CN104258816B - The preparation method of the exfoliated Nano composite material of montmorillonite of a kind of magnetic for wastewater treatment - Google Patents
The preparation method of the exfoliated Nano composite material of montmorillonite of a kind of magnetic for wastewater treatment Download PDFInfo
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- CN104258816B CN104258816B CN201410576782.3A CN201410576782A CN104258816B CN 104258816 B CN104258816 B CN 104258816B CN 201410576782 A CN201410576782 A CN 201410576782A CN 104258816 B CN104258816 B CN 104258816B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
Abstract
The invention discloses the preparation method of the exfoliated Nano composite material of montmorillonite of a kind of magnetic for wastewater treatment, belong to Nano-composite materials technical field.The method is by carboxyls a large amount of in imvite finishing, in-situ chemical reaction is adopted to be introduced by magnetic nano-particle between cheating engaging layer and to obtain exfoliated structure, in conjunction with the Magneto separate performance of tri-iron tetroxide and the carboxyl modified imvite high characterization of adsorption to organic cation dye and heavy metal ion, obtaining can Magneto separate and the exfoliated montmorillonite-based nano composite adsorbing material of the magnetic of high adsorption capacity.Preparation technology of the present invention is simple, condition is controlled, the obtained exfoliated Nano composite material of montmorillonite of magnetic is with low cost, be easy to be separated and have high characterization of adsorption and excellent environment complimentary nature, the adsorption efficiency to organic cation dye and heavy metal ion and adsorption capacity can be significantly improved, be applicable to the fields such as Industrial Wastewater Treatment.
Description
Technical field
The invention belongs to Nano-composite materials technical field, be specifically related to the preparation method of the exfoliated Nano composite material of montmorillonite of a kind of magnetic for wastewater treatment.
Background technology
Along with the development of modern industrial or agricultural, people produce and in life, a large amount of poisonous and hazardous material enters water body, and the mankind depend on for existence and suffer serious destruction with the water environment developed.Because China's water resource is relatively deficient, the effect of wastewater processing technology in production and life is also increasing.
The features such as organic dye waste water tool concentration is high, colourity is dark, change of water quality fluctuation is large and biodegradability is poor are very unmanageable class industrial wastewaters.The dye of positive ion contains very complicated aromatic group and is difficult to biodegradation decolouring.Though electronation or anaerobic bio-treated can make the azo reduction in dyestuff be that amido decolours, the amido class intermediate product toxicity ratio produced is comparatively large, and partial reduction products easily returns look under aerobic conditions.Therefore, the process of cationic dye wastewater especially comes into one's own.
Heavy metal wastewater thereby is one equally needs the urgent pollution problem solved.Because heavy metal contaminants is difficult to be decomposed and destroy, once enter environment will cause permanent pollution, common heavy metal containing wastewater treatment technology comprises: the physics and chemistry methods such as chemical precipitation method, oxidation-reduction method, ion-exchange treatment method, cohesion-flocculence, absorption method, membrane separation process.
Absorption method utilizes porous solid and waste water, utilizes the surface-active of adsorbent, by Wastewater Dyes or adsorption of metal ions and concentrate in its surface, reach the object of purifying waste water.Current sorbing material is activated carbon, molecular sieve and ion exchange resin etc. mainly, but these materials exist or adsorption efficiency is low, capacity is little or the scope of application is little, reproducibility is poor, high in cost of production defect, and be not easily separated from waste water and cause secondary pollution, current people attempt research and development nano composite adsorption material to improve adsorption efficiency further and to reduce costs.
Summary of the invention
The present invention is directed to imvite in prior art and reclaim the problems such as difficult, adsorption efficiency is low as sorbing material, the preparation method of the exfoliated Nano composite material of montmorillonite of a kind of magnetic is provided; The exfoliated Nano composite material of montmorillonite absorption heavy metal ions in wastewater of magnetic prepared by the inventive method and the dye of positive ion, have excellent absorption property.
