CN107930588A - Lithium base magnetism montmorillonite for the pollution of Adsorption caesium and preparation method thereof - Google Patents
Lithium base magnetism montmorillonite for the pollution of Adsorption caesium and preparation method thereof Download PDFInfo
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- CN107930588A CN107930588A CN201711177544.5A CN201711177544A CN107930588A CN 107930588 A CN107930588 A CN 107930588A CN 201711177544 A CN201711177544 A CN 201711177544A CN 107930588 A CN107930588 A CN 107930588A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/027—Compounds of F, Cl, Br, I
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0296—Nitrates of compounds other than those provided for in B01J20/04
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses the lithium base magnetism montmorillonite polluted for Adsorption caesium.Through LiCl, ammonium hydroxide, 4 toluenesulfonic acid pyridines, FeCl after montmorillonite cleaning3、FeCl2The mixed liquor of preparation is modified to be prepared into substance A 04, and 04 dimethyl butyn of substance A, acetic acid N succinimide esters, ethyl carbazate and 3, the mixed liquor of 4,6 trichlorine pyridazines preparation is modified to be prepared into substance A；Substance A is through NbCl4、CeCl3、Cd(NO3)2、Cu(NO3)2The mixed liquor of preparation is modified to be prepared into substance B；Mixed liquor that substance B is prepared through 6 aminopicolinate methyl esters, 1 isoquinolyl methanol and 2 methylamino pyrazines is modified to be prepared into substance C；The modified obtained material of mixed liquor that substance C is prepared through 2 fluorine, 3 aldehyde radical, 4 iodine pyridine, 2 amino, 5 iodine pyrimidine dimethylglyoxime is the lithium base magnetism montmorillonite for being used for the pollution of Adsorption caesium.
Description
Technical field
It is more particularly to a kind of to be used to adsorb the invention belongs to polluted-water and heavy metal in soil pollutant abatement technology field
Remove lithium base magnetism montmorillonite of caesium pollution 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, exploitation is used for
The lithium base magnetism montmorillonite of Adsorption caesium pollution is of great significance polluted-water and heavy metal in soil pollution control.
The content of the invention
The object of the present invention is to provide it is a kind of for Adsorption caesium pollution lithium base magnetism montmorillonite, its preparation method
Comprise the following steps that：
(1) 47.88g montmorillonites are added in the salpeter solution that 250mL mass percent concentrations are 10%, 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 LiCl solution that 450mL molar concentrations are 1.35mol/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 68mL mass concentrations are 19% is added in mixed liquor D, then adds 4.8 grams of 4- methylbenzene sulphurs
Sour pyridine, 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 8.8 grams of FeCl3·6H2O and 13.7 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) 16.1g dimethyl butyns are added in 900mL mass absolute ethyl alcohols, are stirred under the conditions of 1000r/min
Mix 3 minutes, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3, mixed liquor G4, mixed liquor G5；
(8) 7.4 grams of acetic acid-n-succinimidyl esters and 5.3 grams of ethyl carbazates are added to 150mL absolute ethyl alcohols
In, stirred 3 minutes under the conditions of 1000r/min, 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；
(9) by mixed liquor H1 and 8.2 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 2；
(11) by mixed liquor H2 and 8.0 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 4；
(13) by mixed liquor H3 and 7.8 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 6；
(15) by mixed liquor H4 and 7.6 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 8；
(17) by mixed liquor H5 and 7.4 gram 3,4,6- trichlorine pyridazines are added in mixed liquor G5, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J5；
(18) substance A 8 is added in mixed liquor J5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 9, and substance A 9 is placed 65 minutes in 105 DEG C of drying box, obtains substance A；
(19) by 8.11 grams of NbCl4With 6.89 grams of CeCl3It is added in 800mL deionized waters, under the conditions of 1000r/min
Stirring 3 minutes, is divided into 5 parts of equivalent, obtains mixed liquor K1, mixed liquor K2, mixed liquor K3, mixed liquor K4, mixed liquor K5 after shaking up；
(20) Cd (NO by 140mL molar concentrations for 048mol/L3)2Solution and 60mL molar concentrations are 0.62mol/L's
