CN106925232A - For the modified pine branch adsorbent of Adsorption polymyxins - Google Patents
For the modified pine branch adsorbent of Adsorption polymyxins Download PDFInfo
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- CN106925232A CN106925232A CN201710329565.8A CN201710329565A CN106925232A CN 106925232 A CN106925232 A CN 106925232A CN 201710329565 A CN201710329565 A CN 201710329565A CN 106925232 A CN106925232 A CN 106925232A
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- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
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Abstract
The invention discloses the modified pine branch adsorbent for Adsorption polymyxins.Selection particle diameter is that the pine branch of 4~6mm is washed with deionized water, absolute ethyl alcohol, NaOH solution and obtains material Q after drying；Mixed liquors of the material Q through being prepared by 6 Cyanoisoquinolines, 6 carboxyl cumarins, 4,5 pyridazine dicarboxylic acids, 4 (2 aminoethyl) oxinanes, the iodine pyridine of 2 fluorine 3, the methylisoquinolinium of 5 bromine 4 is modified to be prepared into material R；Mixed liquors of the material R through being prepared by copper nitrate, ferric nitrate, lithium chloride, cesium fluoride and ammonium heptamolybdate is modified to be prepared into material S；The mixed liquor modified materials that obtains of the material S through being prepared by methyl tributanoximo silane, dichloromethyl phenylsilane and 2 aminobenzophenones is the modified pine branch adsorbent for Adsorption polymyxins.
Description
Technical field
It is more particularly to a kind of many for Adsorption the invention belongs to the adsorption treatment technical field of antibiotic waste water treatment
The modified pine branch adsorbent of colistin.
Background technology
Antibiotic waste water is class colourity depth, the high concentrated organic wastewater that suspension content is more, salt content is high, and composition is extremely
Complexity, significant damage is produced to environment, is classified as the environmental problem that the new period pays close attention to by many developed countries.It is anti-
Raw element can induce generation endurance strain in use, and continuing to bring out for high drug-resistance bacterium will have a strong impact on ecosystem
Unite, toxicity is produced to aquatile, and human health is threatened by food chain enrichment.Therefore, antibiotic is controlled in environment
Reason is particularly important.Antibiotic with polymyxins as representative has been detected by its presence as broad-spectrum antibacterial agent in drinking water source,
Conventional waste water processing method can not effectively remove antibiotic in waste water, be badly in need of carrying out effective removal skill of such antibiotic waste water
Art.Absorption method is because it is simple, convenient and clearance higher is considered as a kind of method of the most frequently used removal antibiotic.
But conventional adsorbent is present, and, adsorption capacity poor to specific antibiotic selection is low, easily receive environmental factor shadow
The shortcomings of ringing, limits popularization and application of the adsorption technology in antibiotic waste water treatment and development, so being glued for specific more
Rhzomorph antibiotic, research and the preparation of novel absorption material also need to further reinforcement, particularly also lack for adsorbing at present
Remove the adsorbent of polymyxins.
