CN103831134A - Modified bentonite solid phase catalyst preparation method and application thereof - Google Patents
Modified bentonite solid phase catalyst preparation method and application thereof Download PDFInfo
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- CN103831134A CN103831134A CN201410107435.6A CN201410107435A CN103831134A CN 103831134 A CN103831134 A CN 103831134A CN 201410107435 A CN201410107435 A CN 201410107435A CN 103831134 A CN103831134 A CN 103831134A
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Abstract
The invention provides a modified bentonite solid phase catalyst preparation method and an application thereof. The method comprises the step of loading excessive Fe (3+) saturated modified bentonite by adopting a humic acid, wherein the modified bentonite is utilized as a solid phase catalyst and is used for carrying out photocatalytic degradation on polycyclic aromatic hydrocarbon; the modified bentonite has a large adsorption capacity on the polycyclic aromatic hydrocarbon, and the degradation efficiency is high. The experiment proves that the modified bentonite solid phase catalyst prepared by the invention has good adsorption action on the polycyclic aromatic hydrocarbon, and the polycyclic aromatic hydrocarbon can be degraded in an efficient manner. The modified bentonite solid phase catalyst preparation method and the application thereof provided by the invention have the advantages that the preparation technology is simple, the cost is low, and the modified bentonite solid phase catalyst is used for managing the polycyclic aromatic hydrocarbon contaminated soil and has a certain practical application value.
Description
Technical field
The invention belongs to the technical field of modified alta-mud, particularly a kind of modified alta-mud type solid-phase photocatalyst and preparation method thereof.
Background technology
Bentonite is a kind of clay mineral take imvite as main component, abundant at China's reserves, cheap.Bentonite is the silicate clay mineral that is sandwiched in 2: 1 type layer structures of aluminium (magnesium) oxygen (hydroxyl) octahedral sheet formation therebetween by two-layer tetrahedral si-o film and one deck, has larger specific area and certain cation exchange capacity (CEC).In recent years, Fe
3+-bentonite has obtained research widely as photocatalyst for degrading organic pollution.
Humic acid is a kind of natural polymer organic matter; be difficult to be biodegradable, but it contains chromophoric macromolecular compound as one, photochemical reaction faster can occur under ultra-violet radiation or natural lighting; it can become chemical energy by light energy conversion on the one hand, causes the degraded of self; It,, as sensitiser absorption photon, is transferred to material around by energy on the other hand, or light activated humic acid produces reactive intermediate and other materials react, and causes other material generation chemical changes.
With humic acid to Fe
3+-bentonite carries out intercalation modifying, and on the one hand, humic acid contains abundant carboxyl, phenolic hydroxyl group isoreactivity functional group, the absorption that can improve organic pollution, humic acid is as photosensitizer on the other hand, can improve the visible light-responded of catalyst, promote the carrying out of chemical reaction.Therefore, humic acid modified bentonite can obtain higher photocatalysis effect as solid-phase photocatalyst.
Summary of the invention
The object of the invention is to, a kind of modified alta-mud type solid-phase photocatalyst preparation method and its usage is provided, the method adopts humic acid to passing through Fe
3+saturated modified alta-mud carries out load and makes, and the present invention combines the photoactivate characteristic of bentonitic advantageous property and humic acid, has prepared a kind of modified alta-mud type solid-phase photocatalyst.Because humic acid enters bentonitic interlayer, increased original soil interlamellar spacing, and due to the carboxyl of humic acid, the functional groups such as phenolic hydroxyl group make the adsorption capacity of organic pollution polycyclic aromatic hydrocarbon increase, and are easier to the carrying out of degradation reaction.Experiment showed, the modified alta-mud type solid-phase photocatalyst that uses the method for the invention to obtain, the degraded of polycyclic aromatic hydrocarbon is accelerated, in 8 hours, realize degradable to polycyclic aromatic hydrocarbon.
A kind of modified alta-mud type solid-phase photocatalyst preparation method and its usage of the present invention, the method adopts humic acid to passing through Fe
3+saturated modified alta-mud carries out load and makes, and concrete operations follow these steps to carry out:
A, Fe
3+-saturated bentonitic preparation: the FeCl that bentonite is joined to 0.1mol/L
3in solution, put into 25 ℃ of constant temperature of shaking table temperature, vibration 8h, the centrifugal 10min of 3000rpm, abandoning supernatant, adds the FeCl of 200mL 0.1mol/L again
3solution, vibration 8h, the centrifugal 10min of 3000rpm, repeats 4 times, then cleans with distilled water, until detect not chloride ion-containing with silver nitrate in supernatant;
B, humic acid modified bentonitic preparation: by the Fe preparing in step a
3+in-saturated bentonite slurry, add humic acid or fulvic acid, stir, 25 ℃ of constant temperature of shaking table temperature, vibration 8-12 hour, under 3000rpm centrifugal 5 minutes, abandoning supernatant, until centrifugal rear supernatant is light brown, then put into 50 ℃ of oven dry of oven temperature by washed with de-ionized water, grind, cross 80 mesh sieves, obtain modified alta-mud type solid-phase photocatalyst.