Cu(NO3)2Solution is added in mixed liquor K1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor L1, dense with mole
Spend and the pH value of mixed liquor L1 is adjusted to 6.8~7.2 for the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, obtain
Mixed liquor M1；
(21) substance A is added in mixed liquor M1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Body obtains substance B 1, and substance B 1 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
B2；
(22) Cd (NO by 140mL molar concentrations for 0.58mol/L3)2Solution and 60mL molar concentrations are 0.52mol/L
Cu (NO3)2Solution is added in mixed liquor K2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L2, with mole
Concentration is that the pH value of mixed liquor L2 is adjusted to 6.8~7.2 by the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is obtained
To mixed liquor M2；
(23) substance B 2 is added in mixed liquor M2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance B 3, and substance B 3 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter B4；
(24) Cd (NO by 140mL molar concentrations for 0.68mol/L3)2Solution and 60mL molar concentrations are 0.42mol/L
Cu (NO3)2Solution is added in mixed liquor K3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L3, with mole
Concentration is that the pH value of mixed liquor L3 is adjusted to 6.8~7.2 by the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is obtained
To mixed liquor M3；
(25) substance B 4 is added in mixed liquor M3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance B 5, and substance B 5 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter B6；
(26) Cd (NO by 140mL molar concentrations for 0.78mol/L3)2Solution and 60mL molar concentrations are 0.32mol/L
Cu (NO3)2Solution is added in mixed liquor K4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L4, with mole
Concentration is that the pH value of mixed liquor L4 is adjusted to 6.8~7.2 by the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is obtained
To mixed liquor M4；
(27) substance B 6 is added in mixed liquor M4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance B 7, and substance B 7 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter B8；
(28) Cd (NO by 140mL molar concentrations for 0.88mol/L3)2Solution and 60mL molar concentrations are 0.22mol/L
Cu (NO3)2Solution is added in mixed liquor K5, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L5, with mole
Concentration is that the pH value of mixed liquor L4 is adjusted to 6.8~7.2 by the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is obtained
To mixed liquor M5；
(29) substance B 8 is added in mixed liquor M5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance B 9, and substance B 9 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter B；
(30) 22.5 grams of 6- aminopicolinates methyl esters are added to the anhydrous second of 500mL under 1000r/min stirring conditions
In alcohol, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor N1, mixed liquor N2, mixing
Liquid N3, mixed liquor N4, mixed liquor N5；
(31) 7.6 grams of 1- isoquinolyls methanol and 6.5 grams of 2- methylamino pyrazines are added in mixed liquor N1, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O1；
(32) substance B is added in mixed liquor O1, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Substance C 1 is obtained, substance C 1 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance C 2；
(33) 7.2 grams of 1- isoquinolyls methanol and 6.1 grams of 2- methylamino pyrazines are added in mixed liquor N2, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O2；
(34) substance C 2 is added in mixed liquor O2, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Body obtains substance C 3, and substance C 3 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
C4；
(35) 6.8 grams of 1- isoquinolyls methanol and 5.7 grams of 2- methylamino pyrazines are added in mixed liquor N3, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O3；
(36) substance C 4 is added in mixed liquor O3, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Body obtains substance C 5, and substance C 5 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
C6；
(37) 6.4 grams of 1- isoquinolyls methanol and 5.3 grams of 2- methylamino pyrazines are added in mixed liquor N4, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O4；
(38) substance C 6 is added in mixed liquor O4, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Body obtains substance C 7, and substance C 7 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
C8；
(39) 6.0 grams of 1- isoquinolyls methanol and 4.9 grams of 2- methylamino pyrazines are added in mixed liquor N5, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O5；
