CN111185133A - Method for re-stabilizing heavy metal adsorption material and light reaction device thereof - Google Patents
Method for re-stabilizing heavy metal adsorption material and light reaction device thereof Download PDFInfo
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- CN111185133A CN111185133A CN202010149933.2A CN202010149933A CN111185133A CN 111185133 A CN111185133 A CN 111185133A CN 202010149933 A CN202010149933 A CN 202010149933A CN 111185133 A CN111185133 A CN 111185133A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- 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
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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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
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- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
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Abstract
The invention discloses a method for re-stabilizing a heavy metal adsorbing material, which comprises the following steps: preparing a Schneider mineral, namely synthesizing an iron-based adsorbent Schneider mineral SCH by a biological method; preparing a heavy metal adsorption material with large loading capacity in an alkaline environment; photochemical restabilization reaction; selecting a photochemical reaction device and setting relevant parameters thereof, dissolving the heavy metal adsorption material into an organic acid solution for reaction under stable illumination intensity, carrying out sampling analysis at intervals in the photoreaction process, repeating each step for three times and making an error line. The invention also provides a photoreaction device for re-stabilizing the heavy metal adsorption material, the organic acid and the ultraviolet light cooperate to promote the re-fixation of the dissolved heavy metal, the device has practical significance for solving the problem that the content of As in underground water exceeds the standard, and the device is very important for improving the stability of the As-loaded schleman minerals.
Description
Technical Field
The invention belongs to the water treatment technology, is applied to the fields of iron-based adsorption materials and heavy metal wastewater treatment process equipment, relates to a stabilization scheme of an iron-based adsorbent loaded with heavy metals in a water body, and particularly relates to a method for re-stabilizing a heavy metal adsorption material and a photoreaction device thereof.
Background
With the social progress and industrial development, the discharge amount of wastewater containing heavy metal ions increases year by year, however, the content of the alkali metal and the alkaline earth metal in a constant amount does not exceed the standard, and the corresponding water treatment process is required to have high selectivity on the heavy metal ions. Meanwhile, the high-content heavy metal ions in the wastewater have obvious toxic action on microorganisms in the traditional water treatment process. Therefore, it is a task to be faced by the current water treatment technology to research how to effectively remove heavy metal pollutants in water.
Based on the above problems, researches have found that the iron-based adsorption material (iron oxide) has a remarkable adsorption effect on heavy metal ions, is simple and easily available, and widely exists in the nature. However, the removal of heavy metals from water by adding iron oxides such as jarosite, schrader minerals, etc. to the wastewater has been found to be of little benefit. The main reason is that under the acidic condition, especially in the presence of organic acid which is a plant putrefaction product, the iron oxide can accelerate the dissolution of the iron oxide, and the heavy metal is loaded to be dissolved again.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for re-stabilizing a heavy metal adsorption material and a photoreaction device thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for re-stabilizing a heavy metal adsorption material is designed, and comprises the following steps:
s1, preparation of schlieren mineral: synthesizing an iron-based adsorbent Schneider mineral SCH by a biological method;
s2, preparation of the heavy metal adsorption material: preparing a heavy metal adsorbing material with large loading capacity in an alkaline environment;
s3, photochemical stabilization reaction: and (3) selecting a photochemical reaction device and setting relevant parameters of the photochemical reaction device, dissolving the heavy metal adsorption material obtained in the step S2 into an organic acid solution for reaction under stable illumination intensity, and carrying out sampling analysis at intervals in the photoreaction process, wherein each step is repeated for three times and an error line is drawn.
Further, the preparation method of schlerian mineral in S1 specifically includes the following steps:
step 101: weighing quantitative FeSO4 & 7H2O, placing in a container, dissolving with deionized water, and adjusting pH to 1-4 with dilute sulfuric acid;
step 102: inoculating a quantitative A.ferrooxidans LX5 cell suspension, performing constant volume, culturing in a sealed container in a shaking table at 15-38 ℃ and 100-300rpm for 2-4 days, and performing suction filtration and deionized water washing to obtain a schlempe mineral SCH;
step 103: the SCH obtained in step 102 was dried in a vacuum oven at 50-70 ℃ for 8h and stored in a sealed centrifuge tube for further use.
Further, in S2, the heavy metal adsorbing material is SCH-As (iii) adsorbing material.
Further, the preparation method of SCH-As (III) specifically comprises the following steps:
step 201: introducing a quantitative amount of SCH into a quantitative amount of As (III) -containing solution at a pH of 8-12;
step 202: placing the suspension on a reciprocating shaking bed, and shaking at the speed of 100-200r/min at the temperature of 20-30 ℃ for 20-30 hours;
step 203: after step 202 is completed, placing the obtained material in a 4000-;
step 204: drying in a vacuum oven at 50-70 deg.C to obtain As-loaded Schneider mineral SCH-As (III), and storing in a sealed centrifuge tube.