In step b, the addition of humic acid or fulvic acid is humic acid/bentonite=0.10 mg/g-0.65mg/g, fulvic acid/bentonite=0.12 mg/g-0.70mg/g.
The modified alta-mud type solid-phase photocatalyst that described method obtains is in the purposes of preparing degradation of contaminant polycyclic aromatic hydrocarbon under visible ray.
A kind of modified alta-mud type solid-phase photocatalyst preparation method and its usage of the present invention, obtain the analysis to degrading polycyclic aromatic hydrocarbons performance under visible ray of modified alta-mud type solid-phase photocatalyst by the method: 50mg anthracene is dissolved in and in 50mL acetone, joins to obtain the anthracene solution of 1mg/mL, in the modified alta-mud that 1g is obtained, add the anthracene solution of 1mL 1mg/mL, be placed in fume hood, natural air drying.The method of utilizing the people such as Balmer to propose, puts the PTFE packing ring that an internal diameter is 4cm at two glass plate centers, pollution clay is put in packing ring and shakes up, and glass plate surrounding is clamped with clip, and glass plate is 5cm from the distance of lamp, is put in illumination degrading anthracene under xenon lamp.
The present invention combines the photoactivate characteristic of bentonitic advantageous property and humic acid, has prepared a kind of modified alta-mud type solid-phase photocatalyst.Because humic acid enters bentonitic interlayer, increased original soil interlamellar spacing, and due to the carboxyl of humic acid, the functional groups such as phenolic hydroxyl group make the adsorption capacity of organic pollution polycyclic aromatic hydrocarbon increase, and are easier to the carrying out of degradation reaction.Experiment showed, and use modified alta-mud type solid-phase photocatalyst of the present invention, the degraded of polycyclic aromatic hydrocarbon is accelerated, in 8 hours, realize degradable to polycyclic aromatic hydrocarbon.
Accompanying drawing explanation
Fig. 1 is SEM figure of the present invention, the wherein unmodified bentonite of a, b humic acid (HA) modified alta-mud, c fulvic acid (FA) modified alta-mud;
Fig. 2 is the degraded figure of humic acid of the present invention (HA) modified alta-mud to polycyclic aromatic hydrocarbon, wherein ■ embodiment 1, ● embodiment 2, ▲ embodiment 3;
Fig. 3 is the degraded of fulvic acid of the present invention (FA) modified alta-mud to polycyclic aromatic hydrocarbon, wherein ● embodiment 4, and ■ embodiment 5, ▲ embodiment 6.
The specific embodiment
In order to understand better the present invention, further illustrate by following examples;
Embodiment 1:
Preparation Fe
3+-bentonite: the FeCl that 20g bentonite is joined to 200 mL 0.1mol/L
3in solution, put into 25 ℃ of constant temperature of shaking table temperature, vibration 8h, the centrifugal 10min of 3000rpm, abandoning supernatant, adds the FeCl of 200mL 0.1mol/L again
3solution, vibration 8h, the centrifugal 10min of 3000rpm, repeats 4 times successively, with distilled water cleaning, the Fe obtaining
3+-saturated bentonite slurry;
Prepare humic acid modified bentonite: by the Fe obtaining
3+in-saturated bentonite slurry, add the humic acid of 4.3 mg, stir, shaking table vibration 8 hours, the centrifugal 5min of 3000rpm, abandoning supernatant, by washed with de-ionized water until centrifugal rear supernatant is light brown, put into baking oven, temperature 50 C is dried again, and grinds, cross 80 mesh sieves, obtain modified alta-mud type photochemical catalyst;
Modified alta-mud type photochemical catalyst analysis to degrading polycyclic aromatic hydrocarbons performance under visible ray: 50mg anthracene is dissolved in and joins to obtain the anthracene solution of 1mg/mL in 50mL acetone, 1mL 1mg/mL anthracene solution will be added in the modified alta-mud type photochemical catalyst obtaining, be placed in fume hood, natural air drying, the method of utilizing the people such as Balmer to propose, put the PTFE packing ring that an internal diameter is 4cm at two glass plate centers, pollution clay is put in packing ring and is shaken up, glass plate surrounding is clamped with clip, glass plate is 5cm from the distance of lamp, being put in illumination under xenon lamp is degrading polyaromatic hydrocarbon, degradation effect is shown in accompanying drawing 2, illumination realization in 8 hours is degradable to polycyclic aromatic hydrocarbon.
