CN112791708A - Method for preparing attapulgite/polypyrrole composite material based on iron-containing wastewater - Google Patents
Method for preparing attapulgite/polypyrrole composite material based on iron-containing wastewater Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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Abstract
The invention discloses a method for preparing an attapulgite/polypyrrole composite material based on iron-containing wastewater. The invention takes the iron-containing wastewater as an oxidant and the attapulgite as a carrier, and adopts a one-pot method to prepare the attapulgite/polypyrrole composite material. The method is simple to operate, has a clean process, and is expected to provide a new way for high-added-value comprehensive utilization of the attapulgite.
Description
Technical Field
The invention relates to a method for preparing an attapulgite/polypyrrole composite material based on iron-containing wastewater, belonging to the field of composite material preparation.
Background
Polypyrrole is a heterocyclic conjugated conductive polymer material, can be used for biological, ion detection, supercapacitors, antistatic materials and electrode materials, and can also be used for electrolytic capacitors, electrocatalysis, conductive polymer composite materials and the like, and the application range is wide. Meanwhile, the complex has high surface energy and contains a large amount of imino groups, so that the complex has good complexing effect on some ions.
The attapulgite has the characteristics and advantages of special structure, high specific surface area, strong adsorption performance, low price, rich reserves and the like. However, the attapulgite has high surface activity and is easy to agglomerate. Therefore, a few reports are made on the research of compounding the polypyrrole and the attapulgite by combining the characteristics of the polypyrrole and the attapulgite, and the polypyrrole and attapulgite are mainly applied to the field of preparation of conductive materials. For example, chinese patent CN101418122A reports a method for preparing polypyrrole/attapulgite nano conductive composite material. The polypyrrole/attapulgite nanometer conductive composite material is prepared by adopting a rapid chemical oxidation in-situ polymerization method, and the synthesis process is simple and rapid. However, this patent has the following problems: the mass ratio of water to attapulgite is 4-19: 1, the using amount of the attapulgite is relatively large, and the attapulgite is difficult to disperse due to too high slurry concentration. Chinese patent CN102532539B discloses a preparation method of a one-dimensional conductive polypyrrole/attapulgite nano composite material; chinese patent CN106147563A discloses a preparation method of polypyrrole/attapulgite conductive paint. The two methods both need to be stirred for reaction for more than 20 hours, and have the problems of overlong reaction time and low efficiency. Chinese patent CN101838392A discloses a method for preparing a polypyrrole/attapulgite conductive composite material by adopting attapulgite, an oxidant, a pyrrole monomer and sulfamic acid; chinese patent CN102911358B discloses a preparation method of a polypyrrole/organic modified attapulgite conductive composite material. Both methods need to be carried out under the protection of nitrogen, the reaction conditions are harsh, and the method disclosed in the Chinese patent CN102911358B also needs to carry out organic modification on attapulgite, so that the technical process is complex.
Therefore, the patent develops a method for preparing the attapulgite/polypyrrole composite material by taking the iron-containing wastewater as an oxidant. The attapulgite modified water treatment agent effectively improves the dispersibility of attapulgite, improves the specific surface area of the composite material, and has better synergistic effect in the wastewater treatment process. Meanwhile, the method has the advantages of simple process, green and safe solvent and the like, and realizes the resource utilization of the iron-containing wastewater.
Disclosure of Invention
The invention aims to provide a method for preparing an attapulgite/polypyrrole composite material based on iron-containing wastewater.
The invention discloses a method for preparing an attapulgite/polypyrrole composite material based on iron-containing wastewater, which comprises the following steps:
(1) weighing a certain amount of concave-convexThe rod is at 300oAnd C, roasting for 2-4 hours to obtain the activated attapulgite.
(2) Adding the activated attapulgite into the iron-containing wastewater, and carrying out ultrasonic treatment for 5-10 min. Stirring and dissolving, then dropwise adding pyrrole, reacting for 3-5 h, carrying out suction filtration and precipitation, and washing a filter cake with distilled water until the filtrate is colorless. The filter cake is placed at 60oAnd C, drying for 6 hours, and grinding to obtain the black powdery attapulgite/polypyrrole composite material.
