CN108126656A - For the modified activated carbon absorbent of benzene in Adsorption wastewater from chemical industry - Google Patents
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- CN108126656A CN108126656A CN201711414319.9A CN201711414319A CN108126656A CN 108126656 A CN108126656 A CN 108126656A CN 201711414319 A CN201711414319 A CN 201711414319A CN 108126656 A CN108126656 A CN 108126656A
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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
- B01J20/20—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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
- C02F2101/322—Volatile compounds, e.g. benzene
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Abstract
The invention discloses a kind of modified activated carbon absorbents for benzene in Adsorption wastewater from chemical industry.Through 2 cyanobenzothiophenes, 3 methyl, 5 phenyl pyridazine, 2 chlorine, 5 nitropyridine, 3 methyl tetrahydrochysene phthalate anhydrides, 2 methyl, 3 nitrophenyl-acetic acid, 6 bromine, 4 hydroxyl, 3 nitroquinoline, N cinnamyl piperazines, 3 after activated carbon cleaning, 4,6 tribromo pyridazines, 2 pyridinemethanols, 2, mixed liquor prepared by 4 difluoro pyridines, 4 chlorine, 3 pyridazinone, 2,5 dichloropyrazines, dibenzyl phosphite, bromomethyl cyclopropane and 2 bromine, 6 fluoronitrobenzene is modified to be prepared into substance E；Substance E is through Cu (NO3)2、Ce(NO3)3、MnCl2And ZnCl2The substance of the modified preparation of mixed liquor of preparation is for the modified activated carbon absorbent of benzene in Adsorption wastewater from chemical industry.
Description
Technical field
The invention belongs to organic chemical waste water processing technology fields difficult to degrade, more particularly to a kind of to be used for Adsorption chemical industry
The modified activated carbon absorbent of benzene in waste water.
Background technology
Absorption is a kind of surface of solids phenomenon, while is also a kind of transport phenomenon, it is to belong to a spontaneous thermodynamics
Process.Waste water adsorption treatment method is using certain or several pollutants in porous solid adsorbent absorption waste water, is made wherein
One or more components pass through adsorbent material molecular attraction or chemical bond force under the action of accumulation or it is condensing in adsorbent
In duct or surface and the method for reaching separation.The reaction of adsorbate and adsorbent is very fast, it does not need to add again any
Drug, it is easy to operate, while widely used adsorbent all has higher adsorption capacity and bigger specific surface at present
Product, the advantages such as so as to promote the pollutant in absorption method removal waste water efficient and adaptable.Adsorbent also has in itself
The characteristics of secondary pollution will not bring new chemical substance will not be generated, it typically takes place in the surface of adsorbent.Therefore it inhales
Attached method because having the characteristics that easy to operate, flexibility is high, operating cost is low, insensitive and environmental-friendly to toxic pollutant,
It is widely used in organic chemical waste water process field.
Up to the present, various types of adsorbents be found and gradually be introduced in processing wastewater application in.In quilt
It was found that adsorbent in for being broadly divided into three categories in wastewater treatment：One kind is such as zeolite, viscous for inorganic material class adsorbent
The materials such as soil, silica；It is another kind of for the adsorbent based on carbons, such as activated carbon, graphite, carbon molecular sieve etc.；Third
Class is organic polymer species adsorbent.A kind of new adsorbent is researched and developed in field of waste water treatment have become current hot spot and ask
Topic.Also lack the sorbing material for the organic industrial sewage processing containing benzene at present.