Embodiment 2:
Preparation Fe
3+-bentonite: the FeCl that 20g bentonite is joined to 200 mL 0.1mol/L
3in solution, put into 25 ℃ of constant temperature of shaking table temperature, vibration 12h, centrifugal 10min under 3000rpm, abandoning supernatant, adds the FeCl of 200mL 0.1mol/L again
3solution, vibration 8h, centrifugal 10min under 3000rpm, repeats 4 times successively, with distilled water cleaning, the Fe obtaining
3+-saturated bentonite slurry;
Prepare humic acid modified bentonite: by the Fe obtaining
3+in-saturated bentonite slurry, add the humic acid of 2.0 mg, stir, shaking table vibration 12 hours, the centrifugal 5min of 3000rpm, abandoning supernatant, by washed with de-ionized water until centrifugal rear supernatant is light brown, put into again 50 ℃ of oven dry of oven temperature, grind, cross 80 mesh sieves, obtain modified alta-mud type photochemical catalyst;
Modified alta-mud type photochemical catalyst analysis to degrading polycyclic aromatic hydrocarbons performance under visible ray: 50mg anthracene is dissolved in and joins to obtain the anthracene solution of 1mg/mL in 50mL acetone, the anthracene solution of 1mL 1mg/mL will be added in the modified alta-mud type photochemical catalyst obtaining, be placed in fume hood, natural air drying, the method of utilizing the people such as Balmer to propose, put the PTFE packing ring that an internal diameter is 4cm at two glass plate centers, pollution clay is put in packing ring and is shaken up, glass plate surrounding is clamped with clip, glass plate is 5cm from the distance of lamp, being put in illumination under xenon lamp is degrading polyaromatic hydrocarbon, degradation effect is shown in accompanying drawing 2, illumination realization in 8 hours is degradable to polycyclic aromatic hydrocarbon.
Embodiment 3:
Preparation Fe
3+-bentonite: the FeCl that 20g bentonite is joined to 200 mL 0.1mol/L
3in solution, put into 25 ℃ of constant temperature of shaking table temperature, vibration 8h, the centrifugal 10min of 3000rpm, abandoning supernatant, adds the FeCl of 200mL 0.1mol/L again
3solution, vibration 8h, the centrifugal 10min of 3000rpm, repeats 4 times successively, with distilled water cleaning, the Fe obtaining
3+-saturated bentonite slurry;
Prepare humic acid modified bentonite: by the Fe obtaining
3+in-saturated bentonite slurry, add the humic acid of 13mg, stir, shaking table vibration 8 hours, the centrifugal 5min of 3000rpm, abandoning supernatant, by washed with de-ionized water until centrifugal rear supernatant is light brown, put into baking oven, temperature 50 C is dried again, and grinds, cross 80 mesh sieves, obtain modified alta-mud type photochemical catalyst;
Modified alta-mud type photochemical catalyst analysis to degrading polycyclic aromatic hydrocarbons performance under visible ray: 50mg anthracene is dissolved in and joins to obtain the anthracene solution of 1mg/mL in 50mL acetone, 1mL 1mg/mL anthracene solution will be added in the modified alta-mud type photochemical catalyst obtaining, be placed in fume hood, natural air drying, the method of utilizing the people such as Balmer to propose, put the PTFE packing ring that an internal diameter is 4cm at two glass plate centers, pollution clay is put in packing ring and is shaken up, glass plate surrounding is clamped with clip, glass plate is 5cm from the distance of lamp, being put in illumination under xenon lamp is degrading polyaromatic hydrocarbon, degradation effect is shown in accompanying drawing 2, illumination reaches 0.1mg/g to the degraded of polycyclic aromatic hydrocarbon in 8 hours.
