CN102091598A - Shellac modified nano-magnetic adsorbent, preparing method and application thereof - Google Patents
Shellac modified nano-magnetic adsorbent, preparing method and application thereof Download PDFInfo
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- CN102091598A CN102091598A CN2010106040752A CN201010604075A CN102091598A CN 102091598 A CN102091598 A CN 102091598A CN 2010106040752 A CN2010106040752 A CN 2010106040752A CN 201010604075 A CN201010604075 A CN 201010604075A CN 102091598 A CN102091598 A CN 102091598A
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Abstract
The invention discloses a shellac modified nano-magnetic adsorbent, a preparing method and an application thereof, wherein the adsorbent comprises magnetic nano-particle substrates which are coated with the shellac; the preparation method comprises the following steps of: dissolving the shellac in ammonia water to prepare shellac ammonia solution; under room temperature inert gas or nitrogen atmosphere, preparing mixed solution of iron ions and ferrous ions by FeCl3 and FeCl2; and under water bath and stirring condition, at temperature of 85-90 DEG C, orderly adding the ammonia water and the shellac ammonia solution in the mixed solution of the iron ions and the ferrous ions, continuously stirring, cooling the mixed solution, separating precipitates, washing and constanting volume to prepare the adsorbent; the application comprises the following steps of: adding the adsorbent in the solution containing heavy metal ions; under the room temperature, carrying out vibration absorption reaction, and separating the adsorbent by a magnet. The adsorbent disclosed by the invention is low in cost, large in specific surface area, high in absorption performance, easy to separate and environment friendly and the like.
Description
Technical field
The present invention relates to shellac application and field of waste water treatment, refer in particular to a kind of nano-magnetic adsorbent and its production and application.
Background technology
The development of developing rapidly of modern industry, particularly mining industry, metallurgy, machining, surface treatment and heavy industry causes the heavy metal pollution in nature waters serious.The method of heavy metal ion mainly contains in traditional removal water: chemical precipitation method, oxidation-reduction method, ferrite process, electrolysis, evaporation concentration method, ion-exchange-resin process etc., these methods existence investments are big, operating cost is high, operational administrative is loaded down with trivial details and cause secondary pollution problems easily, and can not effectively realize the utilization again of heavy metal and water resource.Therefore, what use morely in the practice at present is absorption method, it has advantages such as material cheaply is easy to get, cost is low, removal effect is good, the adsorbent of removal heavy metal commonly used mainly contains active carbon, mesoporous material, clay, zeolite, shitosan and apatite etc., and these adsorbents all exist shortcoming such as not easily separated after the little or absorption of adsorption capacity, therefore must strive to find new promising adsorbent.
Utilize natural material, synthetic inorganic material or natural material organic and that inorganic material is synthetic to become the research field of a hot topic as adsorbent in recent years, its main cause is: the weak and inorganic adsorbent of the active force between inorganic adsorbent and adsorbate has great heat endurance, thereby makes that its regeneration is fairly simple; Simultaneously, the cheap and environmental friendliness of natural material can not produce secondary pollution.Yet traditional inorganic adsorbent specific area is little, adsorption capacity is lower.Nano material has great specific area, so nano material has become one of widely used adsorbent.
At present, it is in the majority that both at home and abroad shellac is applied to the report of medicine food aspect, but the adsorbent that is applied to the adsorption treatment heavy metal ion does not appear in the newspapers.
Summary of the invention
Technical problem to be solved by this invention is: at the technical problem that prior art exists, the invention provides a kind of with low cost, specific area big, good biocompatibility, absorption property is high and the segregative shellac decorated nanometer magnetic adsorbent that can be used for the adsorption treatment heavy metal ion; And a kind of technology simple, prepare the preparation method of shellac decorated nanometer magnetic adsorbent fast; Also provide fast, the eco-friendly above-mentioned shellac decorated nanometer magnetic adsorbent of a kind of adsorption rate to be used for the application of adsorption treatment heavy metal ion.
For solving the problems of the technologies described above, the present invention by the following technical solutions: a kind of shellac decorated nanometer magnetic adsorbent, it is characterized in that described adsorbent comprises the magnetic nano-particle matrix, be coated with shellac on the described magnetic nano-particle matrix.
In the above-mentioned adsorbent, described magnetic nano-particle matrix is preferably nano magnetic ferrite thing (mass ratio of ferro element and shellac is generally in (2.25～3) in the adsorbent: (1.75～2)).