(40) substance C 8 is added in mixed liquor O5, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Body obtains substance C 9, and substance C 9 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
C；
(41) that the fluoro- 3- aldehyde radicals -4- iodine pyridines of 22.3 grams of 2- are added to 500mL under 1000r/min stirring conditions is anhydrous
In ethanol, stirred 3 minutes under the conditions of 1000r/min and be divided into 5 parts of equivalent after shaking up, obtain mixed liquor P1, mixed liquor P2, mixing
Liquid P3, mixed liquor P4, mixed liquor P5；
(42) 6.9 grams of 2- amino -5- iodine pyrimidines and 4.4 grams of dimethylglyoximes are added in mixed liquor P1,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q1；
(43) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
D2；
(44) 6.6 grams of 2- amino -5- iodine pyrimidines and 4.7 grams of dimethylglyoximes are added in mixed liquor P2,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q2；
(45) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter D4；
(46) 6.3 grams of 2- amino -5- iodine pyrimidines and 5.0 grams of dimethylglyoximes are added in mixed liquor P3,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q3；
(47) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter D6；
(48) 6.0 grams of 2- amino -5- iodine pyrimidines and 5.3 grams of dimethylglyoximes are added in mixed liquor P4,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q4；
(49) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter D8；
(50) 5.7 grams of 2- amino -5- iodine pyrimidines and 5.6 grams of dimethylglyoximes are added in mixed liquor P5,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q5；
(51) 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 65 minutes in 105 DEG C of drying box after the washing of 100mL deionized waters, obtained
Material is the lithium base magnetism montmorillonite for being used for the pollution of Adsorption caesium.
The invention has the advantages that the obtained lithium base magnetism montmorillonite for the pollution of Adsorption caesium has environment friend
The features such as good, high to caesium adsorption efficiency.
Embodiment
The present invention provides a kind of lithium base magnetism montmorillonite for the pollution of Adsorption caesium, come below by an example
Illustrate its implementation process.
Embodiment 1.
(1) 47.88g montmorillonites are added in the salpeter solution that 250mL mass percent concentrations are 10%, 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 LiCl solution that 450mL molar concentrations are 1.35mol/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 68mL mass concentrations are 19% is added in mixed liquor D, then adds 4.8 grams of 4- methylbenzene sulphurs
Sour pyridine, 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 8.8 grams of FeCl3·6H2O and 13.7 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) 16.1g dimethyl butyns are added in 900mL mass absolute ethyl alcohols, are stirred under the conditions of 1000r/min
Mix 3 minutes, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor G1, mixed liquor G2, mixed liquor G3, mixed liquor G4, mixed liquor G5；
(8) 7.4 grams of acetic acid-n-succinimidyl esters and 5.3 grams of ethyl carbazates are added to 150mL absolute ethyl alcohols
In, stirred 3 minutes under the conditions of 1000r/min, 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；
(9) by mixed liquor H1 and 8.2 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 2；
(11) by mixed liquor H2 and 8.0 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 4；
(13) by mixed liquor H3 and 7.8 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 6；
(15) by mixed liquor H4 and 7.6 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 8；
(17) by mixed liquor H5 and 7.4 gram 3,4,6- trichlorine pyridazines are added in mixed liquor G5, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor J5；
(18) substance A 8 is added in mixed liquor J5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance A 9, and substance A 9 is placed 65 minutes in 105 DEG C of drying box, obtains substance A；
(19) by 8.11 grams of NbCl4With 6.89 grams of CeCl3It is added in 800mL deionized waters, under the conditions of 1000r/min
Stirring 3 minutes, is divided into 5 parts of equivalent, obtains mixed liquor K1, mixed liquor K2, mixed liquor K3, mixed liquor K4, mixed liquor K5 after shaking up；
(20) Cd (NO by 140mL molar concentrations for 048mol/L3)2Solution and 60mL molar concentrations are 0.62mol/L's
Cu(NO3)2Solution is added in mixed liquor K1, is stirred 3 minutes under the conditions of 1000r/min, obtains mixed liquor L1, dense with mole
