CN103933954A - Preparation method of magnetic polypyrrole and method of adsorbing nitrate in water - Google Patents

Preparation method of magnetic polypyrrole and method of adsorbing nitrate in water Download PDF

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CN103933954A
CN103933954A CN201410168195.0A CN201410168195A CN103933954A CN 103933954 A CN103933954 A CN 103933954A CN 201410168195 A CN201410168195 A CN 201410168195A CN 103933954 A CN103933954 A CN 103933954A
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water
polypyrrole
magnetic polypyrrole
magnetic
concentration
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王家宏
田昊
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a preparation method of magnetic polypyrrole. The preparation method comprises the following steps: dissolving FeCl2.4H2O and FeCl3.6H2O in HCl liquor, under protection of N2, dropwise adding into NaOH liquor for stirring and co-precipitating, and then washing by deionized water until the liquor is neutral, drying in vacuum and grinding to obtain Fe3O4 nano particles; adding the Fe3O4 nano particles into deionized water, carrying out ultrasonic treatment in the presence of N2, mechanically stirring after adding FeCl3, mechanically stirring again after adding pyrrole, adding acetone to terminate the reaction after the reaction is ended, and washing reactants by deionized water and acetone for a plurality of times; and finally, drying in vacuum and grinding to obtain magnetic polypyrrole. The invention further discloses a method of adsorbing nitrate in water by magnetic polypyrrole, wherein magnetic polypyrrole is added into water for adsorbing nitrate ions in water, and a magnet is separated after adsorption saturation. According to the invention, an in-situ chemical oxidization method is utilized to synthesize a magnetic polypyrrole adsorbent, the synthetic method is simple, a removing effect is remarkable, and the adsorbent can be regenerated and recycled.

Description

The method of nitrate anion in the preparation of magnetic polypyrrole and adsorbed water
Technical field
The invention belongs to water body purification technical field, be specifically related to a kind of preparation method of magnetic polypyrrole, the invention still further relates to the method for utilizing nitrate anion in this magnetic polypyrrole adsorbed water.
Background technology
Drinking water safety and residents ' health are the subject matter receiving much concern, and are just day by day subject to people and pay close attention to widely, and azotate pollution all causes serious impact to people's life and ecological environment, therefore, effectively controls and remove the NO in water 3 -that the important topic that is related to environment and the mankind seeks that cost is lower, the good nitrate removal method for the treatment of effect is very necessary.
At present, removing the nitrate in local underground water, is mainly to solve by engineering measure, as added people's iron powder, activated carbon, microorganism etc. in contaminated water, makes nitric acid be degraded to the gas of colorless and odorless.In engineering measure, there are in recent years some new methods, they than before conventional method, as mixing method, conventional ion exchange process, embrane method etc. have many advantages, and be verified by experiment.
Absorption method has the advantages such as successful, technological process are simple, economical and practical, is particularly suitable for low concentration containing NO 3 -the processing of water.The more sorbing material of research in recent years comprises cheap natural minerals, agriculture and industry waste, rare earth material, chelating resin, corn straw modification etc.These adsorbents have good removal effect to the nitrate anion in water, but this adsorbent exists and is difficult to and processes the shortcoming that separates of water body.
Summary of the invention
The object of this invention is to provide a kind of preparation method of magnetic polypyrrole, its stable chemical nature, renewable, recycle.
Another object of the present invention is to provide the method for nitrate anion in a kind of magnetic polypyrrole adsorbed water of utilizing above-mentioned preparation.