Further, the specific method of the photochemical stabilization reaction in step S3 includes the steps of:
step 301: before the reaction, setting parameters of a light reaction instrument, wherein the water bath temperature is 25 +/-1 ℃, the rotating speed is 400-600r/min, preheating the mercury lamp for 10-15min in advance to ensure stable light intensity, and setting reaction conditions according to reaction requirements;
step 302: selecting a 40mL quartz tube, adding SCH-As (III) into 40mL of 1mmol/L organic acid solution with the pH value of 3, and putting the solution into a rotor;
step 303: setting sampling intervals, taking 2.0mL of solution each time, filtering out insoluble substances through a 0.45-micron filter membrane, and measuring the concentrations of soluble total iron and total arsenic in the solution through the filtrate;
step 304: insoluble substances after the reaction are collected by centrifugation and dried for surface feature analysis.
Further, in step 301, the reaction conditions include DOM concentration, schlieren mineral dosage, pH, and coexisting ion content.
The invention also provides a photoreaction device for the re-stabilization of the heavy metal adsorption material, which comprises a photoreaction unit, a light source control unit and a constant temperature unit;
the photoreaction unit is a photoreactor with a magnetic stirring structure and a constant temperature jacket, and water inlet and outlet ports are arranged on two sides of the constant temperature jacket;
the light source control unit is a light source controller and is used for controlling the illumination intensity of a light source in the photoreactor;
the constant temperature unit is a low-temperature constant temperature tank and is used for providing constant temperature water supply for a constant temperature jacket on the photoreactor, and reaction materials in the photoreactor are ensured to be carried out under the constant temperature condition;
be equipped with a plurality of column grooves that are used for placing the quartz test tube along its circumference in the constant temperature jacket, on the lateral wall of constant temperature jacket, and correspond every the position in column groove all is equipped with the slot of forked tail structure, all be equipped with the detachable picture peg in the slot, one side in the column groove that the picture peg corresponds is equipped with the reflection of light face of arc structure.
Furthermore, a cooling sleeve is arranged on the outer side of the light reactor, which is positioned at the ultraviolet light source and is provided with cooling circulating inlet water and cooling circulating outlet water.
Furthermore, the top of the inserting plate is provided with a handle for plugging and unplugging.
Further, the light reflecting surface is a light reflecting surface with a honeycomb structure.
The invention provides a method for re-stabilizing a heavy metal adsorption material and a reaction device thereof, which have the beneficial effects that: the method can promote the re-fixation of the dissolved heavy metal through the synergy of the organic acid and the ultraviolet light, has practical significance for solving the problem that the content of As in underground water exceeds the standard, and is very important for improving the stability of the As-loaded schleman minerals.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a view of the structure of a Schneider mineral according to the present invention;
FIG. 2 is a schematic view of the structure of the photoreaction apparatus according to the present invention;
FIG. 3 is a graph showing the effect of organic acids on the stability of SCH-As (III) according to the invention;
FIG. 4 is a graph showing the effect of UV light on SCH-As (III) stability according to the invention;
FIG. 5 is a structural diagram of the reaction mechanism of the present invention for improving the stability of SCH-As (III) by the synergy of organic acid and UV light;
FIG. 6 is a schematic view of the structure of a photoreactor according to the present invention;
FIG. 7 is a schematic diagram of the present invention with the insert plate removed from the optical reactor.
Labeled as: 1-a photoreactor; 2-constant temperature jacket; 3-a cylindrical groove; 4-cooling the sleeve; 5-a light source; 6-quartz test tubes; 7-cooling and circulating water inflow; 8-cooling the circulating effluent; 9-slot; 10-inserting plate; 11-a handle; 12-reflecting surface.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "provided with" and "connected" are to be interpreted broadly, e.g., as being fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically 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.
The structural features of the present invention will now be described in detail with reference to the accompanying drawings.
