CN110201644B - Modified montmorillonite, preparation method and application thereof - Google Patents
Modified montmorillonite, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to modified montmorillonite, a preparation method and application thereof. The preparation method of the modified montmorillonite of the invention carries out microwave modification treatment on sodium-based montmorillonite through dioctadecyl tetrahydroxy ethyl dibromopropane diammonium to prepare the modified montmorillonite with larger interlayer spacing, provides more adsorption space for organic pollutants, and simultaneously leads the hydrophobicity of the modified montmorillonite to be enhanced because the modified montmorillonite introduces hydrophobic groups and cationic groups of the dioctadecyl tetrahydroxy ethyl dibromopropane diammonium, the surface of the modified montmorillonite is provided with positive charges, and the modified montmorillonite has electrostatic interaction of mutual attraction with anionic pollutants, thereby leading the modified montmorillonite to be capable of effectively removing the organic pollutants in wastewater, in particular methyl orange, and the adsorption capacity of the modified montmorillonite to the methyl orange can be up to more than 200 mg/g.
Description
Technical Field
The invention belongs to the field of solid materials and the field of water treatment, and relates to modified montmorillonite, a preparation method and application thereof.
Background
Most of the dyes currently used in industry are synthetic dyes containing large amounts of toxic, non-biodegradable organic compounds. Once discharged into the natural environment, untreated dye wastewater can pose a serious environmental pollution challenge and even threaten human life. Therefore, the development of the technology for treating organic matters in synthetic dye wastewater has received extensive attention from researchers. Methyl Orange (MO) is a water-soluble azo compound, which is a representative dye, often present in dye waste water. There are many methods for treating dye wastewater, among which the adsorption method is an economical, efficient, relatively environmentally friendly remediation method, and is one of the most commonly used wastewater treatment techniques.
Montmorillonite is widely used in wastewater treatment because of its low cost, abundant reserves, strong cation exchange capacity and environmental protection. Although montmorillonite has an adsorption ability, this ability is limited and its adsorption property must be improved by an appropriate method. The surfactant can be absorbed on the surface of the montmorillonite or inserted between layers of the montmorillonite through a cation exchange reaction with the montmorillonite, so that the surface of the montmorillonite is changed, the interlayer spacing is increased, the original hydrophilicity is changed into lipophilicity, and the affinity of the montmorillonite to the dye is further increased.
To date, most researchers have been devoted to modifying montmorillonites with traditional single-chain surfactants, and few studies and reports have been made with gemini surfactants, particularly those containing hydroxyl groups in the alkyl chain. Compared with the traditional quaternary ammonium compounds, the gemini quaternary ammonium salts are an emerging class of cationic surfactants, each gemini quaternary ammonium salt molecule has two head groups with positive charges, so that excellent properties such as good synergistic effect, lower Krafft point, improved wetting and foaming performance, better solubilizing capability and surface activity are endowed, and the adsorption behavior of the gemini quaternary ammonium salts is also obviously influenced. However, according to the research results, the adsorption capacity of montmorillonite modified by gemini quaternary ammonium salt to methyl orange is still foundRelatively low, such as Bo Liu et al (B.Liu, X.Wang, B.Yang, R.Sun, Rapid modification of montmorillonite with novel cationic surfactants and Materials adsorption for methyl orange, Materials Chemistry&Physics,2011,130 (3): 1220-1226.) Gemini quaternary ammonium surfactant 18-3-18 (C)43H92N2Cl2And the molecular weight is 707), the organic montmorillonite is prepared by microwave radiation for 1h, the interlayer spacing of the prepared organic montmorillonite (18-3-18-Mt) is only 2.31nm at most, and the maximum adsorption quantity to methyl orange is only about 50 mg/g.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide modified montmorillonite, a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
in a first aspect, the invention provides a preparation method of modified montmorillonite, which comprises the following steps: dispersing sodium montmorillonite (Na-Mt) in water, slowly adding Dioctadecyl Tetrahydroxyethyl Dibromopropane Diammonium (DTDD) water solution to obtain suspension, then placing the suspension in a microwave reactor, setting microwave power, reaction temperature and reaction time, collecting precipitate after the reaction is finished, and then washing the precipitate with water until the washed solution and AgNO are mixed3And (3) detecting no bromide ion in the solution reaction, and then drying the washed precipitate to obtain a dried precipitate, namely the modified montmorillonite (DMt).