Further, the iron-containing wastewater is electroplating wastewater, and the components of the iron-containing wastewater are Zn 0-15 g/L, Fe 8-50 g/L and Cl - 10~60 g/L。
Further, the mass ratio of the activated attapulgite to the iron-containing wastewater is as follows: (0.5-1.0): 100.
Further, the mass ratio of the activated attapulgite to the pyrrole monomer is as follows: (0.4-1.5): 1.
The invention has the beneficial effects that: the method for preparing the attapulgite/polypyrrole composite material by using the iron-containing wastewater is simple to operate, the polypyrrole and the attapulgite are combined, the dispersity of the attapulgite is effectively improved, the specific surface area of the composite material is improved, the space structure of the composite material is further optimized through interaction, and a new way is hopefully provided for the high-added-value comprehensive utilization of the attapulgite.
Drawings
FIG. 1 is an XRD spectrum of activated attapulgite and attapulgite/polypyrrole; mATP stands for activated attapulgite, PPy stands for polypyrrole, and mATP/PPy stands for attapulgite/polypyrrole composite material.
FIG. 2 shows FT-IR spectra of activated attapulgite and/or polypyrrole.
Detailed Description
The following examples are helpful in understanding the present invention, but are not limited to the summary of the invention. The simple replacement or improvement of the present invention by those skilled in the art is within the technical scheme of the present invention.
Example 1
A method for preparing an attapulgite/polypyrrole composite material based on iron-containing wastewater mainly comprises the following steps:
firstly, the attapulgite is added in 300 oAnd C, roasting for 2 hours, and cooling to room temperature to obtain the activated attapulgite. Performing ultrasonic treatment on 200 mL of suspension of activated attapulgite and iron-containing wastewater (8 g/L) at a mass ratio of 0.5: 100 for 5 min, continuously stirring, dropwise adding pyrrole at a mass ratio of 0.4: 1 of activated attapulgite and pyrrole, and reacting for 3 h. After the reaction is finished, the precipitate is filtered and washed by distilled water until the filtrate is colorless, and then the filter cake is filtered at 60 DEGoAnd C, drying for 6 hours, and grinding to obtain the black powdery attapulgite/polypyrrole composite material. The attapulgite/polypyrrole is used in the adsorption experiment of the oxytetracycline hydrochloride, and the adsorption rate can reach 75 percent.
Example 2
A method for preparing an attapulgite/polypyrrole composite material based on iron-containing wastewater mainly comprises the following steps:
firstly, the attapulgite is placed at 300oAnd C, roasting for 3 hours, and cooling to room temperature to obtain the activated attapulgite. Performing ultrasonic treatment on 200 mL of suspension of activated attapulgite and iron-containing wastewater (25 g/L) at a mass ratio of 0.7: 100 for 8 min, continuously stirring, dropwise adding pyrrole at a mass ratio of activated attapulgite to pyrrole of 1: 1, and reacting for 4 h. After the reaction is finished, the precipitate is filtered and washed by distilled water until the filtrate is colorless, and then the filter cake is filtered at 60 DEGoAnd C, drying for 6 hours, and grinding to obtain the black powdery attapulgite/polypyrrole composite material. The attapulgite/polypyrrole is used in the adsorption experiment of the oxytetracycline hydrochloride, and the adsorption rate can reach 80 percent.
Example 3
A method for preparing an attapulgite/polypyrrole composite material based on iron-containing wastewater mainly comprises the following steps:
firstly, the attapulgite is placed at 300oAnd C, roasting for 4 hours, and cooling to room temperature to obtain the activated attapulgite. 200 mL of suspension of activated attapulgite and iron-containing wastewater (50 g/L) in a mass ratio of 1.0: 100 is subjected to ultrasonic treatment for 10 min, then continuously stirred, pyrrole is added dropwise in a mass ratio of the activated attapulgite to the pyrrole of 1.5: 1, and the reaction is carried out for 5 h. After the reaction is finished, the precipitate is filtered and washed by distilled water until the filtrate is colorless, and then the filter cake is filtered at 60 DEGoDrying for 6 h under C, grinding to obtain blackThe color powder substance is attapulgite/polypyrrole composite material. The attapulgite/polypyrrole is used in the adsorption experiment of the oxytetracycline hydrochloride, and the adsorption rate can reach 71 percent.
