KR101526878B1 - Alginate bead impregnated bubble and photocatalyst method for the same - Google Patents
Alginate bead impregnated bubble and photocatalyst method for the same Download PDFInfo
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- KR101526878B1 KR101526878B1 KR1020140018937A KR20140018937A KR101526878B1 KR 101526878 B1 KR101526878 B1 KR 101526878B1 KR 1020140018937 A KR1020140018937 A KR 1020140018937A KR 20140018937 A KR20140018937 A KR 20140018937A KR 101526878 B1 KR101526878 B1 KR 101526878B1
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/34—Regenerating or reactivating
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Abstract
The present invention relates to a bubble and a photocatalyst-bearing alginate bead capable of regenerating by the photocatalytic reaction by improving bubble and photocatalyst loading on the alginate bead and maximizing the photocatalyst carried on the surface of the alginate bead, A method of manufacturing bubbles and photocatalyst-bearing alginate beads according to the present invention comprises the steps of preparing an alginate solution in which an adsorbent is dispersed and a solidifying solution in which a photocatalyst is dispersed, a step of irradiating the solidified solution with ultrasound And dropping the alginate solution into the solidifying solution by one drop to cure the alginate solution of each droplet to form an alginate bead, wherein the adsorbed material is immobilized on the alginate bead, and the alginate bead surface And the photocatalyst reacts with ultraviolet rays to cause a photocatalytic reaction to decompose organic contaminants adsorbed on the alginate beads.
Description
The present invention relates to a bubble and photocatalyst-bearing alginate beads and a method for producing the same. More particularly, the present invention relates to an alginate bead containing bubbles and a photocatalyst in an alginate bead and maximizing a photocatalyst carried on the alginate bead surface, And a photocatalyst-bearing alginate bead capable of being regenerated by a photocatalytic reaction, and a process for producing the same.
The wastewater contains poorly decomposable organic pollutants such as chlorophenols and the like. Such poorly decomposable organic pollutants are not removed by conventional biological wastewater treatment methods and are removed through the adsorbent.
(1997) 2154-7, 1997). In order to remove the degradable organic contaminants, a method using nanosilver iron (CB Wang, WX Zhang, Synthesizing nanoscale iron particles for rapid and complete dechlorination of TCE and PCBs, 2156), a method using a complex of calcium alginate and activated carbon powder (Jorda and Mijangos, Separation Science and Technology, Vol. 38, No. 8, 1851-1867).
On the other hand, regeneration of the adsorbent is required to reuse the adsorbent after removal of organic contaminants in the water. In the conventional case, the adsorbent is regenerated through high-temperature heat treatment or chemical chemical treatment. However, there is a problem that when the heat is applied at a high temperature, the adsorbent is deformed, and when the chemical chemical treatment is performed, the chemical remains in the adsorbent and acts as a new pollutant source.
SUMMARY OF THE INVENTION The present invention has been made in order to solve the above-mentioned problems, and it is an object of the present invention to provide a photocatalytic reaction device, which is capable of enhancing the removal characteristics of a decomposable organic contaminant by maximizing a photocatalyst carried on a surface of alginate beads by supporting bubbles and a photocatalyst on the alginate beads, And to provide a photocatalyst-bearing alginate bead capable of regenerating the alginate bead, and a method for producing the alginate bead.
According to another aspect of the present invention, there is provided a method of manufacturing a bubble and a photocatalyst-bearing alginate bead, the method including: preparing a solidification solution in which an adsorbent is dispersed and an alginate solution and a photocatalyst are dispersed; And dropping the alginate solution into the solidifying solution by one drop to cure the alginate solution of each droplet to form an alginate bead, wherein the adsorbed material is immobilized on the alginate bead, and the alginate bead surface And the photocatalyst reacts with ultraviolet rays to cause a photocatalytic reaction to decompose organic contaminants adsorbed on the alginate beads.
As the frequency of the ultrasonic waves increases, the size of bubbles carried on the alginate beads increases. The frequency of the ultrasonic waves is preferably adjusted in the range of 15 to 90 kHz.
The adsorbent is powder activated carbon, and the photocatalyst is any one of TiO 2 , ZnO, CdS, WO 3 , ZrO 2 and V 2 O 2 . Further, the solidifying solution is the aqueous solution of calcium chloride or the aqueous solution of barium chloride.
The alginate bead according to the present invention is characterized in that the alginate bead contains an adsorbent for removing organic contaminants in the alginate bead, a photocatalyst and a bubble for photocatalytic reaction by irradiation of ultraviolet rays, And the photocatalyst is immobilized on the substrate.
The bubbles and the photocatalyst-bearing alginate beads according to the present invention and the manufacturing method thereof have the following effects.