Referring to fig. 1-7, a method for re-stabilizing a heavy metal adsorption material includes the following steps:
s1, preparation of schlieren mineral: synthesizing an iron-based adsorbent Schneider mineral SCH by a biological method, putting 11.12g of FeSO4 & 7H2O in a conical flask, dissolving the mixture in deionized water, adjusting the pH value to 2.5 by using dilute sulfuric acid, inoculating 5mL of A.ferrooxidans LX5 cell suspension, fixing the volume to 250mL, sealing the solution by using eight layers of sterile gauze, culturing the solution in a shaking table at 28 ℃ and 180rpm for three days, performing suction filtration and deionized water washing to obtain the Schneider mineral, drying the Schneider mineral in a vacuum oven at 60 ℃ for 8 hours, and taking the Schneider mineral into a sealed centrifuge tube for later use;
s2, preparation of SCH-As (III): first, 0.01g of SCH was introduced into 100mL of a solution containing 50mg/LAs (III) at pH 10; through preliminary study, the optimal adsorption pH of the non-pretreated SCH is 10; then, the suspension is placed on a reciprocating shaker, shaken at the speed of 180r/min for 24 hours at the temperature of 25 ℃, centrifuged for 5 minutes in a centrifuge with 5000rpm, washed for 3 times by deionized water, finally dried in a vacuum oven at the temperature of 60 ℃, stored in a sealed centrifuge tube, and the maximum loading capacity of As (III) is calculated to be 110.5 mg/g;
s3, photochemical stabilization reaction: in this example, the photoreaction was performed in a 40mL standard quartz tube, and the specific steps were as follows:
(1) before reaction, setting parameters of a light reaction instrument: the water bath temperature is 25 +/-1 ℃, the rotating speed is 500r/min, and in order to ensure stable light intensity, the mercury lamp is preheated for 15min in advance.
(2) According to the experimental requirements, relevant conditions including DOM concentration, Schneider mineral dosage, pH value and coexisting ion content are set, and the reaction solution is placed in a 40mL quartz test tube and put into a rotor.
(3) Setting sampling intervals, taking 2.0mL of solution each time, filtering out insoluble substances through a 0.45-micron filter membrane, and measuring the concentrations of soluble total iron and total arsenic in the solution through the filtrate;
(4) insoluble substances after the reaction are collected by centrifugation and dried for surface feature analysis.
All reactions were repeated three times and error bars were drawn.
The method can promote the re-fixation of the dissolved heavy metal through the synergy of the organic acid and the ultraviolet light, has practical significance for solving the problem that the content of As in underground water exceeds the standard, and is very important for improving the stability of the As-loaded schleman minerals.
As shown in fig. 2, 6 and 7, the present invention further provides a photoreaction apparatus for re-stabilizing a heavy metal adsorbing material, which comprises a photoreaction unit, a light source control unit and a constant temperature unit;
the photoreaction unit is a photoreactor 1 with a magnetic stirring structure and a constant temperature jacket 2, water inlet and outlet ports are arranged on two sides of the constant temperature jacket 2, a cooling sleeve 4 is arranged on the outer side of the ultraviolet light source 5 capable of emitting light in the photoreactor 1, a cooling circulation water inlet 7 and a cooling circulation water outlet 8 are arranged on the cooling sleeve 4, and the cooling sleeve 4 is made of transparent glass materials.
The light source control unit is a light source controller and is used for controlling the illumination intensity of the ultraviolet light source 5 which can emit light in the photoreactor 1.
The constant temperature unit is a low-temperature constant temperature tank and is used for providing constant temperature water supply for a constant temperature jacket 2 on the photoreactor 1, so that reaction materials in the photoreactor 1 are ensured to be carried out under a constant temperature condition, and the constant temperature jacket 2 is made of a transparent glass material.
Be equipped with a plurality of column grooves 3 that are used for placing quartz test tube 6 along its circumference in the constant temperature jacket 2, on the lateral wall of constant temperature jacket 2 to the position that corresponds every column groove 3 all is equipped with slot 9 of forked tail structure, all is equipped with detachable picture peg 10 in the slot 9, and the top of picture peg 10 is equipped with and is used for pulling out the handle 11 of inserting the dismouting.
One side of the cylindrical groove 3 corresponding to the inserting plate 10 is provided with a reflecting surface 12 with an arc structure, and the reflecting surface 12 is a reflecting surface with a honeycomb structure.
According to the reaction device for re-stabilizing the heavy metal adsorption material, the detachable plugboard 10 is arranged on the outer side of the constant temperature jacket 2 of the photoreactor 1, so that the reaction condition in the quartz test tube 6 can be conveniently observed when the photoreactor is detached, after the reaction device is installed, the reflecting surface 12 on the inner side of the plugboard 10 can improve the irradiation effect of the light source 5, and simultaneously improve the irradiation uniformity of the material in the quartz test tube 6, so that the photoresponse of the material is facilitated.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for re-stabilizing a heavy metal adsorption material is characterized by comprising the following steps:
s1, preparation of schlieren mineral: synthesizing an iron-based adsorbent Schneider mineral SCH by a biological method;
s2, preparation of the heavy metal adsorption material: preparing a heavy metal adsorbing material with large loading capacity in an alkaline environment;
s3, photochemical stabilization reaction: and (3) selecting a photochemical reaction device and setting relevant parameters of the photochemical reaction device, dissolving the heavy metal adsorption material obtained in the step S2 into an organic acid solution for reaction under stable illumination intensity, and carrying out sampling analysis at intervals in the photoreaction process, wherein each step is repeated for three times and an error line is drawn.