Invention content
The object of the present invention is to provide a kind of modified activated carbon absorbent for benzene in Adsorption wastewater from chemical industry, systems
Preparation Method is as follows：
(1) 88 grams of active carbon particles that grain size is 2~4cm are put into 400mL acetone solns and impregnated 20 minutes, crossed and filter out
Liquid is gone to obtain substance A 0, substance A 0 is put into 400mL absolute ethyl alcohols and is impregnated 20 minutes, liquid is filtered to remove and obtains substance
A1, substance A 1 obtain substance A 2 after 300mL originally water washing, and substance A 2 is dry at 105 DEG C after the washing of 300mL deionized waters
It is placed 60 minutes in dry case, obtains substance A；
(2) 3.8 grams of 2- cyanobenzothiophenes and 6.9 grams of 3- methyl -5- phenyl pyridazines are added to 1200mL absolute ethyl alcohols
In, it is stirred 5 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor
M3, mixed liquor M4；
(3) 7.6 grams of 2- chloro-5-nitropyridines are added in 800mL isopropanols, 5 points is stirred under the conditions of 1000r/min
Then clock adds in 8mL concentrated nitric acids, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed liquor
N4；
(4) mixed liquor N1 and 15.8 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M1, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O1；
(5) substance A is added in mixed liquor O1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 1, and substance B 1 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 2；
(6) mixed liquor N2 and 15.1 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M2, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O2；
(7) substance B 2 is added in mixed liquor O2, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 3, and substance B 3 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 4；
(8) mixed liquor N3 and 14.4 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M3, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O3；
(9) substance B 4 is added in mixed liquor O3, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 5, and substance B 5 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 6；
(10) mixed liquor N4 and 13.7 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M4, in 1000r/
It is stirred 3 minutes under the conditions of min, obtains mixed liquor O4；
(11) substance B 6 is added in mixed liquor O4, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance B 7, and substance B 7 in 85 DEG C of drying box is placed 110 minutes, obtains substance C；
(12) 4.8 grams of 2- methyl-3-nitrophenylacetic acids and the bromo- 4- hydroxyls -3- nitroquinolines of 6.4 grams of 6- are added to
In 300mL absolute ethyl alcohols, stirred 5 minutes under the conditions of 1000r/min, obtain mixed liquor P1；
(13) substance C is added in mixed liquor P1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 in 85 DEG C of drying box is placed 110 minutes, obtains substance C 2；
(14) by 7.9 grams of N- cinnamyl piperazines and 11.2 gram 3,4,6- tribromo pyridazines are added in 300mL absolute ethyl alcohols,
It is stirred 5 minutes under the conditions of 1000r/min, obtains mixed liquor P2；
(15) substance C 2 is added in mixed liquor P2, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance C 3, and substance C 3 in 85 DEG C of drying box is placed 110 minutes, obtains substance C 4；
(16) 4.8 grams of 2- pyridinemethanols and 6.3 grams of 2,4- difluoro pyridines are added in 300mL absolute ethyl alcohols,
It is stirred 5 minutes under the conditions of 1000r/min, obtains mixed liquor P3；
(17) substance C 4 is added in mixed liquor P3, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance C 5, and substance C 5 in 85 DEG C of drying box is placed 110 minutes, obtains substance D；
(18) the chloro- 3- pyridazinones of 11.7 grams of 4- and 14.5 grams of 2,5- dichloropyrazines are added in 1500mL absolute ethyl alcohols,
Stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor Q1, mixed liquor Q2, mixed liquor Q3,
Mixed liquor Q4, mixed liquor Q5；
(19) 8.2 grams of dibenzyl phosphites and 9.9 grams of bromomethyl cyclopropanes are added in 750mL n-butanols,
It is stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor R1, mixed liquor R2, mixed liquor R3, mix
Close liquid R4, mixed liquor R5；
(20) mixed liquor R1 and the bromo- 6- fluoronitrobenzenes of 3.9 grams of 2- are added in mixed liquor Q1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S1；
(21) substance D is added in mixed liquor S1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance D1, and substance D1 in 85 DEG C of drying box is placed 110 minutes, obtains substance D2；