The technical solution adopted in the present invention is, the preparation method of magnetic polypyrrole specifically implements according to following steps:
Step 1, by FeCl 24H 2o and FeCl 36H 2o is dissolved in the HCl solution that 50ml, concentration are 0.5moi/L, at N 2under protection, in the NaOH solution that to be added drop-wise to 450ml, concentration be 1.0～2.0mol/L, then at 75～85 DEG C, stir after co-precipitation 30～40min with deionized water washing to neutral, finally, in 45～55 DEG C of vacuum drying 10～12h, grinding, obtain Fe 3o 4nano particle;
Step 2, the Fe that step 1 is prepared 3o 4nano particle joins in deionized water, N 2the lower ultrasonic 10～15min of protection, then add FeCl 3rear mechanical agitation 30～40min, and then continue mechanical agitation reaction 3～3.5h after adding pyrroles (Ppy), after reaction finishes, add 10ml acetone cessation reaction, deionized water and acetone washing several for the reactant obtaining, finally vacuum drying 5～6h at 100～110 DEG C, grinds, and obtains magnetic polypyrrole (Fe 3o 4/ Ppy).
Feature of the present invention is also,
In step 1, FeCl 24H 2o and FeCl 36H 2fe in O 2+with Fe 3+mol ratio be 1:1.5～2.5, Fe 2+concentration be 0.035mol/L.
In step 2, Fe 3o 4mass concentration be 5g/L, Fe 3o 4with pyrroles's mass volume ratio be 2:3～5g/ml, FeCl 3concentration be 0.28mol/L.
Another technical scheme of the present invention is, utilize the method for nitrate anion in above-mentioned magnetic polypyrrole adsorbed water, in the water body purifying in wish, add the magnetic polypyrrole of 0.0004 times of its quality, nitrate ion in adsorbed water under the condition that 25 DEG C, pH are 2.0～9.0, adsorb saturated after, magnet separates, the water being purified.
Feature of the present invention is also,
In the water body that wish purifies, the concentration of nitrate ion is 30～80mg/L.
Adsorption time is 1min～120min.
The invention has the beneficial effects as follows,
1. the preparation method of magnetic polypyrrole of the present invention, utilize in situ chemical oxidation method, by controlling the ratio of monomer and tri-iron tetroxide, pyrrole monomer is aggregated on ferriferrous oxide nano-particle to synthetic a kind of novel magnetic polypyrrole adsorbent, the characteristic of both having utilized Fe 3 O 4 magnetic to separate, there is again the ability of polypyrrole absorption nitrate anion, be the good adsorbent of a kind of application prospect, and synthetic method is simple, with low cost.
2. the present invention utilizes the method for nitrate anion in magnetic polypyrrole adsorbed water, utilizes the existence that has the nitrogen-atoms of positively charged group in polypyrrole molecule, and the anion such as nitrate anion are had to good adsorption capacity, and Fe 3o 4/ Ppy adsorbent stable chemical nature, not affected by external environment factor, adsorb after saturated and can well it be separated with water after treatment with magnet, and can be recycled after Low Concentration NaCl Solution regeneration, and simple to operate, removal effect is remarkable, has good economy and environment benefit.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
The preparation method of magnetic polypyrrole of the present invention, specifically implements according to following steps:
Step 1, by FeCl 24H 2o and FeCl 36H 2o is dissolved in the HCl solution that 50ml, concentration are 0.5moi/L, at N 2under protection, in the NaOH solution that to be added drop-wise to 450ml, concentration be 1.0～2.0mol/L, then at 75～85 DEG C, stir after co-precipitation 30～40min with deionized water washing to neutral, finally, in 45～55 DEG C of vacuum drying 10～12h, grinding, obtain Fe 3o 4nano particle;
Wherein, FeCl 24H 2o and FeCl 36H 2fe in O 2+with Fe 3+mol ratio be 1:1.5～2.5, Fe 2+concentration be 0.035mol/L;
Step 2, the Fe that step 1 is prepared 3o 4nano particle joins in deionized water, N 2the lower ultrasonic 10～15min of protection, then add FeCl 3rear mechanical agitation 30～40min, and then continue mechanical agitation reaction 3～3.5h after adding pyrroles (Ppy), after reaction finishes, add 10ml acetone cessation reaction, deionized water and acetone washing several for the reactant obtaining, finally vacuum drying 5～6h at 100～110 DEG C, grinds, and obtains magnetic polypyrrole (Fe 3o 4/ Ppy).