As the photocatalyst is immobilized on the surface of the alginate bead through the air bubbles, the photocatalyst can be regenerated by the photocatalytic reaction, and no separate chemical treatment for regeneration is required. Further, the photocatalyst is dispersed in the solidifying solution instead of the alginate solution, and the photocatalyst is bonded to the bubbles and moved to the alginate bead surface by the surface tension of the bubbles, thereby improving the photocatalyst immobilization efficiency on the alginate bead surface, Can be increased.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart for explaining a method of manufacturing bubbles and a photocatalyst-bearing alginate bead according to an embodiment of the present invention; FIG.
FIGS. 2A to 2C show alginate beads prepared by applying the ultrasonic frequency at 15 kHz, 37 kHz, and 80 kHz, respectively.
FIG. 3 is a SEM photograph showing the distribution of photocatalyst on the alginate bead surface according to application of ultrasonic waves. FIG.
Figure 4 is a photograph of an alginate bead prepared according to one embodiment of the present invention.
5A and 5B show EDX analysis results showing changes in the amount of TiO 2 before and after ultraviolet irradiation.
The present invention discloses a technique for supporting air bubbles and a photocatalyst in addition to an adsorbent material for removing an organic decomposed organic contaminant in an alginate bead. As a result, it is possible to remove the degradable organic pollutants by the adsorbing material and regenerate the alginate beads by the photocatalytic reaction.
In order to maximize the photocatalytic reaction, the photocatalyst must be provided on the surface of the alginate bead rather than the inside of the alginate bead. In order to increase the proportion of the photocatalyst on the alginate bead surface, the present invention uses bubbles. When producing alginate beads, when bubbles are generated and the generated bubbles are carried in the alginate beads, the photocatalyst is moved to the surface of the alginate beads by the surface tension of the bubbles.
Hereinafter, bubbles and photocatalyst-bearing alginate beads according to one embodiment of the present invention and a method for producing the same will be described in detail.
Referring to FIG. 1, the method of manufacturing a bubble and a photocatalyst-bearing alginate bead according to an embodiment of the present invention includes a step of preparing an alginate solution and a solidifying solution, and a step of manufacturing alginate beads carrying bubbles and a photocatalyst .
First, the step of preparing the alginate solution and the solidified solution (S101) will be described as follows.
The alginate solution is prepared by dissolving Na-Alginate powder or Ca-Alginate powder in ultrapure water. To ensure stable hardness of the alginate beads finally formed, the concentration of the alginate solution is 10-40 w / v% is preferable. Also, in the alginate solution, an adsorbent material for removing the refractory organic contaminants is dispersed. As the adsorbing material, powdered activated carbon may be used.
The solidifying solution is used to solidify the alginate solution to produce an alginate bead. An aqueous solution of calcium chloride (CaCl 2 ) or an aqueous solution of barium chloride (BaCl 2 ) may be used. The photocatalyst may be dispersed in the solidification solution, and any one of TiO 2 , ZnO, CdS, WO 3 , ZrO 2 and V 2 O 2 may be used as the photocatalyst. The photocatalyst generates singlet oxygen when visible light or ultraviolet light is irradiated, and decomposes decomposed organic pollutants adsorbed on alginate beads into carbon dioxide (CO 2 ) and water (H 2 O) .
With the alginate solution and the solidified solution prepared, the above-described <alginate bead-supported alginate bead production step> (S102) is carried out.
Specifically, in a state where ultrasonic waves are irradiated to the solidifying solution, the alginate solution is solidified by dropping one drop into the solidifying solution to form an alginate bead. At this time, the adsorbed material dispersed in the alginate solution and the photocatalyst dispersed in the solidified solution are supported in the alginate bead, and bubbles generated by ultrasonic irradiation are carried. That is, as the solidifying solution is irradiated with ultrasound in the curing process of the alginate solution, the adsorbing material and the photocatalyst are carried in the alginate beads together with the bubbles. In one embodiment, the alginate solution may be titrated with the solidifying solution filled in the ultrasonic wave irradiation reaction tank to proceed with the step of producing the alginate beads carrying the bubbles and the photocatalyst.
Whether or not the bubbles are carried and the size of the bubbles are determined by the intensity of the ultrasonic waves. When the frequency of the ultrasonic waves is 15 kHz or less, air bubbles are not carried on the alginate. When the frequency of the ultrasonic waves is 15 kHz or more, the air bubbles are carried on the alginate. As the frequency of the ultrasonic waves is increased from 15 kHz, However, if the frequency of the ultrasonic waves exceeds 90 kHz, the bubbles are destroyed and the size of the bubbles is reduced again. 2A to 2C show bubble-supported alginate when the frequencies of ultrasonic waves are 15 kHz, 37 kHz, and 80 kHz, respectively.