The structural formula of DTDD is shown below:
after the sodium montmorillonite is subjected to DTDD microwave modification treatment, the interlayer spacing is increased, more adsorption spaces are provided for organic pollutants, and meanwhile, the hydrophobicity of the sodium montmorillonite is enhanced due to the introduction of a hydrophobic group of DTDD; because the cationic group of DTDD is introduced, the surface of the DTDD carries positive charges, and the DTDD and anionic pollutants have electrostatic interaction of mutual attraction, so that the prepared modified montmorillonite can effectively remove organic pollutants in wastewater.
As a preferred embodiment of the preparation method, the dosage of the dioctadecyl tetrahydroxyethyl dibromopropane diammonium is more than 0.5 times of the cation exchange capacity of the sodium-based montmorillonite; as a more preferable embodiment of the preparation method, the dosage of the dioctadecyl tetrahydroxyethyl dibromopropane diammonium is 1.0 to 1.5 times of the cation exchange capacity of the sodium-based montmorillonite. When the dosage of DTDD is more than 0.5 times of the cation exchange capacity of the sodium-based montmorillonite, the interlamellar spacing of the modified montmorillonite is increased to more than 1.96nm from the original 1.24 +/-0.1 nm after the sodium-based montmorillonite is modified, and particularly when the dosage of DTDD is 1.0-1.5 times of the cation exchange capacity of the sodium-based montmorillonite, the interlamellar spacing of the modified montmorillonite reaches 4.09 +/-0.1 nm, so that a larger adsorption space can be provided for organic pollutants, more DTDD groups are introduced, and the adsorption capacity of the modified montmorillonite on the organic pollutants is stronger.
As a preferred embodiment of the preparation method, the microwave power is 800W, the reaction temperature is 85 ℃, and the reaction time is 1 h.
As a preferable embodiment of the preparation method of the present invention, the ratio of sodium montmorillonite to total water in the raw materials for the reaction is 1g:37.5 mL.
As a preferred embodiment of the preparation method of the present invention, the sodium montmorillonite is directly used for preparing the modified montmorillonite without purification treatment after purchase. The sodium-based montmorillonite is directly used for microwave modification without treatment after purchase, the interlamellar spacing of the prepared modified montmorillonite can be obviously improved and can reach 4.09 +/-0.1 nm, and the adsorption capacity to methyl orange can be obviously improved to more than 200 mg/g.
In a second aspect, the invention provides modified montmorillonite prepared by the preparation method.
In a third aspect, the invention also provides application of the modified montmorillonite prepared by the preparation method in removing organic pollutants in wastewater.
As a preferred embodiment of the use of the present invention, the organic contaminants comprise methyl orange; as a more preferable embodiment of the application of the invention, the adsorption capacity of the modified montmorillonite to methyl orange is more than 200 mg/g; as a further preferable embodiment of the application of the invention, the adsorption quantity of the modified montmorillonite to methyl orange is 249.42 mg/g. Under the same adsorption condition, the maximum adsorption quantity of 18-3-18-Mt to methyl orange is only about 50mg/g, while the adsorption quantity of the modified montmorillonite (DMt) to methyl orange can reach 99.81 mg/g; the adsorption capacity can reach 200mg/g or even 249.42mg/g by changing the adsorption condition, which is probably partly due to DMt introduced hydroxyl in DTDD to generate hydrogen bond interaction with methyl orange.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the preparation method of the modified montmorillonite of the invention carries out microwave modification treatment on sodium-based montmorillonite through dioctadecyl tetrahydroxy ethyl dibromopropane diammonium to prepare the modified montmorillonite with larger interlayer spacing, provides more adsorption space for organic pollutants, and simultaneously leads the hydrophobicity of the modified montmorillonite to be enhanced because the modified montmorillonite introduces hydrophobic groups and cationic groups of the dioctadecyl tetrahydroxy ethyl dibromopropane diammonium, the surface of the modified montmorillonite is provided with positive charges, and the modified montmorillonite has electrostatic interaction of mutual attraction with anionic pollutants, thereby leading the modified montmorillonite to be capable of effectively removing the organic pollutants in wastewater.
(2) The modified montmorillonite prepared by the preparation method of the modified montmorillonite can be used for removing organic pollutants in wastewater, particularly methyl orange, and the adsorption capacity can reach more than 200 mg/g.