Spend and the pH value of mixed liquor L1 is adjusted to 6.8~7.2 for the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, obtain
Mixed liquor M1；
(21) substance A is added in mixed liquor M1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Body obtains substance B 1, and substance B 1 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
B2；
(22) Cd (NO by 140mL molar concentrations for 0.58mol/L3)2Solution and 60mL molar concentrations are 0.52mol/L
Cu (NO3)2Solution is added in mixed liquor K2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L2, with mole
Concentration is that the pH value of mixed liquor L2 is adjusted to 6.8~7.2 by the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is obtained
To mixed liquor M2；
(23) substance B 2 is added in mixed liquor M2, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance B 3, and substance B 3 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter B4；
(24) Cd (NO by 140mL molar concentrations for 0.68mol/L3)2Solution and 60mL molar concentrations are 0.42mol/L
Cu (NO3)2Solution is added in mixed liquor K3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L3, with mole
Concentration is that the pH value of mixed liquor L3 is adjusted to 6.8~7.2 by the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is obtained
To mixed liquor M3；
(25) substance B 4 is added in mixed liquor M3, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance B 5, and substance B 5 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter B6；
(26) Cd (NO by 140mL molar concentrations for 0.78mol/L3)2Solution and 60mL molar concentrations are 0.32mol/L
Cu (NO3)2Solution is added in mixed liquor K4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L4, with mole
Concentration is that the pH value of mixed liquor L4 is adjusted to 6.8~7.2 by the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is obtained
To mixed liquor M4；
(27) substance B 6 is added in mixed liquor M4, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance B 7, and substance B 7 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter B8；
(28) Cd (NO by 140mL molar concentrations for 0.88mol/L3)2Solution and 60mL molar concentrations are 0.22mol/L
Cu (NO3)2Solution is added in mixed liquor K5, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L5, with mole
Concentration is that the pH value of mixed liquor L4 is adjusted to 6.8~7.2 by the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is obtained
To mixed liquor M5；
(29) substance B 8 is added in mixed liquor M5, shakes 15 minutes, be filtered to remove in the shaking table that temperature is 30 DEG C
Liquid obtains substance B 9, and substance B 9 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter B；
(30) 22.5 grams of 6- aminopicolinates methyl esters are added to the anhydrous second of 500mL under 1000r/min stirring conditions
In alcohol, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor N1, mixed liquor N2, mixing
Liquid N3, mixed liquor N4, mixed liquor N5；
(31) 7.6 grams of 1- isoquinolyls methanol and 6.5 grams of 2- methylamino pyrazines are added in mixed liquor N1, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O1；
(32) substance B is added in mixed liquor O1, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Substance C 1 is obtained, substance C 1 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance C 2；
(33) 7.2 grams of 1- isoquinolyls methanol and 6.1 grams of 2- methylamino pyrazines are added in mixed liquor N2, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O2；
(34) substance C 2 is added in mixed liquor O2, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Body obtains substance C 3, and substance C 3 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
C4；
(35) 6.8 grams of 1- isoquinolyls methanol and 5.7 grams of 2- methylamino pyrazines are added in mixed liquor N3, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O3；
(36) substance C 4 is added in mixed liquor O3, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Body obtains substance C 5, and substance C 5 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
C6；
(37) 6.4 grams of 1- isoquinolyls methanol and 5.3 grams of 2- methylamino pyrazines are added in mixed liquor N4, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O4；
(38) substance C 6 is added in mixed liquor O4, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Body obtains substance C 7, and substance C 7 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
C8；
(39) 6.0 grams of 1- isoquinolyls methanol and 4.9 grams of 2- methylamino pyrazines are added in mixed liquor N5, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor O5；
