CN105399875A - Preparation method for magnetization hydrophilic modification polystyrene porous adsorption resin - Google Patents
Preparation method for magnetization hydrophilic modification polystyrene porous adsorption resin Download PDFInfo
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- CN105399875A CN105399875A CN201510949671.7A CN201510949671A CN105399875A CN 105399875 A CN105399875 A CN 105399875A CN 201510949671 A CN201510949671 A CN 201510949671A CN 105399875 A CN105399875 A CN 105399875A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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Abstract
A disclosed preparation method for magnetization hydrophilic modification polystyrene porous adsorption resin comprises the following steps: (1) hydrophilic modification; (2) activation reaction; and (3) in-situ polymerization. The preparation method for magnetization hydrophilic modification polystyrene porous adsorption resin is simple in operation and easy to realize. On the basis of scientific formula design, through reasonable technology design, hydrophilic modification and magnetization modification are successively performed on polystyrene-serial porous resin, one the one hand, the solubility of modified resin in wastewater is improved and prerequisite conditions are provided for filtering adsorption, and on the other hand, a magnetic chelating group is formed on the resin surface through surface polymerization, the adsorption filtering effect of the resin on heavy metal ions is improved, and especially, the resin possesses relatively excellent adsorption performance on lead ion. The prepared modified resin possesses great application prospect in the field of heavy-metal-polluted wastewater.
Description
Technical field
The present invention relates to functional resin field, particularly relate to a kind of preparation method of magnetizing hydrophilic modifying polystyrene porous polymeric adsorbent.
Background technology
Along with the fast development of various factory, fuel-burning power plant, burning field, disposal site and smelting enterprise etc., create the waste water of a large amount of metal ion, if be directly discharged in water body, serious pollution can be produced to environment, great harm is all caused to the natural eubiosis and the healthy of the mankind.Have the precipitator method, ion exchange method, membrane separation process and absorption method etc. to the minimizing technology of metal ion, the features such as wherein absorption method has simple to operate, effective and rapid are the most frequently used and the most promising water technologies.
Polystyrene series porous resin is the common used material of waste water adsorption treatment, but its wetting ability is poor, and the plumbous absorption property deficiency in heavy metal ion, be difficult to the lead ion effectively removed in water body, realize the purification that water body is real.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of preparation method of magnetizing hydrophilic modifying polystyrene porous polymeric adsorbent, can solve existing polystyrene series porous resin in process heavy metal wastewater thereby above shortcomings part.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide a kind of preparation method of magnetizing hydrophilic modifying polystyrene porous polymeric adsorbent, comprise the steps:
(1) hydrophilic modifying: by molfraction, the quadrol getting 3 ~ 30 parts is added drop-wise in the swelling polystyrene porous resin matrix of 1 ~ 3 part of organic solvent, stirs at a certain temperature and makes it reaction;
(2) priming reaction: under room temperature condition, a certain amount of activator is added in resin solution in step (1) after hydrophilic modifying, 0 ~ 5 DEG C is down to after mix and blend, and drip a certain amount of acid binding agent aqueous solution, constant temperature stirs 30 ~ 40min, adjusted to ph, continues constant temperature stirring reaction 60 ~ 90min, filtration, washing, vacuum-drying, obtain the resin after activating;
(3) in-situ polymerization: the activated resin obtained in step (2) is joined in the ethanol-water solution of iron trichloride and ferrous sulfate, react in the basic conditions after swelling to solution and become black, then temperature reaction for some time, be cooled to room temperature after reaction terminates, obtain described magnetization hydrophilic modifying polystyrene porous polymeric adsorbent by after product filtration, washing, vacuum-drying.
In a preferred embodiment of the present invention, in described step (1), described reaction conditions is: temperature 80 ~ 100 DEG C, time 3 ~ 5h.
In a preferred embodiment of the present invention, in described step (2), described activator is cyanuric chloride, and its add-on is 5 ~ 15 molfractions; The sodium carbonate solution of the described acid binding agent aqueous solution to be volumetric molar concentration be 0.3 ~ 0.5mol/L, its add-on is the sodium carbonate containing 1 ~ 3 molfraction, and it adds speed is 3 ~ 5/s.