As a total technical conceive, the present invention also provides a kind of preparation method of above-mentioned shellac decorated nanometer magnetic adsorbent, may further comprise the steps:
(1) shellac is dissolved in ammoniacal liquor, makes the shellac ammonia spirit, the concentration of shellac is 0.05g/ml～0.3g/ml in the described shellac ammonia spirit;
(2) under room temperature and inert gas or nitrogen protection atmosphere, be (1.25～2) with mol ratio: 1 FeCl
3And FeCl
2Be dissolved in the deoxidized water, obtain iron ion and ferrous ion mixed solution, be heated to 85 ℃～90 ℃ gradually;
(3) under temperature is 85 ℃～90 ℃ water-bath, stirring condition, in above-mentioned iron ion and ferrous ion mixed solution, dropwise add ammoniacal liquor and described shellac ammonia spirit successively, the volume ratio of described ammoniacal liquor, shellac ammonia spirit and iron ion and ferrous ion mixed solution is 1: (1.5～2.5): (10～15), continue to stir 30min～60min;
(4) the mixed liquor cooling that step (3) is obtained, sediment separate out and washing, constant volume promptly obtain described adsorbent.
Among the above-mentioned preparation method, the mass concentration of described ammoniacal liquor is preferably 25%～28%.
The present invention also provides a kind of above-mentioned application of shellac decorated nanometer magnetic adsorbent in the adsorption treatment heavy metal ion, may further comprise the steps: in the solution that contains heavy metal ion, add described shellac decorated nanometer magnetic adsorbent, vibrate at ambient temperature after the adsorption reaction, with magnet adsorbent is separated, finish adsorption treatment heavy metal ion.
In the above-mentioned application, the consumption of adsorbent is preferably 0.1g/L～0.9g/L in the described solution that contains heavy metal ion.
In the above-mentioned application, the condition of described adsorption reaction is preferably: pH value is 7～8.5, and the reaction time is 1h～24h.
In the above-mentioned application, the described salinity that contains the solution of heavy metal ion is preferably 0～3.5%, and described heavy metal comprises one or more the combination in copper, lead, zinc, the cadmium.
Compared with prior art, the invention has the advantages that:
1, shellac decorated nanometer magnetic adsorbent of the present invention, with low cost, not only have the nano particle specific area is big, surface atom easily combines with other atom or ion characteristics, adsorption efficiency height, and since its have magnetic, thereby be easy to from pending solution, separate, environmental friendliness.
2, the preparation method of shellac decorated nanometer magnetic adsorbent of the present invention, technology and simple to operate, preparation fast can effectively realize the suitability for industrialized production of shellac modified magnetic nano adsorber.
3, shellac decorated nanometer magnetic adsorbent of the present invention is used for the application of adsorption treatment heavy metal ion, magnetic separation technique is combined with adsorption process, realize its effective absorption and processing to heavy metal ions in wastewater, fast, the environmental friendliness of adsorption rate is for the improvement of heavy metal pollution in the waste water provides new approach.
Description of drawings
Fig. 1 is the transmission electron microscope schematic diagram of the shellac modified magnetic nano adsorber of the embodiment of the invention 1;
Fig. 2 is the X ray energy dispersion analysis (EDA) schematic diagram of the shellac modified magnetic nano adsorber of the embodiment of the invention 1;
Fig. 3 is the infrared spectrum schematic diagram of shellac modified magnetic nano adsorber, shellac and the magnetic iron oxide of the embodiment of the invention 1;
Fig. 4 is the magnetization curve schematic diagram of the shellac modified magnetic nano adsorber of the embodiment of the invention 1.
The specific embodiment
Below with reference to Figure of description and specific embodiment the present invention is described in further details.
Embodiment 1:
A kind of shellac decorated nanometer magnetic adsorbent of the present invention, this adsorbent comprises nano magnetic ferrite thing matrix, is coated with shellac on the nano magnetic ferrite thing matrix.This nano magnetic ferrite thing is mainly tri-iron tetroxide, and the mass ratio of ferro element and shellac is 2.5: 1.77 in the adsorbent.This shellac decorated nanometer magnetic adsorbent is prepared by above method:
(1) 1.5g shellac is dissolved in the ammoniacal liquor of 5ml 25%, and adds the dilution of 15ml water, be beneficial to the dissolving of shellac, make the shellac ammonia spirit;
(2) in room temperature and feed under the atmospheric condition of nitrogen, with the FeCl of 0.0227mol
36H
2The FeCl of O and 0.0151mol
24H
2O is dissolved in the deoxidized water, makes iron ion and ferrous ion mixed solution 100ml, then this ferric ion solutions is heated to 90 ℃ gradually in stirred in water bath;
When (3) treating that bath temperature reaches 90 ℃, in above-mentioned iron ion and ferrous ion mixed solution, dropwise add 25% ammoniacal liquor 10ml and above-mentioned shellac ammonia spirit while stirring successively; Continue to stir 30min;
(4) the mixed liquor cooling that step (3) is obtained, sediment separate out and washing, constant volume promptly obtain adsorbent.