(22) mixed liquor R2 and the bromo- 6- fluoronitrobenzenes of 4.4 grams of 2- are added in mixed liquor Q2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S2；
(23) substance D2 is added in mixed liquor S2, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance D3, and substance D3 in 85 DEG C of drying box is placed 110 minutes, obtains substance D4；
(24) mixed liquor R3 and the bromo- 6- fluoronitrobenzenes of 4.9 grams of 2- are added in mixed liquor Q3, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S3；
(25) substance D4 is added in mixed liquor S3, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance D5, and substance D5 in 85 DEG C of drying box is placed 110 minutes, obtains substance D6；
(26) mixed liquor R4 and the bromo- 6- fluoronitrobenzenes of 5.4 grams of 2- are added in mixed liquor Q4, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S4；
(27) substance D6 is added in mixed liquor S4, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance D7, and substance D7 in 85 DEG C of drying box is placed 110 minutes, obtains substance D8；
(28) mixed liquor R5 and the bromo- 6- fluoronitrobenzenes of 5.9 grams of 2- are added in mixed liquor Q5, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S5；
(29) substance D8 is added in mixed liquor S5, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance D9, and substance D9 in 85 DEG C of drying box is placed 110 minutes, obtains substance E；
(30) by 14.9 grams of Cu (NO3)2With 4.8 grams of Ce (NO3)3It is added in 1200mL deionized waters, in 1000r/min
Under the conditions of stir 10 minutes, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor T1, mixed liquor T2, mixed liquor T3, mixed liquor T4；
(31) by 4.2 grams of MnCl2With 5.8 grams of ZnCl2It is added in mixed liquor T1,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U1；
(32) substance E is added in mixed liquor U1, is shaken 15 minutes in the shaking table for being 45 DEG C in temperature, be filtered to remove liquid
Body obtains substance E1, and substance E1 in 85 DEG C of drying box is placed 110 minutes, obtains substance E2；
(33) by 4.7 grams of MnCl2With 5.3 grams of ZnCl2It is added in mixed liquor T2,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U2；
(34) substance E2 is added in mixed liquor U2, shakes 15 minutes, be filtered to remove in the shaking table for being 45 DEG C in temperature
Liquid obtains substance E3, and substance E3 in 85 DEG C of drying box is placed 110 minutes, obtains substance E4；
(35) by 5.2 grams of MnCl2With 4.8 grams of ZnCl2It is added in mixed liquor T3,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U3；
(36) substance E4 is added in mixed liquor U3, shakes 15 minutes, be filtered to remove in the shaking table for being 45 DEG C in temperature
Liquid obtains substance E5, and substance E5 in 85 DEG C of drying box is placed 110 minutes, obtains substance E6；
(37) by 5.7 grams of MnCl2With 4.3 grams of ZnCl2It is added in mixed liquor T4,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U4；
(38) substance E6 is added in mixed liquor U4, shakes 15 minutes, be filtered to remove in the shaking table for being 45 DEG C in temperature
Liquid obtains substance E7, and substance E7 in 85 DEG C of drying box is placed 110 minutes, obtains substance E8；
(39) by 6.2 grams of MnCl2With 3.8 grams of ZnCl2It is added in mixed liquor T5,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U5；
(40) substance E8 is added in mixed liquor U5, shakes 15 minutes, be filtered to remove in the shaking table for being 45 DEG C in temperature
Liquid obtains substance E9, and substance E9 is placed 110 minutes in 85 DEG C of drying box, and obtained substance is for Adsorption
The modified activated carbon absorbent of benzene in wastewater from chemical industry.
The invention has the advantages that the modified activated carbon absorbent tool obtained for benzene in Adsorption wastewater from chemical industry
There is the features such as big, removal efficiency is high to benzene adsorption capacity.
Specific embodiment
The present invention provides a kind of modified activated carbon absorbent for benzene in Adsorption wastewater from chemical industry, below by one
Example illustrates to apply process in fact.
Embodiment 1.
(1) 88 grams of active carbon particles that grain size is 2~4cm are put into 400mL acetone solns and impregnated 20 minutes, crossed and filter out
Liquid is gone to obtain substance A 0, substance A 0 is put into 400mL absolute ethyl alcohols and is impregnated 20 minutes, liquid is filtered to remove and obtains substance
A1, substance A 1 obtain substance A 2 after 300mL originally water washing, and substance A 2 is dry at 105 DEG C after the washing of 300mL deionized waters
It is placed 60 minutes in dry case, obtains substance A；
