CN107930578A - PERFORMANCE OF MODIFIED VERMICULITE adsorbent for benzene in Adsorption wastewater from chemical industry - Google Patents
PERFORMANCE OF MODIFIED VERMICULITE adsorbent for benzene in Adsorption wastewater from chemical industry Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a kind of PERFORMANCE OF MODIFIED VERMICULITE adsorbent for being used for benzene in Adsorption wastewater from chemical industry.Through Pb (NO after vermiculite cleaning3)2、Mn(NO3)2、ZnCl2、CuCl2The mixed liquor of preparation is modified to be prepared into substance C；The mixed liquor that substance C is prepared through acetyl diphenylamine N, N ethyl piperazidines, 5 Aminopyrazine, 2 carboxylic acid, ethyl ester modified is prepared into material D；Material D is through 3 bromothiophene, 2 formaldehyde, 3, the material of the modified preparation of mixed liquor prepared by 4 dibromo thiophenes, 4 methyl, 2 chloroquinoline, 3 chlorine, 6 iodine pyridazine, 2 pyridine carboxylic acid ethyl esters, 2,6 dichlorobenzaldehydes, ethyl p-toluenesulfonate, 2 nitrophenyl-acetic acids is the PERFORMANCE OF MODIFIED VERMICULITE adsorbent for being used for benzene in Adsorption wastewater from chemical industry.
Description
Technical field
It is more particularly to a kind of to be used for Adsorption chemical industry the invention belongs to difficult degradation organic chemical waste water processing technology field
The PERFORMANCE OF MODIFIED VERMICULITE adsorbent 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 reach separated method.The reaction of adsorbate and adsorbent is very fast, it need not add any again
Medicine, it is easy to operate, while widely used adsorbent all has higher adsorption capacity and bigger ratio surface at present
Product, so as to promote absorption method to remove the advantage such as pollutant is efficient and adaptable in waste water.Adsorbent also has in itself
The characteristics of secondary pollution will not bring new chemical substance will not be produced, it typically takes place in the surface of adsorbent.Therefore inhale
Attached method because having the characteristics that easy to operate, flexibility is high, operating cost is low, insensitive to toxic pollutant and environmental-friendly,
It is widely used in organic chemical waste water process field.
Up to the present, various types of adsorbents be found and progressively be introduced in processing wastewater application in.In quilt
It was found that adsorbent in be used for wastewater treatment in be broadly divided into three major types：One kind is inorganic material class adsorbent, such as zeolite, viscous
The materials such as soil, silica；Another kind of is the adsorbent based on carbons, such as activated carbon, graphite, carbon molecular sieve etc.；3rd
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.
The content of the invention
The object of the present invention is to provide a kind of PERFORMANCE OF MODIFIED VERMICULITE adsorbent for being used for benzene in Adsorption wastewater from chemical industry, it is prepared
Method comprises the following steps that：
(1) 54.3 grams of vermiculite granules that particle diameter is 2~4cm are put into 400mL acetone solns and soaked 20 minutes, crossed and filter out
Go liquid to obtain substance A 0, substance A 0 is put into 400mL absolute ethyl alcohols and is soaked 20 minutes, liquid is filtered to remove and obtains material
A1, substance A 1 obtain substance A 2 after 300mL originally water washing, and substance A 2 is dry at 110 DEG C after the washing of 300mL deionized waters
Placed 50 minutes in dry case, obtain substance A；
(2) by 6.6 grams of Pb (NO3)2With 3.7 grams of Mn (NO3)2It is added in 1500mL deionized waters, in 1000r/min bars
Stirred 10 minutes under part, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor H4, mixing
Liquid H5；
(3) ZnCl by 140mL molar concentrations for 2.35mol/L2Solution and 60mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H1, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room temperature
After be filtered to remove liquid and obtain substance B 1, substance B 1 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance B 2；
(5) ZnCl by 130mL molar concentrations for 2.35mol/L2Solution and 70mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H2, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room temperature
After be filtered to remove liquid and obtain substance B 3, substance B 3 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance B 4；
(7) ZnCl by 120mL molar concentrations for 2.35mol/L2Solution and 80mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H3, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room temperature
After be filtered to remove liquid and obtain substance B 5, substance B 5 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance B 6；
(9) ZnCl by 110mL molar concentrations for 2.35mol/L2Solution and 90mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H4, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room
Liquid is filtered to remove after temperature and obtains substance B 7, substance B 7 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance B 8；