The above-mentioned shellac decorated nanometer magnetic adsorbent outward appearance that makes is brownish black, and the transmission electron microscope that is placed on 500,000 times is observed down, its nucleocapsid structure as shown in Figure 1, this adsorbent average grain diameter is about 20～30nm as can be seen, and its matrix surface has coated shellac.This adsorbent is carried out the X ray energy dispersion analysis (EDA), its analysis result as shown in Figure 2, mainly contain three kinds of elements of C, Fe and O as can be seen in this adsorbent (because the content of H element is less, so the intensity of absworption peak a little less than, so do not indicate among the figure), C wherein, H element mainly come from shellac.Above-mentioned adsorbent, shellac and nano magnetic ferrite thing are carried out infrared spectrum analysis respectively, its analysis result as shown in Figure 3, contain functional groups such as a large amount of hydroxyls and carboxyl as can be known in the shellac, these character are also embodied in the above-mentioned adsorbent, thereby cause making the absorption of this ABSORBENTS ABSORPTION metal ion to become possibility.Above-mentioned adsorbent is carried out magnetization test, its magnetization curve figure as shown in Figure 4, therefore this adsorbent has stronger magnetic as can be known, can make it be easy to separate from solution by magnet.
Embodiment 2:
Shellac decorated nanometer magnetic adsorbent of the present invention is used for the heavy metal ion of adsorption treatment waste water, may further comprise the steps:
The shellac decorated nanometer magnetic adsorbent that embodiment 1 is made adds the Cd that contains of two kinds of different heavy metal initial concentrations respectively to
2+50mL waste water in, the consumption of this adsorbent is 0.416g/L, regulate the pH value to 8.0 (± 0.1) of waste water, at ambient temperature, adopt the adsorption reaction of vibrating of constant temperature water bath oscillator, with magnet this adsorbent is separated from waste water behind the 24h, finished adsorption treatment heavy metal ions in wastewater.
After the above-mentioned reaction, measure the Cd that is not adsorbed in the waste water with atomic absorption spectrophotometry respectively
2+Content, calculate adsorbent surface Cd
2+Adsorbance result as shown in table 1:
Table 1: the adsorbance data of adsorbent under the different heavy metal initial concentration conditions
As shown in Table 1, be that this adsorbent has the adsorbance of 18.26mg/g under the condition of 82.8mg/L at initial concentration, and increase with initial concentration.
Embodiment 3:
Shellac decorated nanometer magnetic adsorbent of the present invention is used for the heavy metal ion of adsorption treatment waste water, may further comprise the steps:
Add the shellac decorated nanometer adsorbent of the present invention that makes among the embodiment 1 to 50mL with different dosage and contain Cd
2+In the waste water of ion, the consumption of this adsorbent is for being respectively 0.122g/L, 0.244g/L, 0.366g/L, regulate pH value to 7.5 (± 0.1), at ambient temperature, adopt the adsorption reaction of vibrating of constant temperature water bath oscillator, with magnet adsorbent is separated from above-mentioned waste water behind the 24h, finished adsorption treatment heavy metal ions in wastewater.
After the above-mentioned reaction, measure the Cd that is not adsorbed in the above-mentioned waste water with atomic absorption spectrophotometry respectively
2+Content, calculate adsorbent surface Cd
2+Adsorbance result as shown in table 2:
Table 2: the adsorbance data of adsorbent during different adsorbent consumption
As shown in Table 2, the adsorbance of adsorbent does not increase with the consumption of adsorbent, but is issued to maximum at a certain an amount of consumption.
Embodiment 4:
Shellac decorated nanometer magnetic adsorbent of the present invention is used for the heavy metal ion of adsorption treatment waste water, may further comprise the steps:
The shellac decorated nanometer adsorbent that makes among the embodiment 1 is added to the Cd that contains of each 50mL respectively
2+Waste water in, the consumption of adsorbent is 0.67g/L, regulates pH value to 8.0 (± 0.1), at ambient temperature, adopt the adsorption reaction of vibrating of constant temperature water bath oscillator, with magnet this adsorbent is separated from above-mentioned waste water behind the 24h, finish adsorption treatment heavy metal ions in wastewater.
After the above-mentioned reaction, measure the Cd that is not adsorbed in the waste water with atomic absorption spectrophotometry respectively
2+Content calculates adsorbent surface Cd
2+Adsorbance, under the condition that initial concentration is identical, salinity (being the concentration of NaCl) is different of heavy metal ions in wastewater, absorption result is as shown in table 3:
Table 3: the adsorbance of adsorbent under the different salinity condition
As shown in Table 3, the adsorbance of adsorbent is subjected to the influence of salinity, and adsorbance reduces gradually with the increase of salinity, but still considerable adsorbance is arranged.