The content of the invention
It is an object of the invention to provide a kind of modified pine branch adsorbent for Adsorption polymyxins, its preparation side
Method is comprised the following steps that：
(1) 500 grams of pine branch are placed in pulverizer and are crushed, the sieve that 4mm and 6mm are respectively with aperture is sieved,
Obtain the pine branch that particle diameter is 4~6mm；
(2) 500mL absolute ethyl alcohols are put into after the pine branch that 90 grams are obtained by step (1) is washed with 500mL deionized waters
Middle immersion 1 hour, removes liquid and obtains Substance P after filtering, Substance P obtains Substance P 1 after being washed through 500mL deionized waters, by thing
Matter P1 puts into the NaOH solution that 500mL molar concentrations are 3.7mol/L and soaks 1 hour, liquid is removed after filtering and obtains material
P2, Substance P 2 obtains Substance P 3 after being washed with 500mL deionized waters, Substance P 3 is obtained after being placed 12 hours in 50 DEG C of drying box
To material Q；
(3) 9.9 grams of 6- Cyanoisoquinolines are added in 700mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, be subsequently adding the 2mL concentrated sulfuric acids, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor A 1, mix
Close liquid A2, mixed liquor A 3, mixed liquor A 4, mixed liquor A 5；
(4) 9.9 grams of 6- carboxyls cumarins are added in 700mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, be subsequently adding 12.3 grams of 4,5- pyridazine dicarboxylic acids, 5 parts of equivalent is divided into after shaking up, obtained
Mixed liquid B 1, mixed liquid B 2, mixed liquid B 3, mixed liquid B 4, mixed liquid B 5；
(5) 7.6 grams of 4- (2- aminoethyls) oxinanes and 8.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 1, so
After be placed in temperature to shake 30 minutes in 45 DEG C of shaking tables, obtain mixed liquor C1；
(6) mixed liquor C1 and 8.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor D1；
(7) material Q is added in mixed liquor D1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Body obtains material Q1, and material Q1 is placed 4 hours in 65 DEG C of drying box, obtains material Q2；
(8) 7.1 grams of 4- (2- aminoethyls) oxinanes and 7.8 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 2, so
After be placed in temperature to shake 30 minutes in 45 DEG C of shaking tables, obtain mixed liquor C2；
(9) mixed liquor C2 and 8.1 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor D2；
(10) material Q2 is added in mixed liquor D2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material Q3, and material Q3 is placed 4 hours in 65 DEG C of drying box, obtains material Q4；
(11) 6.6 grams of 4- (2- aminoethyls) oxinanes and 7.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 3,
Temperature is subsequently placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C3 is obtained；
(12) mixed liquor C3 and 7.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 3, in 1000r/min bars
Stirred 3 minutes under part, obtain mixed liquor D3；
(13) material Q4 is added in mixed liquor D3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material Q5, and material Q5 is placed 4 hours in 65 DEG C of drying box, obtains material Q6；
(14) 6.1 grams of 4- (2- aminoethyls) oxinanes and 6.8 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 4,
Temperature is subsequently placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C4 is obtained；
(15) mixed liquor C4 and 7.1 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 4, in 1000r/min bars
Stirred 3 minutes under part, obtain mixed liquor D4；
(16) material Q6 is added in mixed liquor D4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material Q7, and material Q7 is placed 4 hours in 65 DEG C of drying box, obtains material Q8；
(17) 5.6 grams of 4- (2- aminoethyls) oxinanes and 6.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 5,
Temperature is subsequently placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C5 is obtained；
(18) mixed liquor C5 and 6.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 5, in 1000r/min bars
Stirred 3 minutes under part, obtain mixed liquor D5；
(19) material Q8 is added in mixed liquor D5, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material Q9, and material Q9 is placed 4 hours in 65 DEG C of drying box, obtains material R；
(20) by 8.33 grams of copper nitrates and 4.77 grams of ferric nitrates be added under 1000r/min stirring conditions 500mL go from
In sub- water, stirred 15 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor E1, mixed liquor E2, mix
Close liquid E3, mixed liquor E4, mixed liquor E5；
(21) by 2.19 grams lithium chlorides and 2.27 grams of cesium fluorides be added under 1000r/min stirring conditions 500mL go from
In sub- water, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor F1, mixed liquor F2, mix