(40) substance C 8 is added in mixed liquor O5, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid
Body obtains substance C 9, and substance C 9 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
C；
(41) that the fluoro- 3- aldehyde radicals -4- iodine pyridines of 22.3 grams of 2- are added to 500mL under 1000r/min stirring conditions is anhydrous
In ethanol, stirred 3 minutes under the conditions of 1000r/min and be divided into 5 parts of equivalent after shaking up, obtain mixed liquor P1, mixed liquor P2, mixing
Liquid P3, mixed liquor P4, mixed liquor P5；
(42) 6.9 grams of 2- amino -5- iodine pyrimidines and 4.4 grams of dimethylglyoximes are added in mixed liquor P1,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q1；
(43) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material
D2；
(44) 6.6 grams of 2- amino -5- iodine pyrimidines and 4.7 grams of dimethylglyoximes are added in mixed liquor P2,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q2；
(45) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter D4；
(46) 6.3 grams of 2- amino -5- iodine pyrimidines and 5.0 grams of dimethylglyoximes are added in mixed liquor P3,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q3；
(47) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter D6；
(48) 6.0 grams of 2- amino -5- iodine pyrimidines and 5.3 grams of dimethylglyoximes are added in mixed liquor P4,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q4；
(49) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains thing
Matter D8；
(50) 5.7 grams of 2- amino -5- iodine pyrimidines and 5.6 grams of dimethylglyoximes are added in mixed liquor P5,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor Q5；
(51) 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 65 minutes in 105 DEG C of drying box after the washing of 100mL deionized waters, obtained
Material is the lithium base magnetism montmorillonite for being used for the pollution of Adsorption caesium.
Here is to containing caesium with the obtained lithium base magnetism montmorillonite for the pollution of Adsorption caesium of the method for the present invention
Polluted-water carried out adsorption Removal, further illustrate the present invention.
Lithium base magnetism montmorillonite made from the method for the present invention adsorbs the polluted-water containing caesium, the results showed that：
When caesium initial concentration is 56.9mg/L, into 1000mL caesium polluted-waters, addition 11.3g uses lithium made from the method for the present invention
After base magnetism montmorillonite, adsorption time is 12 minutes, and the caesium concentration after processing in water body is reduced to 0.01mg/L.
Claims (1)
1. a kind of lithium base magnetism montmorillonite for the pollution of Adsorption caesium, it is characterised in that prepare the lithium base magnetism montmorillonite
Method comprises the following steps that：
(1) 47.88g montmorillonites are added in the salpeter solution that 250mL mass percent concentrations are 10%, 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 LiCl solution that 450mL molar concentrations are 1.35mol/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 68mL mass concentrations are 19% is added in mixed liquor D, then adds 4.8 grams of 4- toluenesulfonic acid pyrroles
Pyridine, 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, 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 8.8 grams of FeCl3·6H2O and 13.7 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) 16.1g dimethyl butyns are added in 900mL mass absolute ethyl alcohols, 3 is stirred under the conditions of 1000r/min
Minute, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor G1, mixed liquor G2, mixed liquor G3, mixed liquor G4, mixed liquor G5；
(8) 7.4 grams of acetic acid-n-succinimidyl esters and 5.3 grams of ethyl carbazates are added in 150mL absolute ethyl alcohols,
Stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3, mixed
Close liquid H4, mixed liquor H5；
(9) mixed liquor H1 and 8.2 gram 3,4,6- trichlorine pyridazines 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 65 minutes in 105 DEG C of drying box, obtains substance A 2；
(11) mixed liquor H2 and 8.0 gram 3,4,6- trichlorine pyridazines 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 is placed 65 minutes in 105 DEG C of drying box, obtains substance A 4；
(13) mixed liquor H3 and 7.8 gram 3,4,6- trichlorine pyridazines 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 is placed 65 minutes in 105 DEG C of drying box, obtains substance A 6；
(15) mixed liquor H4 and 7.6 gram 3,4,6- trichlorine pyridazines 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 is placed 65 minutes in 105 DEG C of drying box, obtains substance A 8；