In a preferred embodiment of the present invention, in described step (2), the control method of described pH value is: first adjust ph is 4.5 ~ 5, then increases to 9.5 with the speed of 0.5/min.
In a preferred embodiment of the present invention, in described step (3), the volumetric molar concentration of described liquor ferri trichloridi is 0.5 ~ 0.8mol/L, and its add-on is the iron trichloride containing 10 ~ 20 molfractions; The volumetric molar concentration of described copperas solution is 0.3 ~ 0.5mol/L, and its add-on is the ferrous sulfate containing 20 ~ 30 molfractions.
In a preferred embodiment of the present invention, in described step (3), described reaction conditions is: temperature 70 ~ 90 DEG C, time 1 ~ 3h.
The invention has the beneficial effects as follows: a kind of preparation method of magnetizing hydrophilic modifying polystyrene porous polymeric adsorbent of the present invention, easy and simple to handle, easily realize; It is on the basis of the formulating of recipe of science, and by rational technological design, successively p-poly-phenyl ethene system porous resin carries out hydrophilic modifying and magnetization modification, improves the solubleness of modified resin in waste water, for Filtration Adsorption provides precondition on the one hand; On the other hand, formed the chelation group with magnetic behavior at resin surface by surface aggregate, improve the adsorption filtration effect of its heavy metal ion, especially lead ion has preferably absorption property; Prepared modified resin has huge application prospect in heavy metal polluted waste water field.
Embodiment
Below preferred embodiment of the present invention is described in detail, can be easier to make advantages and features of the invention be readily appreciated by one skilled in the art, thus more explicit defining is made to protection scope of the present invention.
The embodiment of the present invention comprises:
Embodiment 1
Magnetize a preparation method for hydrophilic modifying polystyrene porous polymeric adsorbent, comprise the steps:
(1) hydrophilic modifying: in stink cupboard, get 1 part (by molfraction, flask put into by Chloromethyl polystyrene base resin down together), the tetrahydrofuran (THF) of Chloromethyl polystyrene base resin 30 parts of volumes is incorporated as again in flask, cover glass cover, make the fully swelling 6 ~ 12h of Chloromethyl polystyrene base resin; Then the quadrol getting 3 parts drips in above-mentioned swelling Chloromethyl polystyrene base resin matrix, and stirring reaction 5h at 80 DEG C, realizes the hydrophilic modifying to Chloromethyl polystyrene base resin;
(2) priming reaction: under room temperature condition, the cyanuric chloride of 5 parts is added in resin solution in step (1) after hydrophilic modifying, mix and blend makes it to dissolve, then mixed solution is down to 0 ~ 5 DEG C, and drip with the speed of 3 ~ 5/s the sodium carbonate solution that appropriate volumetric molar concentration is 0.3mol/L, the add-on of sodium carbonate is made to be 1 part, drip and finish, constant temperature stirs 30 ~ 40min, be first 4.5 by the pH value of the hydrochloric acid soln of 0.3mol/L adjustment mixing solutions, then the sodium hydroxide solution of 0.2mol/L is dripped, the pH value of mixing solutions is made to increase to 9.5 with the speed of 0.5/min, continue constant temperature stirring reaction 60min subsequently, after reaction terminates, filter, first useful clear water and ethanol respectively wash 3 ~ 5 times, at 0.3 ~ 0.5MPa, dry 30 ~ 60min under the vacuum condition of 60 ~ 80 DEG C, obtain the modified resin after activating,
(3) in-situ polymerization: be that the ethanol of 2:1 and deionized water prepare liquor ferri trichloridi that volumetric molar concentration is 0.5mol/L respectively and volumetric molar concentration is the copperas solution of 0.3mol/L by volume ratio, the activated resin obtained in step (2) is joined in the aqueous ethanolic solution containing the iron trichloride of 10 parts of iron trichlorides, leave standstill swelling 2 ~ 3h, then inert nitrogen gas is passed into, add in the aqueous ethanolic solution of the ferrous sulfate of above-mentioned preparation again, the add-on of ferrous sulfate is made to be 20 parts, be uniformly mixed, sodium hydroxide solution to the mixing solutions dripping 0.2mol/L is again black, drip and finish, mixing solutions is warming up to 70 DEG C, isothermal reaction 3h, room temperature is cooled to after reaction terminates, filtrate is washed with distilled water to for neutral after being filtered by product, use absolute ethanol washing again 2 ~ 3 times, at 0.3 ~ 0.5MPa, dry 30 ~ 60min under the vacuum condition of 60 ~ 80 DEG C, obtain described magnetization hydrophilic modifying polystyrene porous polymeric adsorbent.
