CN107899539A - There is magnetic montmorillonite being modified based on sodium of adsorption function and preparation method thereof to caesium - Google Patents
There is magnetic montmorillonite being modified based on sodium of adsorption function and preparation method thereof to caesium Download PDFInfo
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- CN107899539A CN107899539A CN201711177562.3A CN201711177562A CN107899539A CN 107899539 A CN107899539 A CN 107899539A CN 201711177562 A CN201711177562 A CN 201711177562A CN 107899539 A CN107899539 A CN 107899539A
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Abstract
The invention discloses the magnetic montmorillonite being modified based on sodium to caesium with adsorption function.The mixed liquor through NaCl, ammonium hydroxide, 1 cyclohexyl methyl piperazine, FeCl3 and FeCl2 preparation is modified after montmorillonite cleans is prepared into substance A 04, substance A 04 is through 2 hydroxyl, 5 chloropyrazine, 1 butyl piperazine, 2,2,2 trichloroacetamide benzyl esters and 2, the mixed liquor of 3 dicyano pyrazines preparation is modified to be prepared into substance A；Mixed liquor that substance A is prepared through tetramethylpiperidinol, N (2 chlorphenyl) acetamides and 1 hydroxy-anthraquione is modified to be prepared into substance C；The modified obtained material of mixed liquor that substance C is prepared through 2 piperazine carboxylic acid ethyl esters, 2 fluorine pyridine, 6 carboxylic acid and 3 cyano group, 6 trifluoromethyl pyridine is the magnetic montmorillonite being modified based on sodium for having to caesium adsorption function.
Description
Technical field
It is more particularly to a kind of to have to caesium the invention belongs to polluted-water and heavy metal in soil pollutant abatement technology field
Magnetic montmorillonite being modified based on sodium of adsorption function and preparation method thereof.
Background technology
Since heavy metal has the characteristics that high toxicity, refractory organics, persistence, the heavy metal pollution of water body becomes one sternly
Universal environmental problem again, has been subject to the extensive concern of domestic and foreign scholars.Heavy metal can occur in human body with protein
Interaction, makes it lose activity, can also be enriched with some organs of human body, if the limit that can bear more than human body,
Lung, kidney, liver and other vitals are influenced by blood circulation, the diseases such as poisoning can be caused, to the very harmful of human body.
Therefore, the effective heavy metal pollution of water body treatment technology of exploiting economy, has great society, economy and Significance for Environment.At present,
Common Heavy Metals in Waters ion remaval method has chemical precipitation, absorption, heavy metal chelating, electrolysis, redox, ion to hand over
Change with UF membrane etc., wherein, adsorption technology due to have the advantages that quick, expense is low, treatment effeciency is high, it is easy to operate be subject to it is wide
General concern.But also lack cheap, the efficient sorbing material for removing caesium in polluted-water at present, therefore, develop to caesium
The magnetic montmorillonite being modified based on sodium with adsorption function is to polluted-water with heavy metal in soil pollution control with important
Meaning.
