C 1, and substance C 1 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material C2；
(9) Sr (NO by 140mL molar concentrations for 0.34mol/L3)2Solution and 60mL molar concentrations are 0.51mol/L's Mn(NO3)2Solution is added in mixed liquor J2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K2；
(10) substance C 2 is added in mixed liquor K2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains substance C 3, and substance C 3 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material C4；
(11) Sr (NO by 140mL molar concentrations for 0.44mol/L3)2Solution and 60mL molar concentrations are 0.56mol/L Mn (NO3)2Solution is added in mixed liquor J3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K3；
(12) substance C 4 is added in mixed liquor K3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains substance C 5, and substance C 5 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material C6；
(13) Sr (NO by 140mL molar concentrations for 0.54mol/L3)2Solution and 60mL molar concentrations are 0.61mol/L Mn (NO3)2Solution is added in mixed liquor J4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K4；
(14) substance C 6 is added in mixed liquor K4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains substance C 7, and substance C 7 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material D；
(15) the bromo- 2- toluene fluorides of 5.9 grams of 3- are added in 300mL absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min Minute, obtain mixed liquor L1；
(16) material D is added in mixed liquor L1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains material D1, and material D1 is placed 40 minutes in 80 DEG C of drying box, obtains material E；
(17) by 16.9 grams of 1- bromo-2-iodotetrafluoroethanes and 9.8 grams of 3- chlorothiophene -2- carboxylate methyl esters be added to 1500mL without In water-ethanol, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, Mixed liquor M3, mixed liquor M4, mixed liquor M5；
(18) 8.8 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M1, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N1；
(19) material E is added in mixed liquor N1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains material E1, and material E1 is placed 40 minutes in 80 DEG C of drying box, obtains material E2；
(20) 8.2 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M2, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N2；
(21) material E2 is added in mixed liquor N2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains material E3, and material E3 is placed 40 minutes in 80 DEG C of drying box, obtains material E4；
(22) 7.6 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M3, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N3；
(23) material E4 is added in mixed liquor N3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains material E5, and material E5 is placed 40 minutes in 80 DEG C of drying box, obtains material E6；
(24) 7.0 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M4, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N4；
(25) material E6 is added in mixed liquor N4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains material E7, and material E7 is placed 40 minutes in 80 DEG C of drying box, obtains material E8；
(26) 6.4 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M5, are stirred under the conditions of 1000r/min Mix 3 minutes, obtain mixed liquor N5；
(27) material E8 is added in mixed liquor N5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C Liquid obtains material E9, and material E9 is placed 40 minutes in 80 DEG C of drying box, obtains material F；
(28) by 4.22 grams of PbCl2With 2.19 grams of CuCl2It is added in 300mL deionized waters, under the conditions of 1000r/min Stirring 3 minutes, is divided into 2 parts of equivalent, obtains mixed liquor O after shaking up；
(29) Co (NO by 100mL molar concentrations for 0.65mol/L3)2Solution and 100mL molar concentrations are 0.42mol/L Mg (NO3)2Solution is added in mixed liquor O, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor P；
(30) material F is added in mixed liquor P, is shaken 45 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Body obtains material F1, and material F1 is placed 120 minutes in 80 DEG C of drying box, and obtained material is to the orthophosphoric acid in water body Salt has the modified activated carbon absorbent of absorption property.
Here is with the obtained modified activated carbon to the orthophosphates in water body with absorption property of the method for the present invention Adsorbent has carried out the polluted-water containing orthophosphates adsorption Removal, further illustrates the present invention.
Modified activated carbon absorbent made from the method for the present invention adsorbs the polluted-water containing phosphorus, as a result table It is bright：When phosphorus initial concentration is 7.3mg/L, into 1000mL phosphorus polluted-waters, addition 2.5g is used changes made from the method for the present invention Property acticarbon after, adsorption time be 6 minutes, the phosphorus concentration after processing in water body is reduced to 0.01mg/L, by static state inhale The Freundlich Isothermal Models of attached experiment understand modified activated carbon absorbent made from the method for the present invention align it is phosphatic most Big adsorbance is 56.8mg/g.