Fe 3o 4mass concentration be 5g/L, Fe 3o 4with pyrroles's mass volume ratio be 2:3～5g/ml, FeCl 3concentration be 0.28mol/L.
The preparation method of magnetic polypyrrole of the present invention, utilize in situ chemical oxidation method, by controlling the ratio of monomer and tri-iron tetroxide, pyrrole monomer is aggregated on ferriferrous oxide nano-particle to synthetic a kind of novel magnetic polypyrrole adsorbent, the characteristic of both having utilized Fe 3 O 4 magnetic to separate, there is again the ability of polypyrrole absorption nitrate anion, be the good adsorbent of a kind of application prospect, and synthetic method is simple, with low cost.
In the wish purifying water body that is 30～80mg/L in the concentration of nitrate ion, add the magnetic polypyrrole of 0.0004 times of its quality, nitrate ion in adsorbed water under the condition that 25 DEG C, pH are 2.0～9.0, adsorption time is 1min～120min, adsorb saturated after, magnet separates, the water being purified.
The present invention utilizes the method for nitrate anion in magnetic polypyrrole adsorbed water, utilizes the existence that has the nitrogen-atoms of positively charged group in polypyrrole molecule, and the anion such as nitrate anion are had to good adsorption capacity, and Fe 3o 4/ Ppy adsorbent stable chemical nature, not affected by external environment factor, adsorb after saturated and can well it be separated with water after treatment with magnet, and can be recycled after Low Concentration NaCl Solution regeneration, and simple to operate, removal effect is remarkable, has good economy and environment benefit.
The mechanism of magnetic polypyrrole absorption nitrate ion has two aspects: on the one hand, in polypyrrole molecule, there is nitrogen-atoms group, and positively charged, and nitrate anion is electronegative, thus polypyrrole has very strong suction-operated to nitrate anion; On the other hand, because polymer can carry electric charge in chemical polymerization or electrochemical polymerization process, in order to keep charge balance and electroneutral, the corresponding ion of polymer combination from solution, the counterion of this oppositely charged is commonly referred to adulterant, due to the existence of doping ion, can be in order to the ion in adsorbent solution by ion-exchange, the present invention selects FeCl 3as oxidant and the adulterant of pyrroles's polymerization, Fe 3o 4the Cl-adulterating in/Ppy adsorbent, completes NO 3 -anion exchange absorbing.
Embodiment 1
Magnetic polypyrrole (Fe 3o 4/ Ppy) synthetic
Step 1, takes respectively 3.44g FeCl 24H 2o and 9.44gFeCl 36H 2o, adds the HCl solution of 50ml, 0.5mol/L to dissolve, at N 2under protection, be added dropwise in 450ml, 1.5mol/L NaOH solution, wash neutrality at 80 DEG C after mechanical agitation co-precipitation 30min by deionized water, finally vacuum drying 12h, grinding at 50 DEG C, obtains Fe 3o 4nano particle;
Step 2, takes the Fe that 0.4g step 1 obtains 3o 4nano particle, adds in 80ml deionized water N 2the lower ultrasonic 10min of protection, then add 6g FeCl 3rear mechanical agitation 30min, and then add 0.8ml pyrroles to continue mechanical agitation reaction 3h, after reaction finishes, add 10ml acetone cessation reaction, deionized water and acetone washing several for the reactant obtaining, vacuum drying 6h at 100 DEG C, grinds, and obtains Fe 3o 4/ Ppy.