The content of the invention
The object of the present invention is to provide a kind of magnetic montmorillonite being modified based on sodium to caesium with adsorption function, it is prepared
Method comprises the following steps that：
(1) 53.27g montmorillonites are added in the sulfuric acid solution that 250mL mass percent concentrations are 12%, in 1000r/
Stirred 50 minutes under the conditions of min, be filtered to remove liquid, 35 are placed in 105 DEG C of drying box after the washing of 500mL deionized waters
Minute, obtain substance A 01；
(2) substance A 01 is added in the NaCl solution that 450mL molar concentrations are 1.22mol/L, is 35 DEG C in temperature
When shake 1.5 is small in shaking table, mixed liquor D is obtained；
(3) ammonium hydroxide that 74mL mass concentrations are 19% is added in mixed liquor D, then adds 6.3 grams of 1- cyclohexyl methyls
Piperazine, stirs 4h under the conditions of 1000r/min, obtains mixed liquor E；
(4) mixed liquor E is centrifuged into 5min under conditions of rotating speed is 7000 turn per minute, upper strata supernatant is removed, by under
Layer solid matter dry 24h under the conditions of 60 DEG C, obtains substance A 02；
(5) by 12.9 grams of FeCl3·6H2O and 22.8 gram of FeCl2·4H2O is added sequentially in 450mL deionized waters,
15min is stirred under the conditions of 1000r/min, then adds 50mL NH3·H2O, under the conditions of 1000r/min stirring 1 it is small when after, obtain
To mixed liquor F；
(6) substance A 02 is added in mixed liquor F, is shaken 25 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Body obtains substance A 03, and substance A 03 is placed 65 minutes in 105 DEG C of drying box, obtains substance A 04；
(7) 19.8 grams of 2- hydroxyl -5- chloropyrazines are added in 800mL absolute ethyl alcohols, are stirred under the conditions of 1000r/min
3 minutes, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor G1, mixed liquor G2, mixed liquor G3, mixed liquor G4；
(8) 8.7 grams of 1- butyl piperazines and 5.6 gram 2,2,2- trichloroacetamide benzyl esters are added in 150mL absolute ethyl alcohols,
Stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent be divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3,
Mixed liquor H4；
(9) mixed liquor H1 and 8.8 grams of 2,3- dicyano pyrazines are added in mixed liquor G1, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J1；
(10) substance A 04 is added in mixed liquor J1, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 1, and substance A 1 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace in 485 DEG C of bars
Roasted 45 minutes under part, obtain substance A 2；
(11) mixed liquor H2 and 8.5 grams of 2,3- dicyano pyrazines are added in mixed liquor G2, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J2；
(12) substance A 2 is added in mixed liquor J2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 3, and substance A 3 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace in 485 DEG C of conditions
Lower roasting 45 minutes, obtains substance A 4；
(13) mixed liquor H3 and 8.2 grams of 2,3- dicyano pyrazines are added in mixed liquor G3, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J3；
(14) substance A 4 is added in mixed liquor J3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 5, and substance A 5 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace in 485 DEG C of conditions
Lower roasting 45 minutes, obtains substance A 6；
(15) mixed liquor H4 and 7.9 grams of 2,3- dicyano pyrazines are added in mixed liquor G4, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J4；
(16) substance A 6 is added in mixed liquor J4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 7, and substance A 7 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace in 485 DEG C of conditions
Lower roasting 45 minutes, obtains substance A；
(17) 11.2 grams of tetramethylpiperidinols are added in 500mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed
Close liquid N4；
(18) 4.2 grams of N- (2- chlorphenyls) acetamides and 3.5 grams of 1- hydroxy-anthraquiones are added in mixed liquor N1,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O1；
(19) substance A is added in mixed liquor O1, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain
To substance B, substance B obtains substance C 1 after the washing of 100m deionized waters, and substance C 1 places 45 points in 104 DEG C of drying box
Clock, obtains substance C 2；
(20) 4.5 grams of N- (2- chlorphenyls) acetamides and 3.8 grams of 1- hydroxy-anthraquiones are added in mixed liquor N2,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O2；
(21) substance C 2 is added in mixed liquor O2, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid
Substance C 3 is obtained, substance C 3 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains substance C 4；
(22) 4.8 grams of N- (2- chlorphenyls) acetamides and 4.1 grams of 1- hydroxy-anthraquiones are added in mixed liquor N3,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O3；
(23) substance C 4 is added in mixed liquor O3, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid
Substance C 5 is obtained, substance C 5 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains substance C 6；
(24) 5.1 grams of N- (2- chlorphenyls) acetamides and 4.4 grams of 1- hydroxy-anthraquiones are added in mixed liquor N4,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O4；
(25) substance C 6 is added in mixed liquor O4, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid
Substance C 7 is obtained, substance C 7 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains substance C；
(26) 20.3 grams of 2- piperazine carboxylic acids ethyl esters are added in 500mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3,
Mixed liquor P4, mixed liquor P5；
(27) 2.9 grams of 2- fluorine pyridine -6- carboxylic acids and 1.4 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P1
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q1；
(28) substance C is added in mixed liquor Q1, 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 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material
D2；
(29) 2.7 grams of 2- fluorine pyridine -6- carboxylic acids and 1.6 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P2
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q2；
(30) material D2 is added in mixed liquor Q2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains material D3, and material D3 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material
D4；
(31) 2.5 grams of 2- fluorine pyridine -6- carboxylic acids and 1.8 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P3
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q3；
(32) material D4 is added in mixed liquor Q3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains material D5, and material D5 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material
D6；
(33) 2.3 grams of 2- fluorine pyridine -6- carboxylic acids and 2.0 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P4
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q4；
(34) material D6 is added in mixed liquor Q4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains material D7, and material D7 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material
D8；
(35) 2.1 grams of 2- fluorine pyridine -6- carboxylic acids and 2.2 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P5
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q5；
(36) material D8 is added in mixed liquor Q5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains material D9, and material D9 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtained thing
Matter is the magnetic montmorillonite being modified based on sodium for having to caesium adsorption function.