Claims (1)

1. a kind of orthophosphates in water body has the modified activated carbon absorbent of absorption property, it is characterised in that preparing should Activated carbon adsorption agent method comprises the following steps that：
(1) activated carbon that 58.8 gram particle footpaths are 2~4cm is added to the salpeter solution that 250mL mass percent concentrations are 10% In, stirred 10 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain substance A 0, substance A 0 is washed through 500mL deionizations Placed 35 minutes in 105 DEG C of drying box after washing, obtain substance A；
(2) the bromo- 4- fluoronitrobenzenes of 8.2 grams of 3- are added in 400mL absolute ethyl alcohols, 3 points is stirred under the conditions of 1000r/min Clock, obtains mixed liquor H1；
(3) substance A is added in mixed liquor H1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain To substance B 1, substance B 1 is placed 40 minutes in 80 DEG C of drying box, obtains substance B 2；
(4) the chloro- 2- fluorine pyridines of 4.4 grams of 5- are added in 400mL absolute ethyl alcohols, are stirred 3 minutes under the conditions of 1000r/min, Obtain mixed liquor H1；
(5) substance B 2 is added in mixed liquor H2, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain To substance B 3, substance B 3 is placed 40 minutes in 80 DEG C of drying box, obtains substance C；
(6) by 10.29 grams of NbCl4With 8.53 grams of InCl3It is added in 1200mL deionized waters, is stirred under the conditions of 1000r/min 3 minutes, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor J1, mixed liquor J2, mixed liquor J3, mixed liquor J4；
(7) Sr (NO by 140mL molar concentrations for 0.24mol/L3)2Solution and the Mn that 60mL molar concentrations are 0.46mol/L (NO3)2Solution is added in mixed liquor J1, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K1；
(8) substance C is added in mixed liquor K1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain To substance C 1, substance C 1 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains substance C 2；
(9) Sr (NO by 140mL molar concentrations for 0.34mol/L3)2Solution and the Mn that 60mL molar concentrations are 0.51mol/L (NO3)2Solution is added in mixed liquor J2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K2；
(10) substance C 2 is added in mixed liquor K2, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Substance C 3 is obtained, substance C 3 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains substance C 4；
(11) Sr (NO by 140mL molar concentrations for 0.44mol/L3)2Solution and the Mn that 60mL molar concentrations are 0.56mol/L (NO3)2Solution is added in mixed liquor J3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K3；
(12) substance C 4 is added in mixed liquor K3, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Substance C 5 is obtained, substance C 5 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains substance C 6；
(13) Sr (NO by 140mL molar concentrations for 0.54mol/L3)2Solution and the Mn that 60mL molar concentrations are 0.61mol/L (NO3)2Solution is added in mixed liquor J4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor K4；
(14) substance C 6 is added in mixed liquor K4, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Substance C 7 is obtained, substance C 7 is placed 40 minutes after the washing of 300mL deionized waters in 80 DEG C of drying box, obtains material D；
(15) the bromo- 2- toluene fluorides of 5.9 grams of 3- are added in 300mL absolute ethyl alcohols, are stirred 3 minutes under the conditions of 1000r/min, Obtain mixed liquor L1；
(16) material D is added in mixed liquor L1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain To material D1, material D1 is placed 40 minutes in 80 DEG C of drying box, obtains material E；
(17) 16.9 grams of 1- bromo-2-iodotetrafluoroethanes and 9.8 grams of 3- chlorothiophene -2- carboxylate methyl esters are added to the anhydrous second of 1500mL In alcohol, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixing Liquid M3, mixed liquor M4, mixed liquor M5；
(18) 8.8 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M1,3 points is stirred under the conditions of 1000r/min Clock, obtains mixed liquor N1；
(19) material E is added in mixed liquor N1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain To material E1, material E1 is placed 40 minutes in 80 DEG C of drying box, obtains material E2；
(20) 8.2 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M2,3 points is stirred under the conditions of 1000r/min Clock, obtains mixed liquor N2；