Close liquid F3, mixed liquor F4, mixed liquor F5；
(22) by mixed liquor E1 and 19mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F1
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G1；
(23) material R is added in mixed liquor G1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Body obtains material R1, and material R1 is placed 4 hours in 65 DEG C of drying box, obtains material R2；
(24) by mixed liquor E2 and 17mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F2
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G2；
(25) material R2 is added in mixed liquor G2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material R3, and material R3 is placed 4 hours in 65 DEG C of drying box, obtains material R4；
(26) by mixed liquor E3 and 15mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F3
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G3；
(27) material R4 is added in mixed liquor G3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material R5, and material R5 is placed 4 hours in 65 DEG C of drying box, obtains material R6；
(28) by mixed liquor E4 and 13mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F4
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G4；
(29) material R6 is added in mixed liquor G4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material R7, and material R7 is placed 4 hours in 65 DEG C of drying box, obtains material R8；
(30) by mixed liquor E5 and 11mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F5
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G5；
(31) material R8 is added in mixed liquor G5, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material R9, and material R9 is placed 4 hours in 65 DEG C of drying box, obtains material S；
(32) 8.26 grams of methyl tributanoximo silanes are added to the anhydrous second of 800mL under 1000r/min stirring conditions
In alcohol, stirred 5 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixing
Liquid H3, mixed liquor H4；
(33) 5.6 grams of dichloromethyl phenylsilanes and 8.3 grams of 2- aminobenzophenones are added in mixed liquor H1,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor J1；
(34) material S is added in mixed liquor J1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Body obtains material S1, and material S1 is placed 4 hours in 65 DEG C of drying box, obtains material S2；
(35) 5.1 grams of dichloromethyl phenylsilanes and 7.8 grams of 2- aminobenzophenones are added in mixed liquor H2,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor J2；
(36) material S2 is added in mixed liquor J2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material S3, and material S3 is placed 4 hours in 65 DEG C of drying box, obtains material S4；
(37) 4.6 grams of dichloromethyl phenylsilanes and 7.3 grams of 2- aminobenzophenones are added in mixed liquor H3,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor J3；
(38) material S4 is added in mixed liquor J3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material S5, and material S5 is placed 4 hours in 65 DEG C of drying box, obtains material S6；
(39) 4.1 grams of dichloromethyl phenylsilanes and 6.8 grams of 2- aminobenzophenones are added in mixed liquor H4,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor J4；
(40) material S6 is added in mixed liquor J4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material S7, and material S7 is placed 4 hours in 65 DEG C of drying box, and the material for obtaining is many for Adsorption
The modified pine branch adsorbent of colistin.
The beneficial effects of the invention are as follows the obtained modified pine branch adsorbent for Adsorption polymyxins has right
The features such as polymyxins adsorbs strong selection, adsorption capacity high, strong antijamming capability.
Specific embodiment
The present invention provides a kind of modified pine branch adsorbent for Adsorption polymyxins, below by an example
To illustrate to apply process in fact.
Embodiment 1.
(1) 500 grams of pine branch are placed in pulverizer and are crushed, the sieve that 4mm and 6mm are respectively with aperture is sieved,
Obtain the pine branch that particle diameter is 4~6mm；
(2) 500mL absolute ethyl alcohols are put into after the pine branch that 90 grams are obtained by step (1) is washed with 500mL deionized waters
Middle immersion 1 hour, removes liquid and obtains Substance P after filtering, Substance P obtains Substance P 1 after being washed through 500mL deionized waters, by thing
Matter P1 puts into the NaOH solution that 500mL molar concentrations are 3.7mol/L and soaks 1 hour, liquid is removed after filtering and obtains material
P2, Substance P 2 obtains Substance P 3 after being washed with 500mL deionized waters, Substance P 3 is obtained after being placed 12 hours in 50 DEG C of drying box
To material Q；