The invention has the advantages that it is obtained to caesium with adsorption function based on sodium be modified magnetic montmorillonite with
The features such as environmental-friendly, high to caesium adsorption efficiency.
Embodiment
The present invention provides a kind of magnetic montmorillonite being modified based on sodium to caesium with adsorption function, below by one
Example illustrates to apply process in fact.
Embodiment 1.
(1) 53.27g montmorillonites are added in the sulfuric acid solution that 250mL mass percent concentrations are 12%, in 1000r/
Stirred 50 minutes under the conditions of min, be filtered to remove liquid, 35 are placed in 105 DEG C of drying box after the washing of 500mL deionized waters
Minute, obtain substance A 01；
(2) substance A 01 is added in the NaCl solution that 450mL molar concentrations are 1.22mol/L, is 35 DEG C in temperature
When shake 1.5 is small in shaking table, mixed liquor D is obtained；
(3) ammonium hydroxide that 74mL mass concentrations are 19% is added in mixed liquor D, then adds 6.3 grams of 1- cyclohexyl methyls
Piperazine, stirs 4h under the conditions of 1000r/min, obtains mixed liquor E；
(4) mixed liquor E is centrifuged into 5min under conditions of rotating speed is 7000 turn per minute, upper strata supernatant is removed, by under
Layer solid matter dry 24h under the conditions of 60 DEG C, obtains substance A 02；
(5) by 12.9 grams of FeCl3·6H2O and 22.8 gram of FeCl2·4H2O is added sequentially in 450mL deionized waters,
15min is stirred under the conditions of 1000r/min, then adds 50mL NH3·H2O, under the conditions of 1000r/min stirring 1 it is small when after, obtain
To mixed liquor F；
(6) substance A 02 is added in mixed liquor F, is shaken 25 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Body obtains substance A 03, and substance A 03 is placed 65 minutes in 105 DEG C of drying box, obtains substance A 04；
(7) 19.8 grams of 2- hydroxyl -5- chloropyrazines are added in 800mL absolute ethyl alcohols, are stirred under the conditions of 1000r/min
3 minutes, 4 parts of equivalent is divided into after shaking up, obtains mixed liquor G1, mixed liquor G2, mixed liquor G3, mixed liquor G4；
(8) 8.7 grams of 1- butyl piperazines and 5.6 gram 2,2,2- trichloroacetamide benzyl esters are added in 150mL absolute ethyl alcohols,
Stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent be divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3,
Mixed liquor H4；
(9) mixed liquor H1 and 8.8 grams of 2,3- dicyano pyrazines are added in mixed liquor G1, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J1；
(10) substance A 04 is added in mixed liquor J1, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 1, and substance A 1 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace in 485 DEG C of bars
Roasted 45 minutes under part, obtain substance A 2；
(11) mixed liquor H2 and 8.5 grams of 2,3- dicyano pyrazines are added in mixed liquor G2, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J2；
(12) substance A 2 is added in mixed liquor J2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 3, and substance A 3 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace in 485 DEG C of conditions
Lower roasting 45 minutes, obtains substance A 4；
(13) mixed liquor H3 and 8.2 grams of 2,3- dicyano pyrazines are added in mixed liquor G3, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J3；
(14) substance A 4 is added in mixed liquor J3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 5, and substance A 5 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace in 485 DEG C of conditions
Lower roasting 45 minutes, obtains substance A 6；
(15) mixed liquor H4 and 7.9 grams of 2,3- dicyano pyrazines are added in mixed liquor G4, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J4；
(16) substance A 6 is added in mixed liquor J4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 7, and substance A 7 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace in 485 DEG C of conditions
Lower roasting 45 minutes, obtains substance A；
(17) 11.2 grams of tetramethylpiperidinols are added in 500mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed
Close liquid N4；
(18) 4.2 grams of N- (2- chlorphenyls) acetamides and 3.5 grams of 1- hydroxy-anthraquiones are added in mixed liquor N1,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O1；
(19) substance A is added in mixed liquor O1, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain
To substance B, substance B obtains substance C 1 after the washing of 100m deionized waters, and substance C 1 places 45 points in 104 DEG C of drying box
Clock, obtains substance C 2；
(20) 4.5 grams of N- (2- chlorphenyls) acetamides and 3.8 grams of 1- hydroxy-anthraquiones are added in mixed liquor N2,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O2；
(21) substance C 2 is added in mixed liquor O2, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid
Substance C 3 is obtained, substance C 3 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains substance C 4；
(22) 4.8 grams of N- (2- chlorphenyls) acetamides and 4.1 grams of 1- hydroxy-anthraquiones are added in mixed liquor N3,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O3；
(23) substance C 4 is added in mixed liquor O3, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid
Substance C 5 is obtained, substance C 5 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains substance C 6；
(24) 5.1 grams of N- (2- chlorphenyls) acetamides and 4.4 grams of 1- hydroxy-anthraquiones are added in mixed liquor N4,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor O4；
(25) substance C 6 is added in mixed liquor O4, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid
Substance C 7 is obtained, substance C 7 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains substance C；
(26) 20.3 grams of 2- piperazine carboxylic acids ethyl esters are added in 500mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent be divided into after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3,
Mixed liquor P4, mixed liquor P5；
(27) 2.9 grams of 2- fluorine pyridine -6- carboxylic acids and 1.4 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P1
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q1；
(28) substance C is added in mixed liquor Q1, 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 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material
D2；
(29) 2.7 grams of 2- fluorine pyridine -6- carboxylic acids and 1.6 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P2
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q2；
(30) material D2 is added in mixed liquor Q2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains material D3, and material D3 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material
D4；
(31) 2.5 grams of 2- fluorine pyridine -6- carboxylic acids and 1.8 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P3
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q3；
(32) material D4 is added in mixed liquor Q3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains material D5, and material D5 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material
D6；
(33) 2.3 grams of 2- fluorine pyridine -6- carboxylic acids and 2.0 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P4
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q4；
(34) material D6 is added in mixed liquor Q4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains material D7, and material D7 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material
D8；
(35) 2.1 grams of 2- fluorine pyridine -6- carboxylic acids and 2.2 grams of 3- cyano group -6- trifluoromethyl pyridines are added to mixed liquor P5
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q5；
(36) material D8 is added in mixed liquor Q5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains material D9, and material D9 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtained thing
Matter is the magnetic montmorillonite being modified based on sodium for having to caesium adsorption function.
Here is with the obtained magnetic montmorillonite pair being modified based on sodium to caesium with adsorption function of the method for the present invention
Polluted-water containing caesium has carried out adsorption Removal, further illustrates the present invention.