2. The method for re-stabilizing the heavy metal adsorbing material according to claim 1, wherein the preparation method of the schlerian mineral in S1 specifically comprises the following steps:
step 101: weighing quantitative FeSO4 & 7H2O, placing in a container, dissolving with deionized water, and adjusting pH to 1-4 with dilute sulfuric acid;
step 102: inoculating a quantitative A.ferrooxidans LX5 cell suspension, performing constant volume, culturing in a sealed container in a shaking table at 15-38 ℃ and 100-300rpm for 2-4 days, and performing suction filtration and deionized water washing to obtain a schlempe mineral SCH;
step 103: the SCH obtained in step 102 was dried in a vacuum oven at 50-70 ℃ for 8h and stored in a sealed centrifuge tube for further use.
3. The method of claim 1, wherein the heavy metal adsorbent material is SCH-As (III) adsorbent material at S2.
4. The method for re-stabilizing the heavy metal adsorbing material according to claim 3, wherein the preparation method of SCH-As (III) comprises the following steps:
step 201: introducing a quantitative amount of SCH into a quantitative amount of As (III) -containing solution at a pH of 8-12;
step 202: placing the suspension on a reciprocating shaking bed, and shaking at the speed of 100-200r/min at the temperature of 20-30 ℃ for 20-30 hours;
step 203: after step 202 is completed, placing the obtained material in a 4000-;
step 204: drying in a vacuum oven at 50-70 deg.C to obtain As-loaded Schneider mineral SCH-As (III), and storing in a sealed centrifuge tube.
5. The method for re-stabilizing a heavy metal adsorbing material according to claim 4, wherein the specific method of the photochemical re-stabilizing reaction in step S3 comprises the following steps:
step 301: before the reaction, setting parameters of a light reaction instrument, wherein the water bath temperature is 25 +/-1 ℃, the rotating speed is 400-600r/min, preheating the mercury lamp for 10-15min in advance to ensure stable light intensity, and setting reaction conditions according to reaction requirements;
step 302: selecting a 40mL quartz tube, adding SCH-As (III) into 40mL of 1mmol/L organic acid solution with the pH value of 3, and putting the solution into a rotor;
step 303: setting sampling intervals, taking 2.0mL of solution each time, filtering out insoluble substances through a 0.45-micron filter membrane, and measuring the concentrations of soluble total iron and total arsenic in the solution through the filtrate;
step 304: insoluble substances after the reaction are collected by centrifugation and dried for surface feature analysis.
6. The method for re-stabilizing a heavy metal adsorbing material according to claim 5, wherein in step 301, the reaction conditions are DOM concentration, Schneider mineral dosage, pH value and coexisting ion content.
7. A photoreaction device for any heavy metal adsorption material re-stabilization method according to claims 1 to 6, which comprises a photoreaction unit, a light source control unit and a constant temperature unit;
the photoreaction unit is a photoreactor (1) with a magnetic stirring structure and a constant temperature jacket (2), and water inlet and outlet ports are arranged on two sides of the constant temperature jacket (2);
the light source control unit is a light source controller and is used for controlling the illumination intensity of the ultraviolet lamp source (5) which can be emitted in the photoreactor (1);
the constant temperature unit is a low-temperature constant temperature tank and is used for providing constant-temperature water supply for a constant temperature jacket (2) on the photoreactor (1) and ensuring that reaction materials in the photoreactor (1) are carried out under the constant temperature condition;
be equipped with a plurality of column grooves (3) that are used for placing quartz test tube (6) along its circumference in the constant temperature jacket (2), on the lateral wall of constant temperature jacket (2), and correspond every the position of column groove (3) all is equipped with slot (9) of forked tail structure, all be equipped with detachable picture peg (10) in slot (9), one side of the column groove (3) that picture peg (10) correspond is equipped with reflecting surface (12) of arc structure.
8. The photoreaction device for the re-stabilization of the heavy metal adsorbing material according to claim 7, wherein a cooling jacket (4) is arranged outside the light source (5) in the photoreactor (1), and a cooling circulation water inlet (7) and a cooling circulation water outlet (8) are arranged on the cooling jacket (4).
9. A photoreaction device for re-stabilizing a heavy metal adsorbing material according to claim 7, wherein the top of the insert plate (10) is provided with a handle (11) for plugging and unplugging.
10. The photoreaction apparatus for re-stabilization of a heavy metal adsorbing material as claimed in claim 7, wherein the light-reflecting surface (12) is a honeycomb-structured light-reflecting surface.
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| CN112705151A (en) * | 2020-12-19 | 2021-04-27 | 北京大学 | Liquid phase synthesis auxiliary system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112705151A (en) * | 2020-12-19 | 2021-04-27 | 北京大学 | Liquid phase synthesis auxiliary system |
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Application publication date: 20200522 |