(17) mixed liquor H5 and 7.4 gram 3,4,6- trichlorine pyridazines are added in mixed liquor G5, are stirred under the conditions of 1000r/min
3 minutes, obtain mixed liquor J5；
(18) substance A 8 is added in mixed liquor J5, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance A 9 is obtained, substance A 9 is placed 65 minutes in 105 DEG C of drying box, obtains substance A；
(19) by 8.11 grams of NbCl4With 6.89 grams of CeCl3It is added in 800mL deionized waters, 3 is stirred under the conditions of 1000r/min
Minute, 5 parts of equivalent is divided into after shaking up, obtains mixed liquor K1, mixed liquor K2, mixed liquor K3, mixed liquor K4, mixed liquor K5；
(20) Cd (NO by 140mL molar concentrations for 048mol/L3)2Solution and the Cu that 60mL molar concentrations are 0.62mol/L
(NO3)2Solution is added in mixed liquor K1, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L1, use molar concentration
The pH value of mixed liquor L1 is adjusted to 6.8~7.2 for the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is mixed
Close liquid M1；
(21) substance A is added in mixed liquor M1, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid and obtain
To substance B 1, substance B 1 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance B 2；
(22) Cd (NO by 140mL molar concentrations for 0.58mol/L3)2Solution and the Cu that 60mL molar concentrations are 0.52mol/L
(NO3)2Solution is added in mixed liquor K2, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L2, use molar concentration
The pH value of mixed liquor L2 is adjusted to 6.8~7.2 for the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is mixed
Close liquid M2；
(23) substance B 2 is added in mixed liquor M2, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance B 3 is obtained, substance B 3 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance B 4；
(24) Cd (NO by 140mL molar concentrations for 0.68mol/L3)2Solution and the Cu that 60mL molar concentrations are 0.42mol/L
(NO3)2Solution is added in mixed liquor K3, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L3, use molar concentration
The pH value of mixed liquor L3 is adjusted to 6.8~7.2 for the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is mixed
Close liquid M3；
(25) substance B 4 is added in mixed liquor M3, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance B 5 is obtained, substance B 5 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance B 6；
(26) Cd (NO by 140mL molar concentrations for 0.78mol/L3)2Solution and the Cu that 60mL molar concentrations are 0.32mol/L
(NO3)2Solution is added in mixed liquor K4, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L4, use molar concentration
The pH value of mixed liquor L4 is adjusted to 6.8~7.2 for the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is mixed
Close liquid M4；
(27) substance B 6 is added in mixed liquor M4, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance B 7 is obtained, substance B 7 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance B 8；
(28) Cd (NO by 140mL molar concentrations for 0.88mol/L3)2Solution and the Cu that 60mL molar concentrations are 0.22mol/L
(NO3)2Solution is added in mixed liquor K5, is stirred 3 minutes under the conditions of 1000r/min, is obtained mixed liquor L5, use molar concentration
The pH value of mixed liquor L4 is adjusted to 6.8~7.2 for the hydrochloric acid solution of 0.01mol/L and the NaOH solution of 0.01mol/L, is mixed
Close liquid M5；
(29) substance B 8 is added in mixed liquor M5, is shaken 15 minutes in the shaking table that temperature is 30 DEG C, be filtered to remove liquid
Substance B 9 is obtained, substance B 9 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance B；
(30) 22.5 grams of 6- aminopicolinates methyl 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 N1, mixed liquor N2, mixed liquor N3,
Mixed liquor N4, mixed liquor N5；
(31) 7.6 grams of 1- isoquinolyls methanol and 6.5 grams of 2- methylamino pyrazines are added in mixed liquor N1, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O1；
(32) substance B is added in mixed liquor O1, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid and obtain
Substance C 1, substance C 1 are placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtain substance C 2；
(33) 7.2 grams of 1- isoquinolyls methanol and 6.1 grams of 2- methylamino pyrazines are added in mixed liquor N2, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O2；
(34) substance C 2 is added in mixed liquor O2, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid and obtain
To substance C 3, substance C 3 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance C 4；