Drawings
FIG. 1 is a diagram of the synthesis and adsorption mechanism of modified montmorillonite (DMt) according to the present invention;
FIG. 2 is an infrared spectrum of Na-montmorillonite and the modified montmorillonite of examples 1-3;
FIG. 3 is an X-ray diffraction pattern of sodium-based montmorillonite and the modified montmorillonite of examples 1-3;
FIG. 4 is a graph showing the adsorption effect of sodium-based montmorillonite and the modified montmorillonite of example 2 and comparative example 1 on methyl orange.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
One embodiment of the preparation method of the modified montmorillonite comprises the following steps: firstly, dissolving dioctadecyl tetrahydroxyethyl dibromopropane diammonium into 80mL of water to obtain a dioctadecyl tetrahydroxyethyl dibromopropane diammonium water solution; dispersing 4.0g of sodium montmorillonite which is purchased from the market into 70mL of water directly without treatment, slowly adding aqueous solution of dioctadecyl tetrahydroxyethyl dibromopropane diammonium to obtain suspension, then placing the suspension into a microwave reactor, setting the microwave power to be 800W, the reaction temperature to be 85 ℃, the reaction time to be 1h, collecting precipitate by centrifugation after the reaction is finished, and washing the precipitate by water until the washed solution and AgNO are washed3The solution reaction does not detect bromide ions, then freeze-drying the cleaned precipitate at-40 ℃, and then grinding and screening by a 65-mesh screen to obtain powder with the particle size of below 65 meshes, namely the modified montmorillonite; wherein the dosage of the dioctadecyl tetrahydroxyethyl dibromopropane diammonium is 0.5 times of the cation exchange capacity of the sodium montmorillonite (namely 0.5 CEC).
Example 2
One embodiment of the method of the present invention for preparing modified montmorillonite; the preparation method is the same as that of the example 1 except that the dosage of the dioctadecyl tetrahydroxyethyl dibromopropane diammonium is 1.0 time of the cation exchange capacity of the sodium-based montmorillonite (namely 1.0 CEC).
Example 3
One embodiment of the method of the present invention for preparing modified montmorillonite; the preparation method is the same as that of the example 1 except that the dosage of the dioctadecyl tetrahydroxyethyl dibromopropane diammonium is 1.5 times of the cation exchange capacity of the sodium-based montmorillonite (namely 1.5 CEC).
Comparative example 1
Comparative example 1 is a method of preparing modified montmorillonite; the preparation method is the same as the embodiment 2 except that the modifier is single-chain surfactant octadecyl methyl dihydroxyethyl ammonium bromide (namely OMDAB), and the prepared modified montmorillonite is marked as OMt; the structural formula of OMDAB is shown below:
the applicant carried out the following tests to illustrate the effect of the present application:
(1) infrared Spectrum testing
The applicants conducted IR spectroscopy on Na-montmorillonite (Na-Mt) and the modified montmorillonite of examples 1-3, and the results are shown in FIG. 2.
As can be seen from FIG. 2, the Na-montmorillonite and the modified montmorillonite of examples 1-3 have several common infrared absorption peaks, for example, 1037cm-1At 528cm of Si-O bending vibration peak-1The peak of Al-O-Si bending vibration at, and 463cm-1-1The peak of the Si-O-Si bending vibration. In addition, 3636cm-1The band of (A) corresponds to-OH stretching vibration of Al-OH and Si-OH groups in sodium-based montmorillonite, and is 3325cm-1Broadband sum of (A) 1634cm-1The wider bands of (A) are respectively attributed to stretching and deformation vibration of interlayer water molecules HOH in the sodium-based montmorillonite. Compared with sodium-based montmorillonite, the modified montmorillonite is 2917cm-1And 2852cm-1Two new bands appear, which are the asymmetric and symmetric extensional oscillation peaks of-CH in the surfactant during intercalation, and 1468cm-1The band at (a) corresponds to bending vibration of the-CH bond in the in-plane surfactant. In addition, compared with sodium-based montmorillonite, the modified montmorillonite sample is 3325cm-1And 1634cm-1The peak of the O — H bond at (a) is weakened, indicating that water molecules in the interlayer of the sodium-based montmorillonite are replaced by surfactant, indicating that insertion or adsorption into the sodium-based montmorillonite has been successful.
(2) XRD test
The applicant carried out XRD tests on sodium montmorillonite (Na-Mt) and the modified montmorillonite of examples 1-3, and the specific results are shown in FIG. 3.
In fig. 3, the d001 diffraction peak of sodium montmorillonite appears at 7.138 ° and the corresponding interlayer distance is calculated to be 1.24 ± 0.1nm according to the bragg equation (n λ 2dsin θ). Unlike Na-Mt, the d001 peak of the modified montmorillonite is shifted to a lower 2 θ value, indicating that extension of the interlayer space has occurred and is a surfactant that is embedded due to microwave irradiation. With the increase of the DTDD dosage, the interlayer spacing of the modified montmorillonite is remarkably increased from 1.24 +/-0.1 nm to 4.09 +/-0.1 nm, which shows that the interlayer spacing of the modified montmorillonite is positively correlated with the DTDD dosage.