(11) ZnCl by 100mL molar concentrations for 2.35mol/L2Solution and 100mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H5, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J5；
(12) substance B 8 is added in mixed liquor J5, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room
Liquid is filtered to remove after temperature and obtains substance B 9, substance B 9 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance C；
(13) 18.4 grams of acetyl diphenylamine Ns and 14.1 grams of n-ethylpiperazine are added in 900mL absolute ethyl alcohols,
Stirred 5 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor K1, mixed liquor K2, mixed liquor K3；
(14) 6.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K1, are stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor L1；
(15) substance C is added in mixed liquor L1, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 is placed 120 minutes in 85 DEG C of drying box, obtains substance C 2；
(16) 5.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K2, are stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor L2；
(17) substance C 2 is added in mixed liquor L2, shakes 10 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance C 3, and substance C 3 is placed 120 minutes in 85 DEG C of drying box, obtains substance C 4；
(18) 4.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K3, are stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor L3；
(19) substance C 4 is added in mixed liquor L3, shakes 10 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance C 5, and substance C 5 is placed 120 minutes in 85 DEG C of drying box, obtains material D；
(20) 14.4 grams of 3 bromo thiophene -2- formaldehyde and 9.7 grams of 3,4- dibromo thiophenes 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 M1, mixed liquor M2, mixed liquor M3,
Mixed liquor M4, mixed liquor M5；
(21) 8.8 grams of 4- methyl -2- chlorine-quinolines and the chloro- 6- iodine pyridazines of 7.4 grams of 3- are added in 750mL methanol,
Stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed
Close liquid N4, mixed liquor N5；
(22) mixed liquor N1 and 6.8 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M1, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O1；
(23) material D is added in mixed liquor O1, is shaken 15 minutes in the shaking table that temperature is 40 DEG C, be filtered to remove liquid
Body obtains material D1, and material D1 is placed 100 minutes in 75 DEG C of drying box, obtains material D2；
(24) mixed liquor N2 and 6.2 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M2, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O2；
(25) material D2 is added in mixed liquor O2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 40 DEG C
Liquid obtains material D3, and material D3 is placed 100 minutes in 75 DEG C of drying box, obtains material D4；
(26) mixed liquor N3 and 5.6 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M3, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O3；
(27) material D4 is added in mixed liquor O3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 40 DEG C
Liquid obtains material D5, and material D5 is placed 100 minutes in 75 DEG C of drying box, obtains material D6；
(28) mixed liquor N4 and 5.0 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M4, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O4；
(29) material D6 is added in mixed liquor O4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 40 DEG C
Liquid obtains material D7, and material D7 is placed 100 minutes in 75 DEG C of drying box, obtains material D8；
(30) mixed liquor N5 and 4.4 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M5, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O5；
(31) material D8 is added in mixed liquor O5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 40 DEG C
Liquid obtains material D9, and material D9 is placed 100 minutes in 75 DEG C of drying box, obtains material E；
(32) 7.9 grams of 2,6- dichlorobenzaldehydes and 11.4 grams of ethyl p-toluenesulfonates are added in 800mL n-hexanes,
Stirred 5 minutes under the conditions of 1000r/min, 2 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2；
(33) 8.8 grams of 2- nitrophenyl-acetic acids are added in mixed liquor P1, stir 3 minutes, obtain under the conditions of 1000r/min
To mixed liquor Q1；
(34) material E is added in mixed liquor Q1, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material E1, and material E1 is placed 100 minutes in 75 DEG C of drying box, obtains material E2；
(35) 7.8 grams of 2- nitrophenyl-acetic acids are added in mixed liquor P2, stir 3 minutes, obtain under the conditions of 1000r/min
To mixed liquor Q2；
(36) material 2E is added in mixed liquor Q2, shakes 10 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains material E3, and material E3 is placed 100 minutes in 75 DEG C of drying box, and obtained material is to be used for Adsorption
The PERFORMANCE OF MODIFIED VERMICULITE adsorbent of benzene in wastewater from chemical industry.
The invention has the advantages that the obtained PERFORMANCE OF MODIFIED VERMICULITE adsorbent for being used for benzene in Adsorption wastewater from chemical industry has
, removal efficiency high the features such as big to benzene adsorption capacity.