Embodiment 2
Magnetic polypyrrole (Fe 3o 4/ Ppy) synthetic
Step 1, takes respectively 3.44g FeCl 24H 2o and 6.89gFeCl 36H 2o, adds the HCl solution of 50ml, 0.5mol/L to dissolve, at N 2under protection, be added dropwise in 450ml, 1.0mol/L NaOH solution, wash neutrality at 85 DEG C after mechanical agitation co-precipitation 35min by deionized water, finally vacuum drying 11h, grinding at 45 DEG C, obtains Fe 3o 4nano particle;
Step 2, takes the Fe that 0.4g step 1 obtains 3o 4nano particle, adds in 80ml deionized water N 2the lower ultrasonic 15min of protection, then add 6g FeCl 3rear mechanical agitation 35min, and then add 0.6ml pyrroles to continue mechanical agitation reaction 3.2h, after reaction finishes, add 10ml acetone cessation reaction, deionized water and acetone washing several for the reactant obtaining, vacuum drying 5.5h at 110 DEG C, grinds, and obtains Fe 3o 4/ Ppy.
Embodiment 3
Magnetic polypyrrole (Fe 3o 4/ Ppy) synthetic
Step 1, takes respectively 3.44g FeCl 24H 2o and 11.49gFeCl 36H 2o, adds the HCl solution of 50ml, 0.5mol/L to dissolve, at N 2under protection, be added dropwise in 450ml, 2.0mol/L NaOH solution, wash neutrality at 75 DEG C after mechanical agitation co-precipitation 40min by deionized water, finally vacuum drying 10h, grinding at 55 DEG C, obtains Fe 3o 4nano particle;
Step 2, takes the Fe that 0.4g step 1 obtains 3o 4nano particle, adds in 80ml deionized water N 2the lower ultrasonic 12min of protection, then add 6g FeCl 3rear mechanical agitation 40min, and then add 1.0ml pyrroles to continue mechanical agitation reaction 3.5h, after reaction finishes, add 10ml acetone cessation reaction, deionized water and acetone washing several for the reactant obtaining, vacuum drying 5h at 105 DEG C, grinds, and obtains Fe 3o 4/ Ppy.
With the Fe of preparation in embodiment 1 3o 4/ Ppy is adsorbent, to containing NO 3 -water carry out adsorption test.
Embodiment 4
In the wish purifying water body that is 80mg/L in the concentration of nitrate ion, add the magnetic polypyrrole of 0.0004 times of its quality, nitrate ion in adsorbed water under the condition that 25 DEG C, pH are 4.0, adsorption time is 120min, adsorb saturated after, magnet separates, and records NO 3 -ion saturated extent of adsorption is 46.97mg/g.
Embodiment 5
With embodiment 4, NO 3 -ion initial concentration is 50mg/L, and other conditions are constant, the NO recording 3 -ion saturated extent of adsorption is 37.79mg/g.
Embodiment 6
With embodiment 4, NO 3 -ion initial concentration is 30mg/g, and other conditions are constant, the NO recording 3 -ion saturated extent of adsorption is 29.62mg/g.
From embodiment 4～6, within the scope of finite concentration, Fe 3o 4/ Ppy adsorbent is to NO 3 -the adsorbance of ion is along with NO in water body 3 -the rising of ion concentration and increasing.
Embodiment 7
In the wish purifying water body that is 50mg/L in the concentration of nitrate ion, add the magnetic polypyrrole of 0.0004 times of its quality, nitrate ion in adsorbed water under the condition that 25 DEG C, pH are 2.0, adsorption time is 120min, adsorb saturated after, magnet separates, the NO recording 3 -ion saturated extent of adsorption is 23.13mg/g.
Embodiment 8
With embodiment 7, water body pH=3, other conditions are constant, the NO recording 3 -ion saturated extent of adsorption is 32.23mg/g.
Embodiment 9
With embodiment 7, water body pH=4, other conditions are constant, the NO recording 3 -ion saturated extent of adsorption is 37.57mg/g.
Embodiment 10
With embodiment 7, water body pH=5, other conditions are constant, the NO recording 3 -ion saturated extent of adsorption is 31.34mg/g.