Embodiment 2
Magnetize a preparation method for hydrophilic modifying polystyrene porous polymeric adsorbent, comprise the steps:
(1) hydrophilic modifying: in stink cupboard, get 3 parts (by molfraction, down together) flask put into by Chloromethyl polystyrene base resin, the tetrahydrofuran (THF) of Chloromethyl polystyrene base resin 100 parts of volumes is incorporated as again in flask, cover glass cover, make the fully swelling 6 ~ 12h of Chloromethyl polystyrene base resin; Then the quadrol getting 30 parts drips in above-mentioned swelling Chloromethyl polystyrene base resin matrix, and stirring reaction 3h at 100 DEG C, realizes the hydrophilic modifying to Chloromethyl polystyrene base resin;
(2) priming reaction: under room temperature condition, the cyanuric chloride of 15 parts is added in resin solution in step (1) after hydrophilic modifying, mix and blend makes it to dissolve, then mixed solution is down to 0 ~ 5 DEG C, and drip with the speed of 3 ~ 5/s the sodium carbonate solution that appropriate volumetric molar concentration is 0.5mol/L, the add-on of sodium carbonate is made to be 3 parts, drip and finish, constant temperature stirs 30 ~ 40min, be first 5 by the pH value of the hydrochloric acid soln of 0.3mol/L adjustment mixing solutions, then the sodium hydroxide solution of 0.2mol/L is dripped, the pH value of mixing solutions is made to increase to 9.5 with the speed of 0.5/min, continue constant temperature stirring reaction 60 ~ 90min subsequently, after reaction terminates, filter, first useful clear water and ethanol respectively wash 3 ~ 5 times, at 0.3 ~ 0.5MPa, dry 30 ~ 60min under the vacuum condition of 60 ~ 80 DEG C, obtain the modified resin after activating,
(3) in-situ polymerization: be that the ethanol of 3:1 and deionized water prepare liquor ferri trichloridi that volumetric molar concentration is 0.8mol/L respectively and volumetric molar concentration is the copperas solution of 0.5mol/L by volume ratio, the activated resin obtained in step (2) is joined in the aqueous ethanolic solution containing the iron trichloride of 20 parts of iron trichlorides, leave standstill swelling 2 ~ 3h, then inert nitrogen gas is passed into, add in the aqueous ethanolic solution of the ferrous sulfate of above-mentioned preparation again, the add-on of ferrous sulfate is made to be 30 parts, be uniformly mixed, sodium hydroxide solution to the mixing solutions dripping 0.2mol/L is again black, drip and finish, mixing solutions is warming up to 90 DEG C, isothermal reaction 13h, room temperature is cooled to after reaction terminates, filtrate is washed with distilled water to for neutral after being filtered by product, use absolute ethanol washing again 2 ~ 3 times, at 0.3 ~ 0.5MPa, dry 30 ~ 60min under the vacuum condition of 60 ~ 80 DEG C, obtain described magnetization hydrophilic modifying polystyrene porous polymeric adsorbent.