Embodiment
The present invention provides a kind of PERFORMANCE OF MODIFIED VERMICULITE adsorbent for being used for benzene in Adsorption wastewater from chemical industry, below by a reality
Example illustrates to apply process in fact.
Embodiment 1.
(1) 54.3 grams of vermiculite granules that particle diameter is 2~4cm are put into 400mL acetone solns and soaked 20 minutes, crossed and filter out
Go liquid to obtain substance A 0, substance A 0 is put into 400mL absolute ethyl alcohols and is soaked 20 minutes, liquid is filtered to remove and obtains material
A1, substance A 1 obtain substance A 2 after 300mL originally water washing, and substance A 2 is dry at 110 DEG C after the washing of 300mL deionized waters
Placed 50 minutes in dry case, obtain substance A；
(2) by 6.6 grams of Pb (NO3)2With 3.7 grams of Mn (NO3)2It is added in 1500mL deionized waters, in 1000r/min bars
Stirred 10 minutes under part, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor H4, mixing
Liquid H5；
(3) ZnCl by 140mL molar concentrations for 2.35mol/L2Solution and 60mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H1, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room temperature
After be filtered to remove liquid and obtain substance B 1, substance B 1 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance B 2；
(5) ZnCl by 130mL molar concentrations for 2.35mol/L2Solution and 70mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H2, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room temperature
After be filtered to remove liquid and obtain substance B 3, substance B 3 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance B 4；
(7) ZnCl by 120mL molar concentrations for 2.35mol/L2Solution and 80mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H3, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room temperature
After be filtered to remove liquid and obtain substance B 5, substance B 5 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance B 6；
(9) ZnCl by 110mL molar concentrations for 2.35mol/L2Solution and 90mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H4, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room
Liquid is filtered to remove after temperature and obtains substance B 7, substance B 7 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance B 8；
(11) ZnCl by 100mL molar concentrations for 2.35mol/L2Solution and 100mL molar concentrations are 1.67mol/L's
CuCl2Solution is added in mixed liquor H5, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J5；
(12) substance B 8 is added in mixed liquor J5, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to room
Liquid is filtered to remove after temperature and obtains substance B 9, substance B 9 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace
Roasted 50 minutes under the conditions of 490 DEG C, obtain substance C；
(13) 18.4 grams of acetyl diphenylamine Ns and 14.1 grams of n-ethylpiperazine are added in 900mL absolute ethyl alcohols,
Stirred 5 minutes under the conditions of 1000r/min, 3 parts of equivalent is divided into after shaking up, obtain mixed liquor K1, mixed liquor K2, mixed liquor K3；
(14) 6.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K1, are stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor L1；
(15) substance C is added in mixed liquor L1, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains substance C 1, and substance C 1 is placed 120 minutes in 85 DEG C of drying box, obtains substance C 2；
(16) 5.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K2, are stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor L2；
(17) substance C 2 is added in mixed liquor L2, shakes 10 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance C 3, and substance C 3 is placed 120 minutes in 85 DEG C of drying box, obtains substance C 4；
(18) 4.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K3, are stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor L3；
(19) substance C 4 is added in mixed liquor L3, shakes 10 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains substance C 5, and substance C 5 is placed 120 minutes in 85 DEG C of drying box, obtains material D；
(20) 14.4 grams of 3 bromo thiophene -2- formaldehyde and 9.7 grams of 3,4- dibromo thiophenes 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 M1, mixed liquor M2, mixed liquor M3,
Mixed liquor M4, mixed liquor M5；
(21) 8.8 grams of 4- methyl -2- chlorine-quinolines and the chloro- 6- iodine pyridazines of 7.4 grams of 3- are added in 750mL methanol,
Stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed
Close liquid N4, mixed liquor N5；
(22) mixed liquor N1 and 6.8 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M1, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O1；
(23) material D is added in mixed liquor O1, is shaken 15 minutes in the shaking table that temperature is 40 DEG C, be filtered to remove liquid