As shown in figure 1, mATP is activated attapulgite, and mATP/PPy is attapulgite/polypyrrole composite material. The characteristic diffraction peaks of the XRD pattern of the activated attapulgite appear at 2 theta =8.26 degrees, 19.69 degrees, 26.72 degrees and 35.39 degrees, and the characteristic peaks appear in the XRD pattern of the attapulgite/polypyrrole, but the peaks at 2 theta =8.26 degrees are weakened, and the peaks at 2 theta =61.55 degrees are strengthened.
In figure 2, mATP is activated attapulgite, and mATP/PPy is attapulgite/polypyrrole composite material. As shown in the figure, 985 cm-1And 1030 cm-1The absorption peaks correspond to the asymmetrical stretching vibration of the silicon-oxygen bond in a plane and the asymmetrical stretching vibration out of the plane respectively. 1198 cm-1The peak is caused by the asymmetric stretching vibration of Si-O in the silicon tetrahedron. 3550 cm-1And 3412 cm-1The peak is an antisymmetric absorption peak generated by crystal water and a stretching vibration peak of-OH. Compared with attapulgite, the attapulgite/polypyrrole is 1310 cm-1The peak is the C-N stretching vibration peak, 1462 cm-1、1545 cm-1And 1629 cm-1The peak is the skeleton vibration of the aromatic ring, and the result shows that the attapulgite/polypyrrole composite material is successfully prepared by the method.
In conclusion, the method for preparing the attapulgite/polypyrrole composite material effectively improves the dispersibility of the attapulgite, improves the specific surface area of the composite material and has better synergistic effect in the wastewater treatment process. Meanwhile, the method has the advantages of simple process, green and safe solvent and the like, and realizes the resource utilization of the iron-containing wastewater.
In the description of the embodiments of the present invention, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "center", "top", "bottom", "top", "root", "inner", "outer", "peripheral", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, only for the purpose of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Where "inside" refers to an interior or enclosed area or space. "periphery" refers to an area around a particular component or a particular area.
In the description of the embodiments of the present invention, the terms "first", "second", "third", and "fourth" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, features defined as "first", "second", "third", "fourth" may explicitly or implicitly include one or more of the features. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the embodiments of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "assembled" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In the description of the embodiments of the invention, the particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples.
In the description of the embodiments of the present invention, it is to be understood that "-" and "-" denote ranges of two numerical values, and the ranges include endpoints. For example, "A-B" means a range greater than or equal to A and less than or equal to B. "A to B" represents a range of A or more and B or less.
In the description of the embodiments of the present invention, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three kinds of relationships, for example, a and/or B, and may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A method for preparing an attapulgite/polypyrrole composite material based on iron-containing wastewater comprises the following steps:
(1) weighing a certain amount of attapulgite at 300oAnd C, roasting for 2-4 hours to obtain the activated attapulgite.
(2) Adding the activated attapulgite into the iron-containing wastewater, and carrying out ultrasonic treatment for 5-10 min. Stirring and dissolving, then dropwise adding pyrrole, reacting for 3-5 h, carrying out suction filtration and precipitation, and washing a filter cake with distilled water until the filtrate is colorless. The filter cake is placed at 60oAnd C, drying for 6 hours, and grinding to obtain the black powdery attapulgite/polypyrrole composite material.
2. The method for preparing the attapulgite/polypyrrole composite material based on the iron-containing wastewater according to claim 1, wherein the iron-containing wastewater in the step (2) is electroplating wastewater, and the components of the iron-containing wastewater are Zn 0-15 g/L, Fe 8-50 g/L and Cl- 10~60 g/L。
3. The method for preparing the attapulgite/polypyrrole composite material based on the wastewater containing iron according to claim 1, wherein the mass ratio of the activated attapulgite to the wastewater containing iron in the step (2) is: (0.5-1.0): 100.
4. The method for preparing the attapulgite/polypyrrole composite material based on the iron-containing wastewater according to claim 1, wherein the mass ratio of the activated attapulgite to the pyrrole monomer in the step (2) is as follows: (0.4-1.5): 1.
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| CN114921096A (en) * | 2022-06-15 | 2022-08-19 | 瓮福（集团）有限责任公司 | Method for preparing attapulgite/polypyrrole composite material based on iron-containing wastewater |
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