(3) 9.9 grams of 6- Cyanoisoquinolines are added in 700mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, be subsequently adding the 2mL concentrated sulfuric acids, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor A 1, mix
Close liquid A2, mixed liquor A 3, mixed liquor A 4, mixed liquor A 5；
(4) 9.9 grams of 6- carboxyls cumarins are added in 700mL absolute ethyl alcohols under 1000r/min stirring conditions,
Stirred 3 minutes under the conditions of 1000r/min, be subsequently adding 12.3 grams of 4,5- pyridazine dicarboxylic acids, 5 parts of equivalent is divided into after shaking up, obtained
Mixed liquid B 1, mixed liquid B 2, mixed liquid B 3, mixed liquid B 4, mixed liquid B 5；
(5) 7.6 grams of 4- (2- aminoethyls) oxinanes and 8.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 1, so
After be placed in temperature to shake 30 minutes in 45 DEG C of shaking tables, obtain mixed liquor C1；
(6) mixed liquor C1 and 8.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 1, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor D1；
(7) material Q is added in mixed liquor D1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Body obtains material Q1, and material Q1 is placed 4 hours in 65 DEG C of drying box, obtains material Q2；
(8) 7.1 grams of 4- (2- aminoethyls) oxinanes and 7.8 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 2, so
After be placed in temperature to shake 30 minutes in 45 DEG C of shaking tables, obtain mixed liquor C2；
(9) mixed liquor C2 and 8.1 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 2, in 1000r/min conditions
Lower stirring 3 minutes, obtains mixed liquor D2；
(10) material Q2 is added in mixed liquor D2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material Q3, and material Q3 is placed 4 hours in 65 DEG C of drying box, obtains material Q4；
(11) 6.6 grams of 4- (2- aminoethyls) oxinanes and 7.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 3,
Temperature is subsequently placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C3 is obtained；
(12) mixed liquor C3 and 7.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 3, in 1000r/min bars
Stirred 3 minutes under part, obtain mixed liquor D3；
(13) material Q4 is added in mixed liquor D3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material Q5, and material Q5 is placed 4 hours in 65 DEG C of drying box, obtains material Q6；
(14) 6.1 grams of 4- (2- aminoethyls) oxinanes and 6.8 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 4,
Temperature is subsequently placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C4 is obtained；
(15) mixed liquor C4 and 7.1 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 4, in 1000r/min bars
Stirred 3 minutes under part, obtain mixed liquor D4；
(16) material Q6 is added in mixed liquor D4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material Q7, and material Q7 is placed 4 hours in 65 DEG C of drying box, obtains material Q8；
(17) 5.6 grams of 4- (2- aminoethyls) oxinanes and 6.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 5,
Temperature is subsequently placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C5 is obtained；
(18) mixed liquor C5 and 6.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 5, in 1000r/min bars
Stirred 3 minutes under part, obtain mixed liquor D5；
(19) material Q8 is added in mixed liquor D5, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material Q9, and material Q9 is placed 4 hours in 65 DEG C of drying box, obtains material R；
(20) by 8.33 grams of copper nitrates and 4.77 grams of ferric nitrates be added under 1000r/min stirring conditions 500mL go from
In sub- water, stirred 15 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor E1, mixed liquor E2, mix
Close liquid E3, mixed liquor E4, mixed liquor E5；
(21) by 2.19 grams lithium chlorides and 2.27 grams of cesium fluorides be added under 1000r/min stirring conditions 500mL go from
In sub- water, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtained mixed liquor F1, mixed liquor F2, mix
Close liquid F3, mixed liquor F4, mixed liquor F5；
(22) by mixed liquor E1 and 19mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F1
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G1；
(23) material R is added in mixed liquor G1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Body obtains material R1, and material R1 is placed 4 hours in 65 DEG C of drying box, obtains material R2；
(24) by mixed liquor E2 and 17mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F2
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G2；
(25) material R2 is added in mixed liquor G2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material R3, and material R3 is placed 4 hours in 65 DEG C of drying box, obtains material R4；
(26) by mixed liquor E3 and 15mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F3
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G3；