(2) 3.8 grams of 2- cyanobenzothiophenes and 6.9 grams of 3- methyl -5- phenyl pyridazines are added to 1200mL absolute ethyl alcohols
In, it is stirred 5 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor
M3, mixed liquor M4；
(3) 7.6 grams of 2- chloro-5-nitropyridines are added in 800mL isopropanols, 5 points is stirred under the conditions of 1000r/min
Then clock adds in 8mL concentrated nitric acids, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed liquor
N4；
(4) mixed liquor N1 and 15.8 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M1, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O1；
(5) substance A is added in mixed liquor O1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 1, and substance B 1 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 2；
(6) mixed liquor N2 and 15.1 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M2, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O2；
(7) substance B 2 is added in mixed liquor O2, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 3, and substance B 3 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 4；
(8) mixed liquor N3 and 14.4 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M3, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O3；
(9) substance B 4 is added in mixed liquor O3, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance B 5, and substance B 5 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 6；
(10) mixed liquor N4 and 13.7 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M4, in 1000r/
It is stirred 3 minutes under the conditions of min, obtains mixed liquor O4；
(11) substance B 6 is added in mixed liquor O4, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance B 7, and substance B 7 in 85 DEG C of drying box is placed 110 minutes, obtains substance C；
(12) 4.8 grams of 2- methyl-3-nitrophenylacetic acids and the bromo- 4- hydroxyls -3- nitroquinolines of 6.4 grams of 6- are added to
In 300mL absolute ethyl alcohols, stirred 5 minutes under the conditions of 1000r/min, obtain mixed liquor P1；
(13) substance C is added in mixed liquor P1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 in 85 DEG C of drying box is placed 110 minutes, obtains substance C 2；
(14) by 7.9 grams of N- cinnamyl piperazines and 11.2 gram 3,4,6- tribromo pyridazines are added in 300mL absolute ethyl alcohols,
It is stirred 5 minutes under the conditions of 1000r/min, obtains mixed liquor P2；
(15) substance C 2 is added in mixed liquor P2, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance C 3, and substance C 3 in 85 DEG C of drying box is placed 110 minutes, obtains substance C 4；
(16) 4.8 grams of 2- pyridinemethanols and 6.3 grams of 2,4- difluoro pyridines are added in 300mL absolute ethyl alcohols,
It is stirred 5 minutes under the conditions of 1000r/min, obtains mixed liquor P3；
(17) substance C 4 is added in mixed liquor P3, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance C 5, and substance C 5 in 85 DEG C of drying box is placed 110 minutes, obtains substance D；
(18) the chloro- 3- pyridazinones of 11.7 grams of 4- and 14.5 grams of 2,5- dichloropyrazines are added in 1500mL absolute ethyl alcohols,
Stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor Q1, mixed liquor Q2, mixed liquor Q3,
Mixed liquor Q4, mixed liquor Q5；
(19) 8.2 grams of dibenzyl phosphites and 9.9 grams of bromomethyl cyclopropanes are added in 750mL n-butanols,
It is stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor R1, mixed liquor R2, mixed liquor R3, mix
Close liquid R4, mixed liquor R5；
(20) mixed liquor R1 and the bromo- 6- fluoronitrobenzenes of 3.9 grams of 2- are added in mixed liquor Q1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S1；
(21) substance D is added in mixed liquor S1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Body obtains substance D1, and substance D1 in 85 DEG C of drying box is placed 110 minutes, obtains substance D2；
(22) mixed liquor R2 and the bromo- 6- fluoronitrobenzenes of 4.4 grams of 2- are added in mixed liquor Q2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S2；
(23) substance D2 is added in mixed liquor S2, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance D3, and substance D3 in 85 DEG C of drying box is placed 110 minutes, obtains substance D4；
(24) mixed liquor R3 and the bromo- 6- fluoronitrobenzenes of 4.9 grams of 2- are added in mixed liquor Q3, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S3；
(25) substance D4 is added in mixed liquor S3, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance D5, and substance D5 in 85 DEG C of drying box is placed 110 minutes, obtains substance D6；