(3) Adsorption experiment of methyl orange
The applicant added 40mg of the modified montmorillonite of example 2 to 100mL of 20mg/L, 40mg/L, 60mg/L, 80mg/L, 100mg/L and 120mg/L of Methyl Orange (MO) dye, respectively, sealed with a sealing cap, placed in a constant temperature water bath (room temperature) and stirred at 400rpm for 2 hours, and then rapidly taken the adsorbed solution and passed through a 0.45 μm hydrophilic Polyethersulfone (PES) syringe filter, and then measured the MO concentration with an ultraviolet-visible spectrophotometer, and the results of the MO adsorption amount and removal rate are shown in Table 1.
TABLE 1 MO adsorption amount and removal rate test results
As can be seen from table 1, the amount of MO removed by DMt increased with increasing MO concentration; when the initial concentration of MO was increased from 20mg/L to 120mg/L, the amount of adsorbed MO increased from 49.94mg/g to 249.42mg/g, and the MO removal efficiency decreased from 99.87% to 83.14%, but a high removal rate remained. This phenomenon may be related to an increase in the competition of MO molecules for the available space on the DMt surface, and may also be related to an increase in steric hindrance caused by adsorption of other molecules to nearby adsorption sites. At lower concentrations, DMt has more binding sites not occupied by MO molecules and therefore provides a relatively high removal rate. However, as the concentration of MO increases, DMt tends to saturate at the active sites, and when the concentration of MO exceeds 80mg/L, the removal efficiency of MO decreases rapidly, but the amount of adsorbed MO continues to increase, probably due to the formation of a second layer of adsorbate.
In addition, the applicant also compares the methyl orange adsorption effect of the modified montmorillonite in the example 2 with that of the sodium-based montmorillonite and that of the modified montmorillonite in the comparative example 1, and the specific method is the same as the methyl orange adsorption experiment except that the methyl orange concentration is 40 mg/L. As can be seen from fig. 4, the color of the methyl orange solution after OMt adsorption was lighter than Na-Mt, while the color of the methyl orange solution after DMt adsorption was lighter than OMt and colorless; DMt the adsorption capacity of methyl orange is much higher than that of Na-Mt and OMt, which shows that the gemini surfactant is more beneficial to the improvement of montmorillonite adsorption performance than the traditional single-chain surfactant.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A preparation method of modified montmorillonite is characterized by comprising the following steps: the preparation method comprises the following steps: dispersing sodium-based montmorillonite in water, slowly adding a dioctadecyl tetrahydroxyethyl dibromopropane diammonium water solution to obtain a suspension, then placing the suspension in a microwave reactor, setting microwave power, reaction temperature and reaction time, collecting precipitates after the reaction is finished, and then washing the precipitates with water until the washed solution and AgNO are mixed3And (3) the solution reaction does not detect bromide ions, and then drying the washed precipitate to obtain a dried precipitate, namely the modified montmorillonite.
2. The method of claim 1, wherein: the dosage of the dioctadecyl tetrahydroxy ethyl dibromo diammonium is more than 0.5 times of the cation exchange capacity of the sodium montmorillonite.
3. The method of claim 1, wherein: the dosage of the dioctadecyl tetrahydroxyethyl dibromopropane diammonium is 1.0 to 1.5 times of the cation exchange capacity of the sodium-based montmorillonite.
4. The method of claim 1, wherein: the microwave power is 800W, the reaction temperature is 85 ℃, and the reaction time is 1 h.
5. The method of claim 1, wherein: in the raw materials of the reaction, the ratio of the sodium montmorillonite to the total water is 1g:37.5 mL.
6. The method of claim 1, wherein: the sodium montmorillonite is directly used for preparing the modified montmorillonite without purification treatment after purchase.
7. A modified montmorillonite prepared by the preparation method of any one of claims 1-6.
8. The use of a modified montmorillonite prepared by the method of any one of claims 1-6, wherein: the modified montmorillonite is used for removing organic pollutants in wastewater.
9. Use according to claim 8, characterized in that: the organic contaminants include methyl orange.
10. Use according to claim 9, characterized in that: the adsorption quantity of the modified montmorillonite to methyl orange is up to more than 200 mg/g.
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