(27) material R4 is added in mixed liquor G3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material R5, and material R5 is placed 4 hours in 65 DEG C of drying box, obtains material R6；
(28) by mixed liquor E4 and 13mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F4
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G4；
(29) material R6 is added in mixed liquor G4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material R7, and material R7 is placed 4 hours in 65 DEG C of drying box, obtains material R8；
(30) by mixed liquor E5 and 11mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added to mixed liquor F5
In, stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G5；
(31) material R8 is added in mixed liquor G5, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material R9, and material R9 is placed 4 hours in 65 DEG C of drying box, obtains material S；
(32) 8.26 grams of methyl tributanoximo silanes are added to the anhydrous second of 800mL under 1000r/min stirring conditions
In alcohol, stirred 5 minutes under the conditions of 1000r/min, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixing
Liquid H3, mixed liquor H4；
(33) 5.6 grams of dichloromethyl phenylsilanes and 8.3 grams of 2- aminobenzophenones are added in mixed liquor H1,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor J1；
(34) material S is added in mixed liquor J1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Body obtains material S1, and material S1 is placed 4 hours in 65 DEG C of drying box, obtains material S2；
(35) 5.1 grams of dichloromethyl phenylsilanes and 7.8 grams of 2- aminobenzophenones are added in mixed liquor H2,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor J2；
(36) material S2 is added in mixed liquor J2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material S3, and material S3 is placed 4 hours in 65 DEG C of drying box, obtains material S4；
(37) 4.6 grams of dichloromethyl phenylsilanes and 7.3 grams of 2- aminobenzophenones are added in mixed liquor H3,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor J3；
(38) material S4 is added in mixed liquor J3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material S5, and material S5 is placed 4 hours in 65 DEG C of drying box, obtains material S6；
(39) 4.1 grams of dichloromethyl phenylsilanes and 6.8 grams of 2- aminobenzophenones are added in mixed liquor H4,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor J4；
(40) material S6 is added in mixed liquor J4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove
Liquid obtains material S7, and material S7 is placed 4 hours in 65 DEG C of drying box, and the material for obtaining is many for Adsorption
The modified pine branch adsorbent of colistin.
The beneficial effects of the invention are as follows the obtained modified pine branch adsorbent for Adsorption polymyxins has right
The features such as polymyxins adsorbs strong selection, adsorption capacity high, strong antijamming capability.
Here is being inhaled with the obtained modified pine branch adsorbent for Adsorption polymyxins of the inventive method
Adsorption test has been carried out to the waste water containing polymyxins in reaction enclosure device, the present invention has been further illustrated.
The pine branch adsorbent that is modified obtained in the inventive method is seated in absorption water reactor, to containing polymyxins
Waste water carried out adsorption test, as a result show that the adsorptive reactor for being filled with the modified pine branch adsorbent can be removed efficiently
Polymyxins in waste water, when the polymyxins concentration in waste water is 76.38mg/L, the polymyxins after treatment in water outlet is dense
Degree is reduced to 0.24mg/L.
Claims (1)
1. a kind of modified pine branch adsorbent for Adsorption polymyxins, it is characterised in that prepare the modified pine branch
Adsorbent method is comprised the following steps that：
(1) 500 grams of pine branch are placed in pulverizer and are crushed, the sieve that 4mm and 6mm are respectively with aperture is sieved, obtained
Particle diameter is the pine branch of 4~6mm；
(2) leaching in 500mL absolute ethyl alcohols is put into after the pine branch that 90 grams are obtained by step (1) is washed with 500mL deionized waters
Bubble 1 hour, removes liquid and obtains Substance P after filtering, Substance P obtains Substance P 1 after being washed through 500mL deionized waters, by Substance P 1
Put into the NaOH solution that 500mL molar concentrations are 3.7mol/L and soak 1 hour, liquid is removed after filtering and obtains Substance P 2,
Substance P 2 obtains Substance P 3 after being washed with 500mL deionized waters, Substance P 3 is obtained after being placed 12 hours in 50 DEG C of drying box
Material Q；
(3) 9.9 grams of 6- Cyanoisoquinolines are added in 700mL absolute ethyl alcohols under 1000r/min stirring conditions, in 1000r/