When the size of the bubbles increases with the increase of the ultrasonic frequency, the surface tension of the bubbles increases and the bubbles move to the surface of the alginate beads. The photocatalyst dispersed in the solidifying solution also binds to the bubbles and moves to the surface of the alginate beads. The surface tension of the bubbles enables the photocatalyst to move to the alginate bead surface, thereby increasing the photocatalytic reaction. On the other hand, when the adsorbing material is dispersed in the solidifying solution together with the photocatalyst or the adsorbing material and the photocatalyst are dispersed together in the alginate solution, the activity of the adsorbing material is high and the bonding of the bubbles and the adsorbing material becomes dominant rather than the combination of the bubbles and the photocatalyst. The movement to the alginate bead surface is limited.
The amount of the photocatalyst provided on the surface of the alginate bead can be clearly distinguished by the application of ultrasonic waves. FIG. 3 is a SEM photograph showing the distribution of photocatalyst on the surface of an alginate bead according to application of ultrasonic waves. FIG. 3 shows a case where ultrasonic waves are applied (FIG. 3 (b) It can be seen that the amount of the photocatalyst immobilized on the surface is relatively large.
When the alginate beads having the adsorbent material, the photocatalyst and the air bubbles are produced through the steps of producing the alginate beads carrying the bubbles and the photocatalyst, the alginate beads are dried at a temperature of 100 ° C or lower (S103) The manufacture of bubbles and photocatalyst-bearing alginate beads according to the examples is completed. FIG. 4 is a photograph of alginate beads prepared according to an embodiment of the present invention, and it can be confirmed that a white photocatalyst is provided on the surface.
Next, specific experimental examples of bubbles and photocatalyst-bearing alginate beads according to the present invention will be described.
<Experimental Example 1: Preparation of control beads and beads of the present invention>
Alginate beads (inventive beads) according to the present invention and alginate beads according to the prior art (control 1, control 2, and control 3) were prepared in order to examine characteristics of the alginate beads according to the present invention. Alginate beads according to the prior art were prepared by mixing powdered activated carbon, air bubbles, alginate beads not containing TiO 2 (control 1), alginate beads containing powdered activated carbon (control 2), alginate beads bearing powdered activated carbon and TiO 2 (Control group 3).
The production process of the control group 1 is as follows.
16 g of alginate powder was poured into 400 mL of distilled water and stirred for 24 hours to prepare an alginate solution. Then, calcium chloride solution was prepared by dissolving 20 g of calcium chloride (CaCl 2 ) powder in 400 mL of distilled water, and alginate solution was dropwise added to calcium chloride solution at a height of 30 cm by using burette to form alginate beads. The calcium chloride solution containing the cured alginate beads was stirred for 4 hours, and the alginate beads were recovered and dried in an oven at 60 ° C. to prepare alginate beads of the control 1.
The manufacturing process of the control group 2 is as follows.
5 g of the powdery activated carbon was injected into 400 ml of the alginate solution of the control group 1 and stirred for 10 hours. Then, an alginate bead in which the powdery activated carbon was dispersed in the calcium chloride solution of the control group 1 was titrated to prepare alginate beads of the control group 2. The other manufacturing process is the same as that of Control 1.
The preparation process of the control group 3 is as follows.
5 g of powdered activated carbon and 4 g of TiO 2 were simultaneously injected into 400 mL of the alginate solution of Control 1 and stirred for 10 hours. Then, the alginate beads of the control group 3 were prepared by titrating the powdered activated carbon and the alginate solution in which TiO 2 was dispersed in the calcium chloride solution of the control group 1. The other manufacturing process is the same as that of Control 1.
The manufacturing process of the bead of the present invention is as follows.
5 g of the powdery activated carbon was injected into 400 ml of the alginate solution of the control group 1 and stirred for 10 hours. Then, 4 g of TiO 2 was mixed with 400 ml of the calcium chloride solution of the control group 1, and then the calcium chloride solution in which TiO 2 was dispersed was injected into a sonicator. Then, the alginate solution in which powdered activated carbon was dispersed was irradiated with ultrasonic wave having a frequency of 80 kHz to the ultrasonic generator, and the alginate solution was cured by dropping one drop at a height of 20 cm. During the curing process, the ultrasonic irradiation was continued for 30 minutes, and additional curing process was applied for 3 hours while the ultrasonic irradiation was blocked. The cured alginate beads were taken out and dried in an oven at 60 ° C for 4 hours to obtain the alginate beads of the present invention .
≪ Experimental Example 2: Adsorption and regeneration experiment &
Adsorption and regeneration experiments of control 1, control 2, control 3 and 2,4,6-trichlorophenol (TCP) of the beads of the present invention were carried out.