(26) mixed liquor R4 and the bromo- 6- fluoronitrobenzenes of 5.4 grams of 2- are added in mixed liquor Q4, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S4；
(27) substance D6 is added in mixed liquor S4, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance D7, and substance D7 in 85 DEG C of drying box is placed 110 minutes, obtains substance D8；
(28) mixed liquor R5 and the bromo- 6- fluoronitrobenzenes of 5.9 grams of 2- are added in mixed liquor Q5, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor S5；
(29) substance D8 is added in mixed liquor S5, shakes 15 minutes, be filtered to remove in the shaking table for being 35 DEG C in temperature
Liquid obtains substance D9, and substance D9 in 85 DEG C of drying box is placed 110 minutes, obtains substance E；
(30) by 14.9 grams of Cu (NO3)2With 4.8 grams of Ce (NO3)3It is added in 1200mL deionized waters, in 1000r/min
Under the conditions of stir 10 minutes, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor T1, mixed liquor T2, mixed liquor T3, mixed liquor T4；
(31) by 4.2 grams of MnCl2With 5.8 grams of ZnCl2It is added in mixed liquor T1,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U1；
(32) substance E is added in mixed liquor U1, is shaken 15 minutes in the shaking table for being 45 DEG C in temperature, be filtered to remove liquid
Body obtains substance E1, and substance E1 in 85 DEG C of drying box is placed 110 minutes, obtains substance E2；
(33) by 4.7 grams of MnCl2With 5.3 grams of ZnCl2It is added in mixed liquor T2,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U2；
(34) substance E2 is added in mixed liquor U2, shakes 15 minutes, be filtered to remove in the shaking table for being 45 DEG C in temperature
Liquid obtains substance E3, and substance E3 in 85 DEG C of drying box is placed 110 minutes, obtains substance E4；
(35) by 5.2 grams of MnCl2With 4.8 grams of ZnCl2It is added in mixed liquor T3,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U3；
(36) substance E4 is added in mixed liquor U3, shakes 15 minutes, be filtered to remove in the shaking table for being 45 DEG C in temperature
Liquid obtains substance E5, and substance E5 in 85 DEG C of drying box is placed 110 minutes, obtains substance E6；
(37) by 5.7 grams of MnCl2With 4.3 grams of ZnCl2It is added in mixed liquor T4,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U4；
(38) substance E6 is added in mixed liquor U4, shakes 15 minutes, be filtered to remove in the shaking table for being 45 DEG C in temperature
Liquid obtains substance E7, and substance E7 in 85 DEG C of drying box is placed 110 minutes, obtains substance E8；
(39) by 6.2 grams of MnCl2With 3.8 grams of ZnCl2It is added in mixed liquor T5,10 points is stirred under the conditions of 1000r/min
Clock obtains mixed liquor U5；
(40) substance E8 is added in mixed liquor U5, shakes 15 minutes, be filtered to remove in the shaking table for being 45 DEG C in temperature
Liquid obtains substance E9, and substance E9 is placed 110 minutes in 85 DEG C of drying box, and obtained substance is for Adsorption
The modified activated carbon absorbent of benzene in wastewater from chemical industry.
Here is with the method for the present invention modified activated carbon absorbent obtained for benzene in Adsorption wastewater from chemical industry
Adsorption test has been carried out to the waste water containing benzene, has been further illustrated the present invention.
Modified activated carbon absorbent made from the method for the present invention the organic chemical waste water containing benzene has been carried out to absorption examination
It tests, the results showed that when benzene initial concentration is 33.4mg/L, into 1000mL waste water, addition 12.0g is made with the method for the present invention
Modified activated carbon absorbent after, adsorption time be 5 minutes, the benzene concentration in processed waste water is reduced to 0.1mg/L, by static state
The Freundlich Isothermal Models of adsorption experiment understand that modified activated carbon absorbent made from the method for the present invention inhales the maximum of benzene
Attached amount is 242.6mg/g.
Claims (1)
1. a kind of modified activated carbon absorbent for benzene in Adsorption wastewater from chemical industry, which is characterized in that prepare the activated carbon
Adsorbent method is as follows：
(1) 88 grams of active carbon particles that grain size is 2~4cm are put into 400mL acetone solns and impregnated 20 minutes, be filtered to remove liquid
Body obtains substance A 0, and substance A 0 is put into 400mL absolute ethyl alcohols and is impregnated 20 minutes, liquid is filtered to remove and obtains substance A 1, object