Body obtains material D1, and material D1 is placed 100 minutes in 75 DEG C of drying box, obtains material D2；
(24) mixed liquor N2 and 6.2 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M2, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O2；
(25) material D2 is added in mixed liquor O2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 40 DEG C
Liquid obtains material D3, and material D3 is placed 100 minutes in 75 DEG C of drying box, obtains material D4；
(26) mixed liquor N3 and 5.6 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M3, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O3；
(27) material D4 is added in mixed liquor O3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 40 DEG C
Liquid obtains material D5, and material D5 is placed 100 minutes in 75 DEG C of drying box, obtains material D6；
(28) mixed liquor N4 and 5.0 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M4, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O4；
(29) material D6 is added in mixed liquor O4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 40 DEG C
Liquid obtains material D7, and material D7 is placed 100 minutes in 75 DEG C of drying box, obtains material D8；
(30) mixed liquor N5 and 4.4 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M5, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor O5；
(31) material D8 is added in mixed liquor O5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 40 DEG C
Liquid obtains material D9, and material D9 is placed 100 minutes in 75 DEG C of drying box, obtains material E；
(32) 7.9 grams of 2,6- dichlorobenzaldehydes and 11.4 grams of ethyl p-toluenesulfonates are added in 800mL n-hexanes,
Stirred 5 minutes under the conditions of 1000r/min, 2 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2；
(33) 8.8 grams of 2- nitrophenyl-acetic acids are added in mixed liquor P1, stir 3 minutes, obtain under the conditions of 1000r/min
To mixed liquor Q1；
(34) material E is added in mixed liquor Q1, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Body obtains material E1, and material E1 is placed 100 minutes in 75 DEG C of drying box, obtains material E2；
(35) 7.8 grams of 2- nitrophenyl-acetic acids are added in mixed liquor P2, stir 3 minutes, obtain under the conditions of 1000r/min
To mixed liquor Q2；
(36) material 2E is added in mixed liquor Q2, shakes 10 minutes, be filtered to remove in the shaking table that temperature is 45 DEG C
Liquid obtains material E3, and material E3 is placed 100 minutes in 75 DEG C of drying box, and obtained material is to be used for Adsorption
The PERFORMANCE OF MODIFIED VERMICULITE adsorbent of benzene in wastewater from chemical industry.
Here is with the obtained PERFORMANCE OF MODIFIED VERMICULITE adsorbent pair for being used for benzene in Adsorption wastewater from chemical industry of the method for the present invention
Waste water containing benzene has carried out adsorption test, further illustrates the present invention.
PERFORMANCE OF MODIFIED VERMICULITE adsorbent made from the method for the present invention has been subjected to adsorption test to the organic chemical waste water containing benzene,
The result shows that when benzene initial concentration is 41.1mg/L, 16.5g is added into 1000mL waste water with made from the method for the present invention
After PERFORMANCE OF MODIFIED VERMICULITE adsorbent, adsorption time is 5 minutes, and the benzene concentration in processed waste water is reduced to 0.1mg/L, by Static Adsorption
The Freundlich Isothermal Models of experiment understand that PERFORMANCE OF MODIFIED VERMICULITE adsorbent made from the method for the present invention is to the maximal absorptive capacity of benzene
211.7mg/g。
Claims (1)
1. a kind of PERFORMANCE OF MODIFIED VERMICULITE adsorbent for being used for benzene in Adsorption wastewater from chemical industry, it is characterised in that prepare vermiculite absorption
Agent method comprises the following steps that：
(1) 54.3 grams of vermiculite granules that particle diameter is 2~4cm are put into 400mL acetone solns and soaked 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 soaked 20 minutes, liquid is filtered to remove and obtains substance A 1, thing
Matter A1 obtains substance A 2 after 300mL originally water washing, and substance A 2 is after the washing of 300mL deionized waters in 110 DEG C of drying box
It is middle to place 50 minutes, obtain substance A；
(2) by 6.6 grams of Pb (NO3)2With 3.7 grams of Mn (NO3)2It is added in 1500mL deionized waters, is stirred under the conditions of 1000r/min
Mix 10 minutes, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed liquor H4, mixed liquor H5；
(3) ZnCl by 140mL molar concentrations for 2.35mol/L2Solution and the CuCl that 60mL molar concentrations are 1.67mol/L2It is molten
Liquid is added in mixed liquor H1, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J1；