Magnetization hydrophilic modifying polystyrene porous polymeric adsorbent prepared by aforesaid method, its specific saturation magnetization (Ms) is 0.97 ~ 1.02Am
2/ kg, it is 356 ~ 380mg/g to the maximal absorptive capacity of lead ion; Be 300 ~ 330mg/g to the maximal absorptive capacity of other heavy metal ion.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (6)
1. magnetize a preparation method for hydrophilic modifying polystyrene porous polymeric adsorbent, it is characterized in that, comprise the steps:
(1) hydrophilic modifying: by molfraction, the quadrol getting 3 ~ 30 parts is added drop-wise in the swelling polystyrene porous resin matrix of 1 ~ 3 part of organic solvent, stirs at a certain temperature and makes it reaction;
(2) priming reaction: under room temperature condition, a certain amount of activator is added in resin solution in step (1) after hydrophilic modifying, 0 ~ 5 DEG C is down to after mix and blend, and drip a certain amount of acid binding agent aqueous solution, constant temperature stirs 30 ~ 40min, adjusted to ph, continues constant temperature stirring reaction 60 ~ 90min, filtration, washing, vacuum-drying, obtain the resin after activating;
(3) in-situ polymerization: the activated resin obtained in step (2) is joined in the ethanol-water solution of iron trichloride and ferrous sulfate, react in the basic conditions after swelling to solution and become black, then temperature reaction for some time, be cooled to room temperature after reaction terminates, obtain described magnetization hydrophilic modifying polystyrene porous polymeric adsorbent by after product filtration, washing, vacuum-drying.
2. the preparation method of magnetization hydrophilic modifying polystyrene porous polymeric adsorbent according to claim 1, it is characterized in that, in described step (1), described reaction conditions is: temperature 80 ~ 100 DEG C, time 3 ~ 5h.
3. the preparation method of magnetization hydrophilic modifying polystyrene porous polymeric adsorbent according to claim 1, is characterized in that, in described step (2), described activator is cyanuric chloride, and its add-on is 5 ~ 15 molfractions; The sodium carbonate solution of the described acid binding agent aqueous solution to be volumetric molar concentration be 0.3 ~ 0.5mol/L, its add-on is the sodium carbonate containing 1 ~ 3 molfraction, and it adds speed is 3 ~ 5/s.
4. the preparation method of magnetization hydrophilic modifying polystyrene porous polymeric adsorbent according to claim 1, it is characterized in that, in described step (2), the control method of described pH value is: first adjust ph is 4.5 ~ 5, then increases to 9.5 with the speed of 0.5/min.
5. the preparation method of magnetization hydrophilic modifying polystyrene porous polymeric adsorbent according to claim 1, it is characterized in that, in described step (3), the volumetric molar concentration of described liquor ferri trichloridi is 0.5 ~ 0.8mol/L, and its add-on is the iron trichloride containing 10 ~ 20 molfractions; The volumetric molar concentration of described copperas solution is 0.3 ~ 0.5mol/L, and its add-on is the ferrous sulfate containing 20 ~ 30 molfractions.
6. the preparation method of magnetization hydrophilic modifying polystyrene porous polymeric adsorbent according to claim 1, it is characterized in that, in described step (3), described reaction conditions is: temperature 70 ~ 90 DEG C, time 1 ~ 3h.
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Cited By (3)
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CN107694612A (en) * | 2017-09-05 | 2018-02-16 | 华南理工大学 | It is a kind of to remove material of bromate and its precursor and its preparation method and application in water removal |
CN110407280A (en) * | 2019-04-09 | 2019-11-05 | 临沂大学 | A kind of process using environment steroids organic substance in MAR removal drinking water |
CN110975411A (en) * | 2019-12-20 | 2020-04-10 | 中核二七二铀业有限责任公司 | Pretreatment filtering equipment for extraction stock solution |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110407280A (en) * | 2019-04-09 | 2019-11-05 | 临沂大学 | A kind of process using environment steroids organic substance in MAR removal drinking water |
CN110407280B (en) * | 2019-04-09 | 2021-09-17 | 临沂大学 | Process method for removing environmental hormone organic substances in drinking water by using MAR |
CN110975411A (en) * | 2019-12-20 | 2020-04-10 | 中核二七二铀业有限责任公司 | Pretreatment filtering equipment for extraction stock solution |
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