Matter A1 obtains substance A 2 after 300mL originally water washing, and substance A 2 is after the washing of 300mL deionized waters in 105 DEG C of drying box
It is middle to place 60 minutes, obtain substance A；
(2) 3.8 grams of 2- cyanobenzothiophenes and 6.9 grams of 3- methyl -5- phenyl pyridazines are added in 1200mL absolute ethyl alcohols,
It is stirred 5 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtained mixed liquor M1, mixed liquor M2, mixed liquor M3, mix
Close liquid M4；
(3) 7.6 grams of 2- chloro-5-nitropyridines are added in 800mL isopropanols, are stirred 5 minutes under the conditions of 1000r/min,
Then 8mL concentrated nitric acids are added in, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed liquor N4；
(4) mixed liquor N1 and 15.8 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor O1；
(5) substance A is added in mixed liquor O1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid and obtain
To substance B 1, substance B 1 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 2；
(6) mixed liquor N2 and 15.1 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor O2；
(7) substance B 2 is added in mixed liquor O2, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid and obtain
To substance B 3, substance B 3 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 4；
(8) mixed liquor N3 and 14.4 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M3, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor O3；
(9) substance B 4 is added in mixed liquor O3, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid and obtain
To substance B 5, substance B 5 in 85 DEG C of drying box is placed 110 minutes, obtains substance B 6；
(10) mixed liquor N4 and 13.7 grams of 3- methyl tetrahydrochysene phthalate anhydrides are added in mixed liquor M4, in 1000r/min items
It is stirred 3 minutes under part, obtains mixed liquor O4；
(11) substance B 6 is added in mixed liquor O4, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Substance B 7 is obtained, substance B 7 in 85 DEG C of drying box is placed 110 minutes, obtains substance C；
(12) by 4.8 grams of 2- methyl-3-nitrophenylacetic acids and the bromo- 4- hydroxyls -3- nitroquinolines of 6.4 grams of 6- be added to 300mL without
In water-ethanol, stirred 5 minutes under the conditions of 1000r/min, obtain mixed liquor P1；
(13) substance C is added in mixed liquor P1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid and obtain
To substance C 1, substance C 1 in 85 DEG C of drying box is placed 110 minutes, obtains substance C 2；
(14) by 7.9 grams of N- cinnamyl piperazines and 11.2 gram 3,4,6- tribromo pyridazines are added in 300mL absolute ethyl alcohols,
It is stirred 5 minutes under the conditions of 1000r/min, obtains mixed liquor P2；
(15) substance C 2 is added in mixed liquor P2, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Substance C 3 is obtained, substance C 3 in 85 DEG C of drying box is placed 110 minutes, obtains substance C 4；
(16) 4.8 grams of 2- pyridinemethanols and 6.3 grams of 2,4- difluoro pyridines are added in 300mL absolute ethyl alcohols, in 1000r/min
Under the conditions of stir 5 minutes, obtain mixed liquor P3；
(17) substance C 4 is added in mixed liquor P3, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Substance C 5 is obtained, substance C 5 in 85 DEG C of drying box is placed 110 minutes, obtains substance D；
(18) the chloro- 3- pyridazinones of 11.7 grams of 4- and 14.5 grams of 2,5- dichloropyrazines are added in 1500mL absolute ethyl alcohols,
It is stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor Q1, mixed liquor Q2, mixed liquor Q3, mix
Close liquid Q4, mixed liquor Q5；
(19) 8.2 grams of dibenzyl phosphites and 9.9 grams of bromomethyl cyclopropanes are added in 750mL n-butanols, in 1000r/min
Under the conditions of stir 5 minutes, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor R1, mixed liquor R2, mixed liquor R3, mixed liquor R4, mixed
Close liquid R5；
(20) mixed liquor R1 and the bromo- 6- fluoronitrobenzenes of 3.9 grams of 2- are added in mixed liquor Q1, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor S1；
(21) substance D is added in mixed liquor S1, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid and obtain
To substance D1, substance D1 in 85 DEG C of drying box is placed 110 minutes, obtains substance D2；
(22) mixed liquor R2 and the bromo- 6- fluoronitrobenzenes of 4.4 grams of 2- are added in mixed liquor Q2, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor S2；
(23) substance D2 is added in mixed liquor S2, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Substance D3 is obtained, substance D3 in 85 DEG C of drying box is placed 110 minutes, obtains substance D4；