The preparation method of the exfoliated Nano composite material of montmorillonite of a kind of magnetic for wastewater treatment provided by the present invention, concrete steps are as follows:
(1) preparation of modifier solution: methylacryoyloxyethyl-3-ammonio methacrylate, methacrylic acid and ammonium persulfate are dissolved in deionized water, wherein the gross mass of methylacryoyloxyethyl-3-ammonio methacrylate and methacrylic acid accounts for 5% of solution, the mol ratio of methylacryoyloxyethyl-3-ammonio methacrylate and methacrylic acid is 1:10, the quality of ammonium persulfate accounts for 0.05% of solution, logical N
2heating water bath to 70 DEG C after stirring 30min, reaction 7h, obtains modifier solution;
(2) preparation of organic modification montmonrillonite: be dispersed in water by sodium-based montmorillonite, obtains sodium-based montmorillonite solution, is 2 ~ 5 by hydrochloric acid conditioning solution pH value, wherein: the quality of sodium-based montmorillonite accounts for 0.5 ~ 2% of solution; The modifier solution that step (1) obtains is joined in above-mentioned sodium-based montmorillonite solution, wherein: the mass ratio of modifier and imvite is 0.2 ~ 0.8:1, is uniformly mixed 3 ~ 4h, carry out filtering and washing, obtain organic modification montmonrillonite;
(3) preparation of the exfoliated Nano composite material of montmorillonite of magnetic: the organic modification montmonrillonite that step (2) obtains is dispersed in water, obtain organic modification montmonrillonite dispersion liquid, ferric trichloride and frerrous chloride are added in this dispersion liquid, wherein: the quality of organic modification montmonrillonite accounts for 0.2% ~ 0.5% of solution, the mol ratio of ferric trichloride and frerrous chloride is 1.5:1, and the mass ratio of organic modification montmonrillonite and ferric trichloride is 0.4 ~ 1.0:1; Logical N
2after stirring 30min, add ammonia spirit, solution ph controlled 10 ~ 11 at 80 DEG C, after stirring reaction 2h, after cooling, filtration, washing, drying, namely grinding distribution obtains the exfoliated Nano composite material of montmorillonite of magnetic.
Compared with prior art, beneficial effect of the present invention is:
1, the present invention adopts amphiphilic polymers to carry out modification to sodium-based montmorillonite, introduces the interlamellar spacing that organic polymer improves imvite on the one hand by modification between cheating engaging layer; On the other hand introduce a large amount of carboxyls, improve the adsorption capacity of nano composite material to the dye of positive ion and heavy metal ion.
2, the present invention adopts in-situ chemical reaction magnetic nano-particle introduced amphiphilic polymers modified montmorillonoid interlayer and then obtain exfoliated structure, in conjunction with the Magneto separate performance of tri-iron tetroxide and the amphiphilic polymers modified montmorillonoid high characterization of adsorption to organic cation dye and heavy metal ion, obtaining can Magneto separate and the exfoliated montmorillonite-based nano composite adsorbing material of the magnetic of high adsorption capacity.
3, preparation technology of the present invention is simple, condition is controlled, the obtained exfoliated Nano composite material of montmorillonite of magnetic is with low cost, be easy to be separated and have high characterization of adsorption and excellent environment complimentary nature, the adsorption efficiency to organic cation dye and heavy metal ion and adsorption capacity can be significantly improved, be applicable to the fields such as Industrial Wastewater Treatment.
Accompanying drawing explanation
Fig. 1 is the small angle X-ray diffraction spectrogram of the exfoliated Nano composite material of montmorillonite (c) of sodium-based montmorillonite (a), organic modification montmonrillonite (b) and magnetic;
As can be seen from Figure 1, the interlamellar spacing of imvite is increased to 1.53nm from 1.32nm, show the successful modification of imvite, magnetic Nano composite material of montmorillonite does not have diffraction maximum within the scope of 1 ° ~ 10 °, indicates magnetic Nano composite material of montmorillonite and has exfoliated structure.
Fig. 2 is Fe
3o
4the wide-angle X-ray diffraction curve of (a) and the exfoliated Nano composite material of montmorillonite (b) of magnetic;
As can be seen from Figure 2, prepared magnetic Nano composite material of montmorillonite contains the characteristic peak of tri-iron tetroxide, shows the successful preparation of the exfoliated Nano composite material of montmorillonite of magnetic.
Detailed description of the invention
Below in conjunction with specific embodiment in detail the present invention is described in detail, but the present invention is not limited to following embodiment.