Embodiment 4:
Preparation Fe
3+-bentonite: the FeCl that 20g bentonite is joined to 200 mL 0.1mol/L
3in solution, put into 25 ℃ of constant temperature of shaking table temperature, vibration 8h, centrifugal 10min under 3000rpm, abandoning supernatant, adds the FeCl of 200mL 0.1M again
3solution, vibration 8h, centrifugal 10min under 3000rpm, repeats 4 times successively, with distilled water cleaning, the Fe obtaining
3+-saturated bentonite slurry;
Prepare humic acid modified bentonite: by the Fe obtaining
3+in-saturated bentonite slurry, add the fulvic acid of 5mg, stir, shaking table vibration 12 hours, the centrifugal 5min of 3000rpm, abandoning supernatant, by washed with de-ionized water until centrifugal rear supernatant is light brown, put into again 50 ℃ of oven dry of oven temperature, grind, cross 80 mesh sieves, obtain modified alta-mud type photochemical catalyst;
Modified alta-mud type photochemical catalyst analysis to degrading polycyclic aromatic hydrocarbons performance under visible ray: 50mg anthracene is dissolved in and joins to obtain the anthracene solution of 1mg/mL in 50mL acetone, the anthracene solution of 1mL 1mg/mL will be added in the modified alta-mud type photochemical catalyst obtaining, be placed in fume hood, natural air drying, the method of utilizing the people such as Balmer to propose, put the PTFE packing ring that an internal diameter is 4cm at two glass plate centers, pollution clay is put in packing ring and is shaken up, glass plate surrounding is clamped with clip, glass plate is 5cm from the distance of lamp, being put in illumination under xenon lamp is degrading polyaromatic hydrocarbon, degradation effect is shown in accompanying drawing 3, illumination reaches 0.01mg/g to the degraded of polycyclic aromatic hydrocarbon in 4 hours.
Embodiment 5:
Preparation Fe
3+-bentonite: the FeCl that 20g bentonite is joined to 200 mL 0.1mol/L
3in solution, put into 25 ℃ of constant temperature of shaking table temperature, vibration 8h, centrifugal 10min under 3000rpm, abandoning supernatant, adds the FeCl of 200mL 0.1mol/L again
3solution, vibration 8h, centrifugal 10min under 3000rpm, repeats 4 times successively, with distilled water cleaning, Fe obtained above
3+-saturated bentonite slurry;
Prepare humic acid modified bentonite: by the Fe obtaining
3+in-saturated bentonite slurry, add the fulvic acid of 2.4mg, stir, shaking table vibration 12 hours, the centrifugal 5min of 3000rpm, abandoning supernatant, by washed with de-ionized water until centrifugal rear supernatant is light brown, put into baking oven, temperature 50 C is dried again, and grinds, cross 80 mesh sieves, obtain modified alta-mud type photochemical catalyst;
Modified alta-mud type photochemical catalyst analysis to degrading polycyclic aromatic hydrocarbons performance under visible ray: 50mg anthracene is dissolved in and joins to obtain the anthracene solution of 1mg/mL in 50mL acetone, the anthracene solution of 1mL 1mg/mL will be added in the modified alta-mud type photochemical catalyst obtaining, be placed in fume hood, natural air drying, the method of utilizing the people such as Balmer to propose, put the PTFE packing ring that an internal diameter is 4cm at two glass plate centers, pollution clay is put in packing ring and is shaken up, glass plate surrounding is clamped with clip, glass plate is 5cm from the distance of lamp, being put in illumination under xenon lamp is degrading polyaromatic hydrocarbon, degradation effect is shown in accompanying drawing 3, illumination can realize degradable to polycyclic aromatic hydrocarbon for 8 hours.
Embodiment 6:
Preparation Fe
3+-bentonite: the FeCl that 20g bentonite is joined to 200 mL 0.1mol/L
3in solution, put into 25 ℃ of constant temperature of shaking table temperature, vibration 8h, centrifugal 10min under 3000rpm, abandoning supernatant, adds the FeCl of 200mL 0.1mol/L again
3solution, vibration 8h, centrifugal 10min under 3000rpm, repeats 4 times successively, with distilled water cleaning, Fe obtained above
3+-saturated bentonite slurry;
Prepare humic acid modified bentonite: by the Fe obtaining
3+in-saturated bentonite slurry, add the fulvic acid of 14mg, stir, shaking table vibration 12 hours, the centrifugal 5min of 3000rpm, abandoning supernatant, by washed with de-ionized water until centrifugal rear supernatant is light brown, put into baking oven, temperature 50 C is dried again, and grinds, cross 80 mesh sieves, obtain modified alta-mud type photochemical catalyst;
Modified alta-mud type photochemical catalyst analysis to degrading polycyclic aromatic hydrocarbons performance under visible ray: 50mg anthracene is dissolved in and joins to obtain the anthracene solution of 1mg/mL in 50mL acetone, the anthracene solution of 1mL 1mg/mL will be added in the modified alta-mud type photochemical catalyst obtaining, be placed in fume hood, natural air drying, the method of utilizing the people such as Balmer to propose, put the PTFE packing ring that an internal diameter is 4cm at two glass plate centers, pollution clay is put in packing ring and is shaken up, glass plate surrounding is clamped with clip, glass plate is 5cm from the distance of lamp, being put in illumination under xenon lamp is degrading polyaromatic hydrocarbon, degradation effect is shown in accompanying drawing 3, illumination can realize degradable to polycyclic aromatic hydrocarbon for 8 hours.