(24) mixed liquor R3 and the bromo- 6- fluoronitrobenzenes of 4.9 grams of 2- are added in mixed liquor Q3, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor S3；
(25) substance D4 is added in mixed liquor S3, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Substance D5 is obtained, substance D5 in 85 DEG C of drying box is placed 110 minutes, obtains substance D6；
(26) mixed liquor R4 and the bromo- 6- fluoronitrobenzenes of 5.4 grams of 2- are added in mixed liquor Q4, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor S4；
(27) substance D6 is added in mixed liquor S4, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Substance D7 is obtained, substance D7 in 85 DEG C of drying box is placed 110 minutes, obtains substance D8；
(28) mixed liquor R5 and the bromo- 6- fluoronitrobenzenes of 5.9 grams of 2- are added in mixed liquor Q5, are stirred under the conditions of 1000r/min
It mixes 3 minutes, obtains mixed liquor S5；
(29) substance D8 is added in mixed liquor S5, is shaken 15 minutes in the shaking table for being 35 DEG C in temperature, be filtered to remove liquid
Substance D9 is obtained, substance D9 in 85 DEG C of drying box is placed 110 minutes, obtains substance E；
(30) by 14.9 grams of Cu (NO3)2With 4.8 grams of Ce (NO3)3It is added in 1200mL deionized waters, under the conditions of 1000r/min
Stirring 10 minutes, is divided into 4 parts of equivalent, obtains mixed liquor T1, mixed liquor T2, mixed liquor T3, mixed liquor T4 after shaking up；
(31) by 4.2 grams of MnCl2With 5.8 grams of ZnCl2It is added in mixed liquor T1, is stirred 10 minutes under the conditions of 1000r/min,
Obtain mixed liquor U1；
(32) substance E is added in mixed liquor U1, is shaken 15 minutes in the shaking table for being 45 DEG C in temperature, be filtered to remove liquid and obtain
To substance E1, substance E1 in 85 DEG C of drying box is placed 110 minutes, obtains substance E2；
(33) by 4.7 grams of MnCl2With 5.3 grams of ZnCl2It is added in mixed liquor T2, is stirred 10 minutes under the conditions of 1000r/min,
Obtain mixed liquor U2；
(34) substance E2 is added in mixed liquor U2, is shaken 15 minutes in the shaking table for being 45 DEG C in temperature, be filtered to remove liquid
Substance E3 is obtained, substance E3 in 85 DEG C of drying box is placed 110 minutes, obtains substance E4；
(35) by 5.2 grams of MnCl2With 4.8 grams of ZnCl2It is added in mixed liquor T3, is stirred 10 minutes under the conditions of 1000r/min,
Obtain mixed liquor U3；
(36) substance E4 is added in mixed liquor U3, is shaken 15 minutes in the shaking table for being 45 DEG C in temperature, be filtered to remove liquid
Substance E5 is obtained, substance E5 in 85 DEG C of drying box is placed 110 minutes, obtains substance E6；
(37) by 5.7 grams of MnCl2With 4.3 grams of ZnCl2It is added in mixed liquor T4, is stirred 10 minutes under the conditions of 1000r/min,
Obtain mixed liquor U4；
(38) substance E6 is added in mixed liquor U4, is shaken 15 minutes in the shaking table for being 45 DEG C in temperature, be filtered to remove liquid
Substance E7 is obtained, substance E7 in 85 DEG C of drying box is placed 110 minutes, obtains substance E8；
(39) by 6.2 grams of MnCl2With 3.8 grams of ZnCl2It is added in mixed liquor T5, is stirred 10 minutes under the conditions of 1000r/min,
Obtain mixed liquor U5；
(40) substance E8 is added in mixed liquor U5, is shaken 15 minutes in the shaking table for being 45 DEG C in temperature, be filtered to remove liquid
Substance E9 is obtained, substance E9 is placed 110 minutes in 85 DEG C of drying box, obtained substance is for Adsorption chemical industry
The modified activated carbon absorbent of benzene in waste water.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106925232A (en) * | 2017-05-11 | 2017-07-07 | 北京益净环保设备科技有限公司 | For the modified pine branch adsorbent of Adsorption polymyxins |
| 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 |
| CN107486158A (en) * | 2017-10-13 | 2017-12-19 | 北京清水润土环保科技有限公司 | There is the montmorillonite-base sorbing material its preparation method of solidification function to mercury in river bottom mud |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106925232A (en) * | 2017-05-11 | 2017-07-07 | 北京益净环保设备科技有限公司 | For the modified pine branch adsorbent of Adsorption polymyxins |
| 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 |
| CN107486158A (en) * | 2017-10-13 | 2017-12-19 | 北京清水润土环保科技有限公司 | There is the montmorillonite-base sorbing material its preparation method of solidification function to mercury in river bottom mud |
Non-Patent Citations (1)
| Title |
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| 王晓玭，等: ""活性炭负载金属改性对废水和废气处理的研究进展"", 《江西化工》 * |
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