In sum, shellac modified magnetic nano adsorber among the present invention is compared with adsorbents such as active carbon, zeolite, clay, shitosans, not only specific area is bigger, adsorption efficiency is higher, and prepares simple, with low cost, environmental friendliness and be easy to and separate from solution and recycle; This adsorbent can be widely used in the adsorption treatment of heavy metal ion as a kind of nano material absorbent of being made up of inorganic matter and natural organic matter.
Below only be preferred implementation of the present invention, protection scope of the present invention also not only is confined to the foregoing description, conceives the various process programs of no substantial differences all in protection scope of the present invention with the present invention.
Claims (8)
1. a shellac decorated nanometer magnetic adsorbent is characterized in that described adsorbent comprises the magnetic nano-particle matrix, is coated with shellac on the described magnetic nano-particle matrix.
2. shellac decorated nanometer magnetic adsorbent as claimed in claim 1 is characterized in that described magnetic nano-particle matrix is the nano magnetic ferrite thing.
3. the preparation method of a shellac decorated nanometer magnetic adsorbent as claimed in claim 2 may further comprise the steps:
(1) shellac is dissolved in ammoniacal liquor, makes the shellac ammonia spirit, the concentration of shellac is 0.05g/ml～0.3g/ml in the described shellac ammonia spirit;
(2) under room temperature and inert gas or nitrogen protection atmosphere, be (1.25～2) with mol ratio: 1 FeCl
3And FeCl
2Be dissolved in the deoxidized water, obtain iron ion and ferrous ion mixed solution, be heated to 85 ℃～90 ℃ gradually;
(3) under temperature is 85 ℃～90 ℃ water-bath, stirring condition, in above-mentioned iron ion and ferrous ion mixed solution, dropwise add ammoniacal liquor and described shellac ammonia spirit successively, the volume ratio of described ammoniacal liquor, shellac ammonia spirit and iron ion and ferrous ion mixed solution is 1: (1.5～2.5): (10～15), continue to stir 30min～60min;
(4) the mixed liquor cooling that step (3) is obtained, sediment separate out and washing, constant volume promptly obtain described adsorbent.
4. the preparation method of shellac decorated nanometer magnetic adsorbent according to claim 3 is characterized in that, the mass concentration of described ammoniacal liquor is 25%～28%.
5. the application of a shellac decorated nanometer magnetic adsorbent as claimed in claim 2 in the adsorption treatment heavy metal ion, may further comprise the steps: in the solution that contains heavy metal ion, add described shellac decorated nanometer magnetic adsorbent, vibrate at ambient temperature after the adsorption reaction, with magnet adsorbent is separated, finish adsorption treatment heavy metal ion.
6. application according to claim 5 is characterized in that, the consumption of adsorbent is 0.1g/L～0.9g/L in the described solution that contains heavy metal ion.
7. application according to claim 5 is characterized in that, the condition of described adsorption reaction is: pH value is 7～8.5, and the reaction time is 1h～24h.
8. application according to claim 5 is characterized in that, the described salinity that contains the solution of heavy metal ion is 0～3.5%, and described heavy metal comprises one or more the combination in copper, lead, zinc, the cadmium.
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| CN102266750A (en) * | 2011-08-01 | 2011-12-07 | 武汉工程大学 | In situ preparation method of magnetic bio-absorbent |
| CN102380348A (en) * | 2011-09-21 | 2012-03-21 | 湖南大学 | Pectin modified magnetic nano-adsorbent and preparation method and application thereof |
| CN107823720A (en) * | 2013-05-02 | 2018-03-23 | 卡迪奥诺沃姆有限公司 | Balloon surface coating |
| CN114525127A (en) * | 2021-12-31 | 2022-05-24 | 宁波市第一医院 | Preparation method and application of carbon quantum dot nano assembly |
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| CN108483548B (en) * | 2017-12-20 | 2021-10-08 | 广西大学 | Application of organic modified magnetic alkaline calcium bentonite in heavy metal adsorption |
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Cited By (5)
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| CN102266750A (en) * | 2011-08-01 | 2011-12-07 | 武汉工程大学 | In situ preparation method of magnetic bio-absorbent |
| CN102380348A (en) * | 2011-09-21 | 2012-03-21 | 湖南大学 | Pectin modified magnetic nano-adsorbent and preparation method and application thereof |
| CN107823720A (en) * | 2013-05-02 | 2018-03-23 | 卡迪奥诺沃姆有限公司 | Balloon surface coating |
| CN114525127A (en) * | 2021-12-31 | 2022-05-24 | 宁波市第一医院 | Preparation method and application of carbon quantum dot nano assembly |
| CN114525127B (en) * | 2021-12-31 | 2023-12-12 | 宁波市第一医院 | Preparation method and application of carbon quantum dot nano assembly |
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