The magnetic montmorillonite being modified made from the method for the present invention based on sodium adsorbs the polluted-water containing caesium, ties
Fruit shows：When caesium initial concentration is 88.3mg/L, into 1000mL caesium polluted-waters, addition 12.8g uses the method for the present invention system
After the magnetic montmorillonite being modified based on sodium obtained, adsorption time is 15 minutes, and the caesium concentration after processing in water body is reduced to
0.02mg/L。
Claims (1)
1. a kind of magnetic montmorillonite being modified based on sodium to caesium with adsorption function, it is characterised in that it is de- to prepare magnetism illiteracy
Cubic meter of stone method comprises the following steps that：
(1) 53.27g montmorillonites are added in the sulfuric acid solution that 250mL mass percent concentrations are 12%, in 1000r/min
Under the conditions of stir 50 minutes, be filtered to remove liquid, through 500mL deionized waters washing after in 105 DEG C of drying box place 35 points
Clock, obtains substance A 01；
(2) substance A 01 is added in the NaCl solution that 450mL molar concentrations are 1.22mol/L, in the shaking table that temperature is 35 DEG C
It is middle shake 1.5 it is small when, obtain mixed liquor D；
(3) ammonium hydroxide that 74mL mass concentrations are 19% is added in mixed liquor D, then adds 6.3 grams of 1- cyclohexyl methyl piperazines,
4h is stirred under the conditions of 1000r/min, obtains mixed liquor E；
(4) mixed liquor E is centrifuged into 5min under conditions of rotating speed is 7000 turn per minute, removes upper strata supernatant, lower floor is consolidated
Body material dry 24h under the conditions of 60 DEG C, obtains substance A 02；
(5) by 12.9 grams of FeCl3·6H2O and 22.8 gram of FeCl2·4H2O is added sequentially in 450mL deionized waters, in 1000r/
15min is stirred under the conditions of min, then adds 50mL NH3·H2O, under the conditions of 1000r/min stirring 1 it is small when after, mixed
Liquid F；
(6) substance A 02 is added in mixed liquor F, is shaken 25 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain
To substance A 03, substance A 03 is placed 65 minutes in 105 DEG C of drying box, obtains substance A 04；
(7) 19.8 grams of 2- hydroxyl -5- chloropyrazines are added in 800mL absolute ethyl alcohols, 3 points is stirred under the conditions of 1000r/min
Clock, is divided into 4 parts of equivalent after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3, mixed liquor G4；
(8) 8.7 grams of 1- butyl piperazines and 5.6 gram 2,2,2- trichloroacetamide benzyl esters are added in 150mL absolute ethyl alcohols,
Stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed
Close liquid H4；
(9) mixed liquor H1 and 8.8 grams of 2,3- dicyano pyrazines are added in mixed liquor G1,3 is stirred under the conditions of 1000r/min
Minute, obtain mixed liquor J1；
(10) substance A 04 is added in mixed liquor J1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance A 1 is obtained, substance A 1 is placed 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace under the conditions of 485 DEG C
Roasting 45 minutes, obtains substance A 2；
(11) mixed liquor H2 and 8.5 grams of 2,3- dicyano pyrazines are added in mixed liquor G2, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor J2；
(12) substance A 2 is added in mixed liquor J2, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance A 3 is obtained, substance A 3 places 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace and roasted under the conditions of 485 DEG C
Burn 45 minutes, obtain substance A 4；
(13) mixed liquor H3 and 8.2 grams of 2,3- dicyano pyrazines are added in mixed liquor G3, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor J3；
(14) substance A 4 is added in mixed liquor J3, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance A 5 is obtained, substance A 5 places 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace and roasted under the conditions of 485 DEG C
Burn 45 minutes, obtain substance A 6；
(15) mixed liquor H4 and 7.9 grams of 2,3- dicyano pyrazines are added in mixed liquor G4, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor J4；
(16) substance A 6 is added in mixed liquor J4, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance A 7 is obtained, substance A 7 places 35 minutes in 105 DEG C of drying box, is subsequently placed in Muffle furnace and roasted under the conditions of 485 DEG C
Burn 45 minutes, obtain substance A；
(17) 11.2 grams of tetramethylpiperidinols are added in 500mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor N1, mixed liquor N2, mixed liquor N3, mixed
Close liquid N4；
(18) 4.2 grams of N- (2- chlorphenyls) acetamides and 3.5 grams of 1- hydroxy-anthraquiones are added in mixed liquor N1, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O1；
(19) substance A is added in mixed liquor O1, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain thing