(21) material E2 is added in mixed liquor N2, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Material E3 is obtained, material E3 is placed 40 minutes in 80 DEG C of drying box, obtains material E4；
(22) 7.6 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M3,3 points is stirred under the conditions of 1000r/min Clock, obtains mixed liquor N3；
(23) material E4 is added in mixed liquor N3, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Material E5 is obtained, material E5 is placed 40 minutes in 80 DEG C of drying box, obtains material E6；
(24) 7.0 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M4,3 points is stirred under the conditions of 1000r/min Clock, obtains mixed liquor N4；
(25) material E6 is added in mixed liquor N4, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Material E7 is obtained, material E7 is placed 40 minutes in 80 DEG C of drying box, obtains material E8；
(26) 6.4 grams of 2- hydroxyl -3- pyrazine carboxylic acid methyl esters are added in mixed liquor M5,3 points is stirred under the conditions of 1000r/min Clock, obtains mixed liquor N5；
(27) material E8 is added in mixed liquor N5, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid Material E9 is obtained, material E9 is placed 40 minutes in 80 DEG C of drying box, obtains material F；
(28) by 4.22 grams of PbCl2With 2.19 grams of CuCl2It is added in 300mL deionized waters, 3 is stirred under the conditions of 1000r/min Minute, 2 parts of equivalent is divided into after shaking up, obtains mixed liquor O；
(29) Co (NO by 100mL molar concentrations for 0.65mol/L3)2Solution and the Mg that 100mL molar concentrations are 0.42mol/L (NO3)2Solution is added in mixed liquor O, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor P；
(30) material F is added in mixed liquor P, is shaken 45 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain Placed 120 minutes in 80 DEG C of drying box to material F1, material F1, obtained material is to have to the orthophosphates in water body There is the modified activated carbon absorbent of absorption property.
CN201711414289.1A 2017-12-25 2017-12-25 There is the modified activated carbon absorbent of absorption property to the orthophosphates in water body Withdrawn CN108031441A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102614854A (en) * 2012-03-31 2012-08-01 复旦大学 Method for preparaing dephosphorized and ferrum-carried activated carbon adsorbent
CN105251445A (en) * 2015-11-04 2016-01-20 中国科学院化学研究所 Porous carbon adsorbent as well as preparation method and application thereof
CN106140087A (en) * 2016-07-22 2016-11-23 四川大学 A kind of sludge activity carbon adsorbent for sewage dephosphorization and preparation method thereof
CN106365268A (en) * 2016-11-21 2017-02-01 北京益清源环保科技有限公司 Modified active carbon particle electrode having function of removing phenol through electro-catalysis and manufacturing method
CN106582534A (en) * 2017-01-07 2017-04-26 北京源清益壤环保科技有限公司 Modified active carbon adsorbent for removing nickel from polluted water and preparation method for modified active carbon adsorbent
CN106975460A (en) * 2017-05-11 2017-07-25 北京益净环保设备科技有限公司 Modified corn core adsorbent for Adsorption kanamycins

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102614854A (en) * 2012-03-31 2012-08-01 复旦大学 Method for preparaing dephosphorized and ferrum-carried activated carbon adsorbent
CN105251445A (en) * 2015-11-04 2016-01-20 中国科学院化学研究所 Porous carbon adsorbent as well as preparation method and application thereof
CN106140087A (en) * 2016-07-22 2016-11-23 四川大学 A kind of sludge activity carbon adsorbent for sewage dephosphorization and preparation method thereof
CN106365268A (en) * 2016-11-21 2017-02-01 北京益清源环保科技有限公司 Modified active carbon particle electrode having function of removing phenol through electro-catalysis and manufacturing method
CN106582534A (en) * 2017-01-07 2017-04-26 北京源清益壤环保科技有限公司 Modified active carbon adsorbent for removing nickel from polluted water and preparation method for modified active carbon adsorbent
CN106975460A (en) * 2017-05-11 2017-07-25 北京益净环保设备科技有限公司 Modified corn core adsorbent for Adsorption kanamycins

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
ZHENGFANG WANG ET AL: "Influence of moderate pre-oxidation treatment on the physical, chemical and phosphate adsorption properties of iron-containing activated carbon", 《JOURNAL OF ENVIRONMENTAL SCIENCES》 *

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