Under the conditions of min stir 3 minutes, be subsequently adding the 2mL concentrated sulfuric acids, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor A 1, mixed liquor A 2,
Mixed liquor A 3, mixed liquor A 4, mixed liquor A 5；
(4) 9.9 grams of 6- carboxyls cumarins are added in 700mL absolute ethyl alcohols under 1000r/min stirring conditions, in 1000r/
Stirred 3 minutes under the conditions of min, be subsequently adding 12.3 grams of 4,5- pyridazine dicarboxylic acids, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor
B1, mixed liquid B 2, mixed liquid B 3, mixed liquid B 4, mixed liquid B 5；
(5) 7.6 grams of 4- (2- aminoethyls) oxinanes and 8.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 1, are then put
Shaken 30 minutes in temperature is 45 DEG C of shaking tables, obtain mixed liquor C1；
(6) mixed liquor C1 and 8.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 1, are stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor D1；
(7) material Q is added in mixed liquor D1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid and obtain
To material Q1, material Q1 is placed 4 hours in 65 DEG C of drying box, obtain material Q2；
(8) 7.1 grams of 4- (2- aminoethyls) oxinanes and 7.8 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 2, are then put
Shaken 30 minutes in temperature is 45 DEG C of shaking tables, obtain mixed liquor C2；
(9) mixed liquor C2 and 8.1 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 2, are stirred under the conditions of 1000r/min
Mix 3 minutes, obtain mixed liquor D2；
(10) material Q2 is added in mixed liquor D2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material Q3 is obtained, material Q3 is placed 4 hours in 65 DEG C of drying box, obtain material Q4；
(11) 6.6 grams of 4- (2- aminoethyls) oxinanes and 7.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 3, then
Temperature is placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C3 is obtained；
(12) mixed liquor C3 and 7.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 3, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor D3；
(13) material Q4 is added in mixed liquor D3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material Q5 is obtained, material Q5 is placed 4 hours in 65 DEG C of drying box, obtain material Q6；
(14) 6.1 grams of 4- (2- aminoethyls) oxinanes and 6.8 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 4, then
Temperature is placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C4 is obtained；
(15) mixed liquor C4 and 7.1 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 4, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor D4；
(16) material Q6 is added in mixed liquor D4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material Q7 is obtained, material Q7 is placed 4 hours in 65 DEG C of drying box, obtain material Q8；
(17) 5.6 grams of 4- (2- aminoethyls) oxinanes and 6.3 grams of fluoro- 3- iodine pyridines of 2- are added in mixed liquor A 5, then
Temperature is placed in be shaken 30 minutes in 45 DEG C of shaking tables, mixed liquor C5 is obtained；
(18) mixed liquor C5 and 6.6 grams of bromo- 4- methylisoquinoliniums of 5- are added in mixed liquid B 5, under the conditions of 1000r/min
Stirring 3 minutes, obtains mixed liquor D5；
(19) material Q8 is added in mixed liquor D5, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material Q9 is obtained, material Q9 is placed 4 hours in 65 DEG C of drying box, obtain material R；
(20) 8.33 grams of copper nitrates and 4.77 grams of ferric nitrates are added to 500mL deionized waters under 1000r/min stirring conditions
In, stirred 15 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor E1, mixed liquor E2, mixed liquor
E3, mixed liquor E4, mixed liquor E5；
(21) 2.19 grams lithium chlorides and 2.27 grams of cesium fluorides are added to 500mL deionized waters under 1000r/min stirring conditions
In, stirred 3 minutes under the conditions of 1000r/min, 5 parts of equivalent is divided into after shaking up, obtain mixed liquor F1, mixed liquor F2, mixed liquor
F3, mixed liquor F4, mixed liquor F5；
(22) by mixed liquor E1 and 19mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added in mixed liquor F1,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G1；
(23) material R is added in mixed liquor G1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid and obtain
To material R1, material R1 is placed 4 hours in 65 DEG C of drying box, obtain material R2；
(24) by mixed liquor E2 and 17mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added in mixed liquor F2,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G2；
(25) material R2 is added in mixed liquor G2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material R3 is obtained, material R3 is placed 4 hours in 65 DEG C of drying box, obtain material R4；
(26) by mixed liquor E3 and 15mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added in mixed liquor F3,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G3；