(35) 6.8 grams of 1- isoquinolyls methanol and 5.7 grams of 2- methylamino pyrazines are added in mixed liquor N3, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O3；
(36) substance C 4 is added in mixed liquor O3, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid and obtain
To substance C 5, substance C 5 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance C 6；
(37) 6.4 grams of 1- isoquinolyls methanol and 5.3 grams of 2- methylamino pyrazines are added in mixed liquor N4, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O4；
(38) substance C 6 is added in mixed liquor O4, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid and obtain
To substance C 7, substance C 7 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance C 8；
(39) 6.0 grams of 1- isoquinolyls methanol and 4.9 grams of 2- methylamino pyrazines are added in mixed liquor N5, in 1000r/min
Under the conditions of stir 3 minutes, obtain mixed liquor O5；
(40) substance C 8 is added in mixed liquor O5, is stirred 3 minutes under the conditions of 1000r/min, after be filtered to remove liquid and obtain
To substance C 9, substance C 9 is placed 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains substance C；
(41) the fluoro- 3- aldehyde radicals -4- iodine pyridines of 22.3 grams of 2- are added to 500mL absolute ethyl alcohols under 1000r/min stirring conditions
In, stirred 3 minutes under the conditions of 1000r/min and be divided into 5 parts of equivalent after shaking up, obtain mixed liquor P1, mixed liquor P2, mixed liquor
P3, mixed liquor P4, mixed liquor P5；
(42) 6.9 grams of 2- amino -5- iodine pyrimidines and 4.4 grams of dimethylglyoximes are added in mixed liquor P1, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor Q1；
(43) 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 65 minutes in 105 DEG C of drying box after the washing of 100mL deionized waters to material D1, material D1, obtain material D2；
(44) 6.6 grams of 2- amino -5- iodine pyrimidines and 4.7 grams of dimethylglyoximes are added in mixed liquor P2, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor Q2；
(45) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material D4；
(46) 6.3 grams of 2- amino -5- iodine pyrimidines and 5.0 grams of dimethylglyoximes are added in mixed liquor P3, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor Q3；
(47) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material D6；
(48) 6.0 grams of 2- amino -5- iodine pyrimidines and 5.3 grams of dimethylglyoximes are added in mixed liquor P4, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor Q4；
(49) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtains material D8；
(50) 5.7 grams of 2- amino -5- iodine pyrimidines and 5.6 grams of dimethylglyoximes are added in mixed liquor P5, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor Q5；
(51) 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 65 minutes after the washing of 100mL deionized waters in 105 DEG C of drying box, obtained material
As it is used for the lithium base magnetism montmorillonite of Adsorption caesium pollution.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105286A (en) * | 1993-09-29 | 1995-07-19 | 美国胶体公司 | Method of improving the contaminant resistance of a smectite clay by rewetting and impregnating the clay with a water-soluble poly mer, and redrying the polymer-impregnated clay |
| 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 |
| CN106669595A (en) * | 2017-01-07 | 2017-05-17 | 北京源清益壤环保科技有限公司 | Modified attapulgite adsorbent for removing cadmium in polluted water and preparation method of modified attapulgite adsorbent |
| CN106853361A (en) * | 2017-01-07 | 2017-06-16 | 北京源清益壤环保科技有限公司 | Modified zeolite adsorbent and preparation method thereof for removing mercury in polluted-water |
-
2017
- 2017-11-23 CN CN201711177544.5A patent/CN107930588A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1105286A (en) * | 1993-09-29 | 1995-07-19 | 美国胶体公司 | Method of improving the contaminant resistance of a smectite clay by rewetting and impregnating the clay with a water-soluble poly mer, and redrying the polymer-impregnated clay |
| 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 |
| CN106669595A (en) * | 2017-01-07 | 2017-05-17 | 北京源清益壤环保科技有限公司 | Modified attapulgite adsorbent for removing cadmium in polluted water and preparation method of modified attapulgite adsorbent |
| CN106853361A (en) * | 2017-01-07 | 2017-06-16 | 北京源清益壤环保科技有限公司 | Modified zeolite adsorbent and preparation method thereof for removing mercury in polluted-water |
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Application publication date: 20180420 |