Embodiment 1
Being scattered in the distilled water of 600mL by 3.0g sodium-based montmorillonite, is 3 by hydrochloric acid conditioning solution pH value, then joins in above-mentioned solution by 2.4g modifier, mix and blend 4h, filters and washing, obtains organic modification montmonrillonite.Get organic modification montmonrillonite 1.66g to be scattered in the distilled water of 700mL and to add 2.69g Iron(III) chloride hexahydrate and 1.32g Iron dichloride tetrahydrate, logical N
2after stirring 30min, add ammonia spirit, solution ph controlled 10 ~ 11 at 80 DEG C, after stirring reaction 2h, cooling, filtration, washing, after dry, namely grinding distribution obtains the exfoliated Nano composite material of montmorillonite of magnetic.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 100mL methylene blue solution of 60mg/L, and after absorption 6h, after magnet separating adsorbent, recording methylene blue concentration is 0.98mg/L, and adsorption rate is 98.4%.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 10mL rhodamine liquor of 50mg/L, and after absorption 6h, after magnet separating adsorbent, recording rhodamine concentration is 4.43mg/L, and adsorption rate is 91.1%.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 100mL nickel ion solution of 10mg/L, and after absorption 6h, after magnet separating adsorbent, recording nickel ion concentration is 2.93mg/L, and adsorption rate is 70.7%.
Embodiment 2
Being scattered in the distilled water of 300mL by 3.0g sodium-based montmorillonite, is 3 by hydrochloric acid conditioning solution pH value, then joins in above-mentioned solution by 1.2g modifier, mix and blend 4h, filters and washing, obtains organic modification montmonrillonite.Get organic modification montmonrillonite 2.32g to be scattered in the distilled water of 700mL and to add 2.69g Iron(III) chloride hexahydrate and 1.32g Iron dichloride tetrahydrate, logical N
2after stirring 30min, add ammonia spirit, solution ph controlled 10 ~ 11 at 80 DEG C, after stirring reaction 2h, cooling, filtration, washing, after dry, namely grinding distribution obtains the exfoliated Nano composite material of montmorillonite of magnetic.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 100mL methylene blue solution of 60mg/L, and after absorption 6h, after magnet separating adsorbent, recording methylene blue concentration is 0.12mg/L, and adsorption rate is 99.8%.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 100mL rhodamine liquor of 50mg/L, and after absorption 6h, after magnet separating adsorbent, recording rhodamine concentration is 2.32mg/L, and adsorption rate is 95.3%.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 10mL nickel ion solution of 10mg/L, and after absorption 6h, after magnet separating adsorbent, recording nickel ion concentration is 1.54mg/L, and adsorption rate is 84.6%.
Embodiment 3
Being scattered in the distilled water of 300mL by 4.5g sodium-based montmorillonite, is 3 by hydrochloric acid conditioning solution pH value, then joins in above-mentioned solution by 0.9g modifier, mix and blend 4h, filters and washing, obtains organic modification montmonrillonite.Get organic modification montmonrillonite 2.69g to be scattered in the distilled water of 700mL and to add 2.69g Iron(III) chloride hexahydrate and 1.32g Iron dichloride tetrahydrate, logical N
2after stirring 30min, add ammonia spirit, solution ph controlled 10 ~ 11 at 80 DEG C, after stirring reaction 2h, cooling, filtration, washing, after dry, namely grinding distribution obtains the exfoliated Nano composite material of montmorillonite of magnetic.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 100mL methylene blue solution of 60mg/L, and after absorption 6h, after magnet separating adsorbent, recording methylene blue concentration is 0.76mg/L, and adsorption rate is 98.7%.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 10mL rhodamine liquor of 50mg/L, and after absorption 6h, after magnet separating adsorbent, recording rhodamine concentration is 3.21mg/L, and adsorption rate is 93.6%.
Get the above-mentioned nano composite material of 0.10g, dropping into initial concentration is in the 10mL nickel ion solution of 10mg/L, and after absorption 6h, after magnet separating adsorbent, recording nickel ion concentration is 3.42mg/L, and adsorption rate is 65.8%.