(4) substance A is added in mixed liquor J1, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to mistake after room temperature
Filter out liquid and obtain substance B 1, substance B 1 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace at 490 DEG C
Under the conditions of roast 50 minutes, obtain substance B 2；
(5) ZnCl by 130mL molar concentrations for 2.35mol/L2Solution and the CuCl that 70mL molar concentrations are 1.67mol/L2It is molten
Liquid is added in mixed liquor H2, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J2；
(6) substance B 2 is added in mixed liquor J2, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to mistake after room temperature
Filter out liquid and obtain substance B 3, substance B 3 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace at 490 DEG C
Under the conditions of roast 50 minutes, obtain substance B 4；
(7) ZnCl by 120mL molar concentrations for 2.35mol/L2Solution and the CuCl that 80mL molar concentrations are 1.67mol/L2It is molten
Liquid is added in mixed liquor H3, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J3；
(8) substance B 4 is added in mixed liquor J3, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, be cooled to mistake after room temperature
Filter out liquid and obtain substance B 5, substance B 5 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace at 490 DEG C
Under the conditions of roast 50 minutes, obtain substance B 6；
(9) ZnCl by 110mL molar concentrations for 2.35mol/L2Solution and the CuCl that 90mL molar concentrations are 1.67mol/L2It is molten
Liquid is added in mixed liquor H4, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J4；
(10) substance B 6 is added in mixed liquor J4, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, after being cooled to room temperature
It is filtered to remove liquid and obtains substance B 7, substance B 7 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace 490
Roasted 50 minutes under the conditions of DEG C, obtain substance B 8；
(11) ZnCl by 100mL molar concentrations for 2.35mol/L2Solution and the CuCl that 100mL molar concentrations are 1.67mol/L2
Solution is added in mixed liquor H5, is stirred 10 minutes under the conditions of 1000r/min, is obtained mixed liquor J5；
(12) substance B 8 is added in mixed liquor J5, is shaken 20 minutes in the shaking table that temperature is 95 DEG C, after being cooled to room temperature
It is filtered to remove liquid and obtains substance B 9, substance B 9 is placed 90 minutes in 85 DEG C of drying box, is subsequently placed in Muffle furnace 490
Roasted 50 minutes under the conditions of DEG C, obtain substance C；
(13) 18.4 grams of acetyl diphenylamine Ns and 14.1 grams of n-ethylpiperazine are added in 900mL absolute ethyl alcohols, in 1000r/min
Under the conditions of stir 5 minutes, 3 parts of equivalent is divided into after shaking up, obtains mixed liquor K1, mixed liquor K2, mixed liquor K3；
(14) 6.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K1,3 points is stirred under the conditions of 1000r/min
Clock, obtains mixed liquor L1；
(15) substance C is added in mixed liquor L1, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid and obtain
To substance C 1, substance C 1 is placed 120 minutes in 85 DEG C of drying box, obtains substance C 2；
(16) 5.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K2,3 points is stirred under the conditions of 1000r/min
Clock, obtains mixed liquor L2；
(17) substance C 2 is added in mixed liquor L2, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance C 3 is obtained, substance C 3 is placed 120 minutes in 85 DEG C of drying box, obtains substance C 4；
(18) 4.3 grams of 5- Aminopyrazine -2- carboxylic acid, ethyl esters are added in mixed liquor K3,3 points is stirred under the conditions of 1000r/min
Clock, obtains mixed liquor L3；
(19) substance C 4 is added in mixed liquor L3, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Substance C 5 is obtained, substance C 5 is placed 120 minutes in 85 DEG C of drying box, obtains material D；
(20) 14.4 grams of 3 bromo thiophene -2- formaldehyde and 9.7 grams of 3,4- dibromo thiophenes are added in 1500mL absolute ethyl alcohols,
Stirred 5 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor M1, mixed liquor M2, mixed liquor M3, mixed
Close liquid M4, mixed liquor M5；
(21) 8.8 grams of 4- methyl -2- chlorine-quinolines and the chloro- 6- iodine pyridazines of 7.4 grams of 3- are added in 750mL methanol, in 1000r/
Stirred 5 minutes under the conditions of min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed liquor N4,
Mixed liquor N5；
(22) mixed liquor N1 and 6.8 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M1, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor O1；
(23) material D is added in mixed liquor O1, is shaken 15 minutes in the shaking table that temperature is 40 DEG C, be filtered to remove liquid and obtain