(27) material R4 is added in mixed liquor G3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material R5 is obtained, material R5 is placed 4 hours in 65 DEG C of drying box, obtain material R6；
(28) by mixed liquor E4 and 13mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added in mixed liquor F4,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G4；
(29) material R6 is added in mixed liquor G4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material R7 is obtained, material R7 is placed 4 hours in 65 DEG C of drying box, obtain material R8；
(30) by mixed liquor E5 and 11mL molar concentration for the Ammoniun Heptamolybdate Solution of 0.75mol/L is added in mixed liquor F5,
Stirred 3 minutes under the conditions of 1000r/min, obtain mixed liquor G5；
(31) material R8 is added in mixed liquor G5, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material R9 is obtained, material R9 is placed 4 hours in 65 DEG C of drying box, obtain material S；
(32) 8.26 grams of methyl tributanoximo silanes are added in 800mL absolute ethyl alcohols under 1000r/min stirring conditions,
Under the conditions of 1000r/min stir 5 minutes, 4 parts of equivalent is divided into after shaking up, obtain mixed liquor H1, mixed liquor H2, mixed liquor H3,
Mixed liquor H4；
(33) 5.6 grams of dichloromethyl phenylsilanes and 8.3 grams of 2- aminobenzophenones are added in mixed liquor H1, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor J1；
(34) material S is added in mixed liquor J1, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid and obtain
To material S1, material S1 is placed 4 hours in 65 DEG C of drying box, obtain material S2；
(35) 5.1 grams of dichloromethyl phenylsilanes and 7.8 grams of 2- aminobenzophenones are added in mixed liquor H2, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor J2；
(36) material S2 is added in mixed liquor J2, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material S3 is obtained, material S3 is placed 4 hours in 65 DEG C of drying box, obtain material S4；
(37) 4.6 grams of dichloromethyl phenylsilanes and 7.3 grams of 2- aminobenzophenones are added in mixed liquor H3, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor J3；
(38) material S4 is added in mixed liquor J3, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material S5 is obtained, material S5 is placed 4 hours in 65 DEG C of drying box, obtain material S6；
(39) 4.1 grams of dichloromethyl phenylsilanes and 6.8 grams of 2- aminobenzophenones are added in mixed liquor H4, in 1000r/
Stirred 3 minutes under the conditions of min, obtain mixed liquor J4；
(40) material S6 is added in mixed liquor J4, is shaken 25 minutes in the shaking table that temperature is 65 DEG C, be filtered to remove liquid
Material S7 is obtained, material S7 is placed 4 hours in 65 DEG C of drying box, the material for obtaining is for many Acarasiales of Adsorption
The modified pine branch adsorbent of element.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108126656A (en) * | 2017-12-25 | 2018-06-08 | 北京益清源环保科技有限公司 | For the modified activated carbon absorbent of benzene in Adsorption wastewater from chemical industry |
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| CN103111265A (en) * | 2013-02-27 | 2013-05-22 | 南京工业大学 | Preparation method of adsorbent for removing antibiotics in water, prepared adsorbent and application thereof |
| 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 |
| CN106423108A (en) * | 2016-09-24 | 2017-02-22 | 北京益净环保设备科技有限公司 | Granular adsorbent for adsorbing thiophene and preparation method thereof |
| CN106423092A (en) * | 2016-09-24 | 2017-02-22 | 北京益净环保设备科技有限公司 | Function board for adsorbing nitrobenzene and preparation method thereof |
| CN106629978A (en) * | 2016-12-30 | 2017-05-10 | 北京师范大学 | Adsorption and regeneration integrated reactor system for radioactive wastewater treatment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103111265A (en) * | 2013-02-27 | 2013-05-22 | 南京工业大学 | Preparation method of adsorbent for removing antibiotics in water, prepared adsorbent and application thereof |
| 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 |
| CN106423108A (en) * | 2016-09-24 | 2017-02-22 | 北京益净环保设备科技有限公司 | Granular adsorbent for adsorbing thiophene and preparation method thereof |
| CN106423092A (en) * | 2016-09-24 | 2017-02-22 | 北京益净环保设备科技有限公司 | Function board for adsorbing nitrobenzene and preparation method thereof |
| CN106629978A (en) * | 2016-12-30 | 2017-05-10 | 北京师范大学 | Adsorption and regeneration integrated reactor system for radioactive wastewater treatment |
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| CN108126656A (en) * | 2017-12-25 | 2018-06-08 | 北京益清源环保科技有限公司 | For the modified activated carbon absorbent of benzene in Adsorption wastewater from chemical industry |
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