Claims (3)
1. a modified alta-mud type solid-phase photocatalyst preparation method, is characterized in that adopting humic acid to passing through Fe
3+saturated modified alta-mud carries out load and makes, and concrete operations follow these steps to carry out:
A, Fe
3+-saturated bentonitic preparation: the FeCl that bentonite is joined to 0.1mol/L
3in solution, put into 25 ℃ of constant temperature of shaking table temperature, vibration 8h, the centrifugal 10min of 3000rpm, abandoning supernatant, adds the FeCl of 200mL 0.1mol/L again
3solution, vibration 8h, the centrifugal 10min of 3000rpm, repeats 4 times, then cleans with distilled water, until detect not chloride ion-containing with silver nitrate in supernatant;
B, humic acid modified bentonitic preparation: by the Fe preparing in step a
3+in-saturated bentonite slurry, add humic acid or fulvic acid, stir, 25 ℃ of constant temperature of shaking table temperature, vibration 8-12 hour, under 3000rpm centrifugal 5 minutes, abandoning supernatant, until centrifugal rear supernatant is light brown, then put into 50 ℃ of oven dry of oven temperature by washed with de-ionized water, grind, cross 80 mesh sieves, obtain modified alta-mud type solid-phase photocatalyst.
2. method as claimed in claim 1, is characterized in that the addition of humic acid in step b or fulvic acid is humic acid/bentonite=0.10 mg/g-0.65mg/g, fulvic acid/bentonite=0.12 mg/g-0.70mg/g.
3. the modified alta-mud type solid-phase photocatalyst that method obtains is as claimed in claim 1 in the purposes of preparing degradation of contaminant polycyclic aromatic hydrocarbon under visible ray.
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| CN107511138A (en) * | 2017-09-22 | 2017-12-26 | 湖南化工研究院有限公司 | Flocculation adsorption agent for landfill leachate treatment and preparation method thereof |
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| CN102407117A (en) * | 2011-11-14 | 2012-04-11 | 江苏星晨环保集团有限公司 | Photocatalysis water-treating material as well as preparation method and application thereof |
| CN102423696A (en) * | 2011-09-02 | 2012-04-25 | 中国科学院新疆理化技术研究所 | Preparation method for humic acid-modified nano-ferroferric oxide, and use thereof |
| GR1007843B (en) * | 2011-12-13 | 2013-02-27 | Ιωαννης Γεωργιου Δεληγιαννακης | Absorbent for removing phosphorous and ammonia |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102423696A (en) * | 2011-09-02 | 2012-04-25 | 中国科学院新疆理化技术研究所 | Preparation method for humic acid-modified nano-ferroferric oxide, and use thereof |
| CN102407117A (en) * | 2011-11-14 | 2012-04-11 | 江苏星晨环保集团有限公司 | Photocatalysis water-treating material as well as preparation method and application thereof |
| GR1007843B (en) * | 2011-12-13 | 2013-02-27 | Ιωαννης Γεωργιου Δεληγιαννακης | Absorbent for removing phosphorous and ammonia |
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| HANZHONG JIA ET.AL.: "Visible light photodegradation of phenanthrene catalyzed by Fe(III)-smectite: Role of soil organic matter", 《JOURNAL OF HAZARDOUS MATERIALS》, vol. 256257, 16 April 2013 (2013-04-16) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107511138A (en) * | 2017-09-22 | 2017-12-26 | 湖南化工研究院有限公司 | Flocculation adsorption agent for landfill leachate treatment and preparation method thereof |
| CN107511138B (en) * | 2017-09-22 | 2020-09-11 | 湖南化工研究院有限公司 | Flocculation adsorbent for landfill leachate treatment and preparation method thereof |
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Application publication date: 20140604 |