Embodiment 11
With embodiment 7, water body pH=9, other conditions are constant, the NO recording 3 -ion saturated extent of adsorption is 6.30mg/g.
From embodiment 7～11, slant acidity condition is more conducive to Fe 3o 4/ Ppy is to NO 3 -the absorption of ion, and have maximal absorptive capacity in pH value of solution=4.
Embodiment 12
In the wish purifying water body that is 80mg/L in the concentration of nitrate ion, add the magnetic polypyrrole of 0.0004 times of its quality, nitrate ion in adsorbed water under the condition that 25 DEG C, pH are 4.0, adsorption time is 1min, adsorb saturated after, magnet separates, and records NO 3 -the adsorbance of ion is 40.69mg/g.
Embodiment 13
With embodiment 12, adsorption time is 3min, and other conditions are constant, record NO 3 -the adsorbance of ion is 44.50mg/g.
Embodiment 14
With embodiment 12, adsorption time is 10min, and other conditions are constant, record NO 3 -the adsorbance of ion is 46.57mg/g.
Embodiment 15
With embodiment 12, adsorption time is 20min, and other conditions are constant, record NO 3 -the adsorbance of ion is 46.92mg/g.
From embodiment 4,12～15, absorption reaches before balance, and adsorption time is longer, Fe 3o 4/ Ppy is to NO 3 -the adsorbance of ion is higher, and the time of arrival adsorption equilibrium is very fast, and adsorption efficiency is very high.
Embodiment 16
In the wish purifying water body that is 80mg/L in the concentration of nitrate ion, add the magnetic polypyrrole of 0.0004 times of its quality, H in water 2pO 3 -concentration is to adsorb in the condition of 2mmol/L, and 25 DEG C, pH are 4.0, adsorption time is 120min, adsorb saturated after, magnet separates, and records NO 3 -the saturated extent of adsorption of ion is 33.45mg/g.
Embodiment 17
With embodiment 16, H in water 2pO 3 -concentration is to adsorb in the condition of 8mmol/L, and other conditions are constant, record NO 3 -the saturated extent of adsorption of ion is 25.06mg/g.
Embodiment 18
With embodiment 16, H in water 2pO 3 -concentration is to adsorb in the condition of 20mmol/L, and other conditions are constant, record NO 3 -the saturated extent of adsorption of ion is 9.98mg/g.
From embodiment 16～18, Fe 3o 4/ Ppy adsorbent is to NO 3the adsorbance of-ion reduces rapidly with the increase of anion intensity.
Embodiment 19
Embodiment 4 is adsorbed to the Fe after saturated 3o 4/ Ppy, with the Fe after magnet collection absorption 3o 4/ Ppy taking 0.01mol/L NaCl solution as desorbing agent, carries out desorption, 25 DEG C of constant temperature oscillations, NaCl solution and Fe in closed container 3o 4the mass ratio of/Ppy is 2000:1, desorption time 2h, Fe after desorption 3o 4washed with de-ionized water several for/Ppy, carries out adsorption experiment again, and experiment condition is with embodiment 4.(desorption and regeneration rate is this absorption of adsorbent NO to measure for the first time desorption and regeneration rate 3 -mass of ion and the first NO adsorbing 3 -mass of ion ratio) be 81.2%.Loop adsorption and desorption regeneration tests, regenerate after four times, desorption and regeneration rate is 57.13%, and tends towards stability.
Visible, Fe 3o 4/ Ppy adsorbent is after four regeneration, and adsorbance remains unchanged substantially, shows that absorption property is stable, reusable edible.