Control 1, control 2, control 3 and beads of the present invention were prepared as 0.02, 0.05, 0.1 and 0.15 g, respectively, and reacted with 20 ml of TCP at a concentration of 500 mm. After about 15 hours, each reaction sample was sampled and analyzed by high performance liquid chromatography (HPLC). The TCP adsorption capacity of each bead is shown in Table 1 below.
Control 1, control 2, control 3 and beads of the present invention were taken out from each reaction sample, dried in an oven at 60 ° C for about 1 hour, and irradiated with ultraviolet rays in a UV light reactor for 16 hours. Then, after confirming that there was no change in mass of the control 1, control 2, control 3, and bead of the present invention, the above TCP test with the TCP was carried out again to measure the TCP concentration change. The results of adsorption experiments after regeneration are shown in Table 2 below.
As shown in Table 1 and Table 2, the results of the adsorption and regeneration experiments showed that the removal efficiency of the control group 1 was very low, 1.68 mg / g, and the regeneration efficiency was 8.3% . In the case of the control group 2, the control group 3 and the beads of the present invention, the removal efficiencies of TCP were 21.89, 22.82 and 32.05 mg / g, respectively. Overall, TCP removal ability was excellent, but the regeneration efficiency of the bead of the present invention was 89.6% And the control group 3, respectively. In the case of the bead of the present invention, the photocatalyst provided on the surface of the alginate bead may undergo photocatalytic reaction upon irradiation with ultraviolet rays, so that the degradable organic contaminant adsorbed on the alginate bead is decomposed.
≪ Experimental Example 3: Confirmation of deformation after regeneration >
Change in the amount of TiO 2 before and after UV irradiation for the present invention means that the beads were analyzed with the change of the reproduction before and after the TiO 2 amount EDX (Energy Dispersive X-ray Spectroscopy ). 5A and 5B, it was confirmed that TiO 2 occupying 4.54 wt% (see FIG. 5A) on the surface of the alginate bead before regeneration was distributed to 4.49 wt% (see FIG. 5B) after regeneration. It can be seen that there is almost no loss of the photocatalyst.
Claims (8)
And dropping the alginate solution into the solidification solution by one drop in the state of irradiating the solidified solution with ultrasonic waves to cure the alginate solution of each droplet to form an alginate bead,
The adsorbent material is immobilized in the alginate beads and the bubbles and the photocatalyst are carried on the surfaces of the alginate beads,
Wherein the photocatalyst reacts with ultraviolet light to cause a photocatalytic reaction to decompose organic contaminants adsorbed on the alginate beads.
An adsorbent material for removing organic contaminants from the alginate beads, a photocatalyst for photocatalytic reaction by ultraviolet irradiation, and bubbles are supported,
Wherein the photocatalyst is immobilized on the surface of the alginate bead.
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| KR1020140018937A KR101526878B1 (en) | 2014-02-19 | 2014-02-19 | Alginate bead impregnated bubble and photocatalyst method for the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9579630B2 (en) | 2015-07-07 | 2017-02-28 | Korea Institute Of Science And Technology | Bead immobilized with absorbent and microorganisms |
| CN108816291A (en) * | 2018-05-14 | 2018-11-16 | 福建农林大学 | A kind of alginic acid alkali composite photocatalyst aerogel material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1170384A (en) * | 1997-07-01 | 1999-03-16 | Samsung General Chem Co Ltd | Alginic acid gel water treatment agent and preparation |
| JP2005218956A (en) * | 2004-02-05 | 2005-08-18 | Japan Organo Co Ltd | Photocatalyst-containing porous granular body and manufacturing method therefor |
| KR20110082749A (en) * | 2010-01-12 | 2011-07-20 | 한밭대학교 산학협력단 | Active carbon and manufacturing method thereof, and filter with the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1170384A (en) * | 1997-07-01 | 1999-03-16 | Samsung General Chem Co Ltd | Alginic acid gel water treatment agent and preparation |
| JP2005218956A (en) * | 2004-02-05 | 2005-08-18 | Japan Organo Co Ltd | Photocatalyst-containing porous granular body and manufacturing method therefor |
| KR20110082749A (en) * | 2010-01-12 | 2011-07-20 | 한밭대학교 산학협력단 | Active carbon and manufacturing method thereof, and filter with the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9579630B2 (en) | 2015-07-07 | 2017-02-28 | Korea Institute Of Science And Technology | Bead immobilized with absorbent and microorganisms |
| CN108816291A (en) * | 2018-05-14 | 2018-11-16 | 福建农林大学 | A kind of alginic acid alkali composite photocatalyst aerogel material and preparation method thereof |
| CN108816291B (en) * | 2018-05-14 | 2020-12-29 | 福建农林大学 | Alginate-based composite photocatalytic aerogel material and preparation method thereof |
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