Matter B, substance B obtain substance C 1 after the washing of 100m deionized waters, and substance C 1 is placed 45 minutes in 104 DEG C of drying box, obtained
To substance C 2；
(20) 4.5 grams of N- (2- chlorphenyls) acetamides and 3.8 grams of 1- hydroxy-anthraquiones are added in mixed liquor N2, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O2；
(21) substance C 2 is added in mixed liquor O2, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain
Substance C 3, substance C 3 are placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtain substance C 4；
(22) 4.8 grams of N- (2- chlorphenyls) acetamides and 4.1 grams of 1- hydroxy-anthraquiones are added in mixed liquor N3, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O3；
(23) substance C 4 is added in mixed liquor O3, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain
Substance C 5, substance C 5 are placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtain substance C 6；
(24) 5.1 grams of N- (2- chlorphenyls) acetamides and 4.4 grams of 1- hydroxy-anthraquiones are added in mixed liquor N4, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O4；
(25) substance C 6 is added in mixed liquor O4, is stirred 3 minutes under the conditions of 1000r/min, be filtered to remove liquid and obtain
Substance C 7, substance C 7 are placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtain substance C；
(26) 20.3 grams of 2- piperazine carboxylic acids ethyl esters are added in 500mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor P3, mixed
Close liquid P4, mixed liquor P5；
(27) 2.9 grams of 2- fluorine pyridine -6- carboxylic acids and 1.4 grams of 3- cyano group -6- trifluoromethyl pyridines are added in mixed liquor P1,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q1；
(28) substance C is added in mixed liquor Q1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain
Placed 45 minutes in 104 DEG C of drying box after the washing of 100m deionized waters to material D1, material D1, obtain material D2；
(29) 2.7 grams of 2- fluorine pyridine -6- carboxylic acids and 1.6 grams of 3- cyano group -6- trifluoromethyl pyridines are added in mixed liquor P2,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q2；
(30) material D2 is added in mixed liquor Q2, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Material D3 is obtained, material D3 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material D4；
(31) 2.5 grams of 2- fluorine pyridine -6- carboxylic acids and 1.8 grams of 3- cyano group -6- trifluoromethyl pyridines are added in mixed liquor P3,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q3；
(32) material D4 is added in mixed liquor Q3, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Material D5 is obtained, material D5 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material D6；
(33) 2.3 grams of 2- fluorine pyridine -6- carboxylic acids and 2.0 grams of 3- cyano group -6- trifluoromethyl pyridines are added in mixed liquor P4,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q4；
(34) material D6 is added in mixed liquor Q4, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Material D7 is obtained, material D7 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, obtains material D8；
(35) 2.1 grams of 2- fluorine pyridine -6- carboxylic acids and 2.2 grams of 3- cyano group -6- trifluoromethyl pyridines are added in mixed liquor P5,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q5；
(36) material D8 is added in mixed liquor Q5, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Material D9 is obtained, material D9 is placed 45 minutes after the washing of 100m deionized waters in 104 DEG C of drying box, and obtained material is i.e.
To have the magnetic montmorillonite being modified based on sodium of adsorption function to caesium.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103611514A (en) * | 2013-12-12 | 2014-03-05 | 北京师范大学 | Multifunctional adsorption particles capable of treating industrial organic wastewater with imbalance of nitrogen and phosphorus and preparation method thereof |
| CN106475045A (en) * | 2017-01-07 | 2017-03-08 | 北京源清益壤环保科技有限公司 | For removing modified bentonite adsorbent of copper and preparation method thereof in polluted-water |
| CN106552579A (en) * | 2017-01-07 | 2017-04-05 | 北京源清益壤环保科技有限公司 | For removing modified kaolin adsorbent of lead in polluted-water and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103611514A (en) * | 2013-12-12 | 2014-03-05 | 北京师范大学 | Multifunctional adsorption particles capable of treating industrial organic wastewater with imbalance of nitrogen and phosphorus and preparation method thereof |
| CN106475045A (en) * | 2017-01-07 | 2017-03-08 | 北京源清益壤环保科技有限公司 | For removing modified bentonite adsorbent of copper and preparation method thereof in polluted-water |
| CN106552579A (en) * | 2017-01-07 | 2017-04-05 | 北京源清益壤环保科技有限公司 | For removing modified kaolin adsorbent of lead in polluted-water and preparation method thereof |
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Application publication date: 20180413 |