To material D1, material D1 is placed 100 minutes in 75 DEG C of drying box, obtains material D2；
(24) mixed liquor N2 and 6.2 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M2, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor O2；
(25) material D2 is added in mixed liquor O2, is shaken 15 minutes in the shaking table that temperature is 40 DEG C, be filtered to remove liquid
Material D3 is obtained, material D3 is placed 100 minutes in 75 DEG C of drying box, obtains material D4；
(26) mixed liquor N3 and 5.6 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M3, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor O3；
(27) material D4 is added in mixed liquor O3, is shaken 15 minutes in the shaking table that temperature is 40 DEG C, be filtered to remove liquid
Material D5 is obtained, material D5 is placed 100 minutes in 75 DEG C of drying box, obtains material D6；
(28) mixed liquor N4 and 5.0 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M4, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor O4；
(29) material D6 is added in mixed liquor O4, is shaken 15 minutes in the shaking table that temperature is 40 DEG C, be filtered to remove liquid
Material D7 is obtained, material D7 is placed 100 minutes in 75 DEG C of drying box, obtains material D8；
(30) mixed liquor N5 and 4.4 grams of 2- pyridine carboxylic acid ethyl esters are added in mixed liquor M5, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor O5；
(31) material D8 is added in mixed liquor O5, is shaken 15 minutes in the shaking table that temperature is 40 DEG C, be filtered to remove liquid
Material D9 is obtained, material D9 is placed 100 minutes in 75 DEG C of drying box, obtains material E；
(32) 7.9 grams of 2,6- dichlorobenzaldehydes and 11.4 grams of ethyl p-toluenesulfonates are added in 800mL n-hexanes,
Stirred 5 minutes under the conditions of 1000r/min, 2 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2；
(33) 8.8 grams of 2- nitrophenyl-acetic acids are added in mixed liquor P1, stir 3 minutes, mixed under the conditions of 1000r/min
Close liquid Q1；
(34) material E is added in mixed liquor Q1, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid and obtain
To material E1, material E1 is placed 100 minutes in 75 DEG C of drying box, obtains material E2；
(35) 7.8 grams of 2- nitrophenyl-acetic acids are added in mixed liquor P2, stir 3 minutes, mixed under the conditions of 1000r/min
Close liquid Q2；
(36) material 2E is added in mixed liquor Q2, is shaken 10 minutes in the shaking table that temperature is 45 DEG C, be filtered to remove liquid
Material E3 is obtained, material E3 is placed 100 minutes in 75 DEG C of drying box, obtained material is to be used for Adsorption chemical industry
The PERFORMANCE OF MODIFIED VERMICULITE adsorbent of benzene in waste water.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU3113999A (en) * | 1998-03-24 | 1999-10-18 | Mycelx Technologies Corporation | Filter constructions and methods |
| US20020036168A1 (en) * | 1998-03-24 | 2002-03-28 | Hal Alper | Protection of crossflow membranes from organic fouling |
| CN101455955A (en) * | 2007-12-13 | 2009-06-17 | 中国科学院兰州化学物理研究所 | Clay base composite absorbent and preparation method thereof |
| CN101811021A (en) * | 2010-04-26 | 2010-08-25 | 西北农林科技大学 | Amphiphilic adsorbent capable of adsorbing both organic matter and heavy metal cation and preparation method thereof |
| CN102350301A (en) * | 2011-07-05 | 2012-02-15 | 中国科学院广州地球化学研究所 | Organically modified expanded vermiculite |
| CN106669594A (en) * | 2017-01-07 | 2017-05-17 | 北京源清益壤环保科技有限公司 | Modified vermiculite adsorbent for removing manganese in polluted water body and preparation method of modified vermiculite adsorbent |
| 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 |
-
2017
- 2017-12-25 CN CN201711414332.4A patent/CN107930578A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU3113999A (en) * | 1998-03-24 | 1999-10-18 | Mycelx Technologies Corporation | Filter constructions and methods |
| US20020036168A1 (en) * | 1998-03-24 | 2002-03-28 | Hal Alper | Protection of crossflow membranes from organic fouling |
| CN101455955A (en) * | 2007-12-13 | 2009-06-17 | 中国科学院兰州化学物理研究所 | Clay base composite absorbent and preparation method thereof |
| CN101811021A (en) * | 2010-04-26 | 2010-08-25 | 西北农林科技大学 | Amphiphilic adsorbent capable of adsorbing both organic matter and heavy metal cation and preparation method thereof |
| CN102350301A (en) * | 2011-07-05 | 2012-02-15 | 中国科学院广州地球化学研究所 | Organically modified expanded vermiculite |
| CN106669594A (en) * | 2017-01-07 | 2017-05-17 | 北京源清益壤环保科技有限公司 | Modified vermiculite adsorbent for removing manganese in polluted water body and preparation method of modified vermiculite adsorbent |
| 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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