Claims (6)

1. the preparation method of magnetic polypyrrole, is characterized in that, specifically implements according to following steps:
Step 1, by FeCl 24H 2o and FeCl 36H 2o is dissolved in the HCl solution that 50ml, concentration are 0.5moi/L, at N 2under protection, in the NaOH solution that to be added drop-wise to 450ml, concentration be 1.0～2.0mol/L, then at 75～85 DEG C, stir after co-precipitation 30～40min with deionized water washing to neutral, finally, in 45～55 DEG C of vacuum drying 10～12h, grinding, obtain Fe 3o 4nano particle;
Step 2, the Fe that step 1 is prepared 3o 4nano particle joins in deionized water, N 2the lower ultrasonic 10～15min of protection, then add FeCl 3rear mechanical agitation 30～40min, and then continue mechanical agitation reaction 3～3.5h after adding pyrroles (Ppy), after reaction finishes, add 10ml acetone cessation reaction, deionized water and acetone washing several for the reactant obtaining, finally vacuum drying 5～6h at 100～110 DEG C, grinds, and obtains magnetic polypyrrole (Fe 3o 4/ Ppy).
2. the preparation method of magnetic polypyrrole according to claim 1, is characterized in that, in step 1, and FeCl 24H 2o and FeCl 36H 2fe in O 2+with Fe 3+mol ratio be 1:1.5～2.5, Fe 2+concentration be 0.035mol/L.
3. the preparation method of magnetic polypyrrole according to claim 1 and 2, is characterized in that, in step 2, and Fe 3o 4mass concentration be 5g/L, Fe 3o 4with pyrroles's mass volume ratio be 2:3～5g/ml, FeCl 3concentration be 0.28mol/L.
4. utilize the method for nitrate anion in the magnetic polypyrrole adsorbed water described in claim 1, it is characterized in that, in the water body purifying in wish, add the magnetic polypyrrole of 0.0004 times of its quality, nitrate ion in adsorbed water under the condition that 25 DEG C, pH are 2.0～9.0, adsorb saturated after, magnet separates, the water being purified.
5. the method for nitrate anion in magnetic polypyrrole adsorbed water according to claim 4, is characterized in that, in the water body that wish purifies, the concentration of nitrate ion is 30～80mg/L.
6. according to the method for nitrate anion in the magnetic polypyrrole adsorbed water described in claim 4 or 5, it is characterized in that, adsorption time is 1min～120min.
CN201410168195.0A 2014-04-24 2014-04-24 Preparation method of magnetic polypyrrole and method of adsorbing nitrate in water Pending CN103933954A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104324706A (en) * 2014-11-05 2015-02-04 齐鲁工业大学 Preparation method of magnetic nanometer compound used for selectively separating silver ions
CN104785223A (en) * 2015-04-03 2015-07-22 西北民族大学 PPy (polypyrrole)/ nickel ferrite nanocomposite material as well as preparation and application thereof
CN107301913A (en) * 2017-05-15 2017-10-27 江汉大学 Magnetic Fe3O4The preparation method of@PPy composite nano materials
CN111318269A (en) * 2020-03-04 2020-06-23 河北工业大学 Preparation method and application of reductive amino acid doped polypyrrole adsorbent

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104324706A (en) * 2014-11-05 2015-02-04 齐鲁工业大学 Preparation method of magnetic nanometer compound used for selectively separating silver ions
CN104785223A (en) * 2015-04-03 2015-07-22 西北民族大学 PPy (polypyrrole)/ nickel ferrite nanocomposite material as well as preparation and application thereof
CN104785223B (en) * 2015-04-03 2017-11-28 西北民族大学 Polypyrrole/nickel ferrite based magnetic loaded nano composite material and its preparation and application
CN107301913A (en) * 2017-05-15 2017-10-27 江汉大学 Magnetic Fe3O4The preparation method of@PPy composite nano materials
CN107301913B (en) * 2017-05-15 2019-07-16 江汉大学 Magnetic Fe3O4The preparation method of@PPy composite nano materials
CN111318269A (en) * 2020-03-04 2020-06-23 河北工业大学 Preparation method and application of reductive amino acid doped polypyrrole adsorbent
CN111318269B (en) * 2020-03-04 2022-11-08 河北工业大学 Preparation method and application of reductive amino acid doped polypyrrole adsorbent

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