Claims (1)
1., for a preparation method for the exfoliated Nano composite material of montmorillonite of magnetic of wastewater treatment, it is characterized in that, the method concrete steps are as follows:
(1) preparation of modifier solution: methylacryoyloxyethyl-3-ammonio methacrylate, methacrylic acid and ammonium persulfate are dissolved in deionized water, wherein the gross mass of methylacryoyloxyethyl-3-ammonio methacrylate and methacrylic acid accounts for 5% of solution, the mol ratio of methylacryoyloxyethyl-3-ammonio methacrylate and methacrylic acid is 1:10, the quality of ammonium persulfate accounts for 0.05% of solution, logical N
2heating water bath to 70 DEG C after stirring 30min, reaction 7h, obtains modifier solution;
(2) preparation of organic modification montmonrillonite: be dispersed in water by sodium-based montmorillonite, obtains sodium-based montmorillonite solution, is 2 ~ 5 by hydrochloric acid conditioning solution pH value, wherein: the quality of sodium-based montmorillonite accounts for 0.5 ~ 2% of solution; The modifier solution that step (1) obtains is joined in above-mentioned sodium-based montmorillonite solution, wherein: the mass ratio of modifier and imvite is 0.2 ~ 0.8:1, is uniformly mixed 3 ~ 4h, carry out filtering and washing, obtain organic modification montmonrillonite;
(3) preparation of the exfoliated Nano composite material of montmorillonite of magnetic: the organic modification montmonrillonite that step (2) obtains is dispersed in water, obtain organic modification montmonrillonite dispersion liquid, ferric trichloride and frerrous chloride are added in this dispersion liquid, wherein: the quality of organic modification montmonrillonite accounts for 0.2% ~ 0.5% of solution, the mol ratio of ferric trichloride and frerrous chloride is 1.5:1, and the mass ratio of organic modification montmonrillonite and ferric trichloride is 0.4 ~ 1.0:1; Logical N
2after stirring 30min, add ammonia spirit, solution ph controlled 10 ~ 11 at 80 DEG C, after stirring reaction 2h, after cooling, filtration, washing, drying, namely grinding distribution obtains the exfoliated Nano composite material of montmorillonite of magnetic.
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| CN105203463B (en) * | 2015-09-10 | 2018-01-05 | 北京师范大学 | Visual inspection method based on polarized light microscope observing montmorillonite absorption lipid |
| CN105536752A (en) * | 2015-12-12 | 2016-05-04 | 常州大学 | Preparation method of magnetic montmorillonite composite granular adsorbent |
| CN109354778A (en) * | 2018-09-19 | 2019-02-19 | 安徽卧龙泵阀股份有限公司 | A kind of rubber packing material preparation method of the modified montmorillonoid containing nano-magnetic powder |
| CN110180497A (en) * | 2019-05-27 | 2019-08-30 | 广西壮族自治区农业科学院 | The preparation method of the magnetic material of methyl blue in a kind of absorption effluent |
| CN110813261A (en) * | 2019-11-22 | 2020-02-21 | 安徽工业大学 | Preparation method of magnetic chitosan/montmorillonite/humic acid composite microcapsule adsorption material for wastewater treatment |
| CN112390337B (en) * | 2020-10-30 | 2022-01-28 | 西南科技大学 | Preparation method of modified montmorillonite, product and application thereof |
| CN113908799B (en) * | 2021-12-14 | 2022-03-08 | 山东省科学院生态研究所(山东省科学院中日友好生物技术研究中心) | Preparation method and application of magnetic Prussian blue nano clay |
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| CN102886250A (en) * | 2012-10-23 | 2013-01-23 | 安徽工业大学 | Preparation method of polyaniline/montmorillonite composite adsorbent with sheet structure |
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| EP1138377A1 (en) * | 2000-03-27 | 2001-10-04 | Ceca S.A. | Method for separating molecules in gaseous phase by adsorption with solid agglomerated inorganic adsorbents having a narrow and calibrated distribution of mesopores |
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Effective date of registration: 20181025 Address after: 243000 18-, 169 Zhao Ming Road, Ma'anshan high tech Zone, Anhui. Patentee after: Ma'anshan Jian Ding Chemical Co., Ltd. Address before: 243002 59 Hudong Middle Road, Huashan District, Ma'anshan, Anhui Patentee before: Anhui University of Technology |