CN113041992B - Halloysite-based efficient adsorbent for removing radioactive I-and preparation method thereof - Google Patents
Halloysite-based efficient adsorbent for removing radioactive I-and preparation method thereof Download PDFInfo
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- CN113041992B CN113041992B CN202110376103.8A CN202110376103A CN113041992B CN 113041992 B CN113041992 B CN 113041992B CN 202110376103 A CN202110376103 A CN 202110376103A CN 113041992 B CN113041992 B CN 113041992B
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
Abstract
The invention discloses a method for removing radioactivity I ‑ The halloysite-based efficient adsorbent and a preparation method thereof. The method comprises the steps of evacuating water vapor and air in a halloysite nano-tube by vacuum drying and vacuumizing, and enabling a bismuth nitrate solution to enter the halloysite nano-tube in a vacuum state; removing the bismuth nitrate solution on the outer surface of the halloysite through solid-liquid separation; further calcining bismuth nitrate to generate Bi in the halloysite nanotube 2 O 3 And (4) nano particles to obtain the halloysite-based efficient adsorbent. The method has the advantages of short preparation period, simple process, low cost and the like. Bi in the prepared halloysite-based high-efficiency adsorbent 2 O 3 The nanoparticles exist in the halloysite nanotube, and have the advantages of stable structure, strong selectivity on radioactive iodide ions, high removal speed, high removal rate and the like.
Description
The technical field is as follows:
the invention belongs to the technical field of mineral materials, and particularly relates to a method for removing radioactivity I - The halloysite-based efficient adsorbent and a preparation method thereof.
The background art comprises the following steps:
radioactive iodine is one of the products of nuclear fission and is widely present in nuclear waste. Since most of the rocks and minerals in nature are neutral or negatively charged, I - Difficult to adsorb and block effectively; I.C. A - Has the characteristics of weak adsorbability and high mobility in the environment, so the radioactivity I - Is considered one of the most intractable radionuclides. The adsorption method becomes the most widely used radioactivity I due to the advantages of high efficiency, universality, simple operation, low cost and the like - A removal method; the performance of the adsorbent is the determining factor for the effectiveness of the adsorption process, and therefore, the development of a high-efficiency adsorbent is the key to ensure the effective implementation of the process. In the prior art, for removing radiation I - The adsorbent is selected from activated carbon, natural inorganic materials (such as montmorillonite, chrysotile, and layered double hydroxide), ion exchange resin, and nanocomposite. Wherein the nanocomposite is generally to be mixed with I - Compounding active ingredients with strong adsorption capacity (such as silver oxide, bismuth oxide, cuprous chloride, etc.) with carrier to increase dispersibility of the active ingredients, and its application to I - The adsorption has better selectivity and higher adsorption capacity, and is more efficient I - An adsorbent. However, the use for adsorbing radioactive I has been reported so far - The nano composite material needs to be prepared into a carrier material firstly, has the problems of long preparation period, high energy consumption and the like, and is not beneficial to popularization and application; more importantly, the active ingredients in the existing nano composite material adsorbent are mainly present on the outer surface of the carrier, and the radioactivity I is fixed - Also exists on the outer surface of the adsorbent, and has the problems of unstable structure, possibility of falling off from the carrier and entering a water body, secondary pollution and the like.
The invention content is as follows:
the object of the invention is to address the radioactivity I existing in the prior art - The defects of the preparation and the use of the adsorbent are to provide a method for removing the radioactivity I - The halloysite-based high-efficiency adsorbent and the preparation method thereof, which aim to solve the problem of I in the prior art - Long preparation period of the adsorbent, high preparation cost, unstable structure and the like.
Removal of radioactivity I of the present invention - The halloysite-based high-efficiency adsorbent is prepared by a method for removing radioactivity I - The halloysite-based efficient adsorbent and the preparation method thereof comprise the following steps:
1) putting halloysite into a vacuum drying oven, and drying for 12-24 h at 120 ℃ under a vacuum condition;
2) carrying out vacuum filtration on the halloysite dried in the step 1);
3) mixing bismuth nitrate and halloysite for reaction to obtain a suspension;
4) carrying out solid-liquid separation on the suspension in the step 3);
5) placing the solid obtained in the step 4) in a tube furnace, heating to 450-500 ℃ at a heating speed of 1-10 ℃/min in an air atmosphere, calcining for 2-6 h, and cooling to room temperature to obtain the product with radioactivity I removed - The halloysite-based high-efficiency adsorbent.
Further, the halloysite is more than 70wt% pure.
Further, the specific vacuum filtration process in step 2) is to place the halloysite in a vacuum filtration bottle, a side port of the vacuum filtration bottle is connected with a vacuum pump, a magnetic stirring magneton is placed in the vacuum filtration bottle, the upper part of the vacuum filtration bottle is connected with a separating funnel through a grinding port, the grinding port has a sealing effect, a cock of the separating funnel is in a sealing state, the vacuum pump is opened, and the vacuum is pumped for 3-10 hours.
Further, the specific process of mixing and reacting bismuth nitrate and the halloysite in the step 3) to obtain the suspension is to fill a bismuth nitrate solution into a separating funnel, open a cock of the separating funnel, drip the bismuth nitrate solution according to the ratio of the mass of the halloysite to the volume of the bismuth nitrate solution of 1g/100mL, mix and stir the bismuth nitrate solution and the halloysite in a vacuum state, completely open the cock of the separating funnel when the bismuth nitrate solution is about to drip, allow air to enter, and continue stirring for 2-10 hours.
Further, the vacuum state is that the vacuum degree in the vacuum filtration bottle is lower than-0.07 MPa.
Further, the bismuth nitrate solution is one of a bismuth nitrate ethylene glycol solution, a bismuth nitrate glycerin solution or a bismuth nitrate acetone solution. The bismuth nitrate glycol solution, the bismuth nitrate glycerin solution or the bismuth nitrate acetone solution are respectively used for dissolving bismuth nitrate in glycol, glycerin or acetone.
Further, the bismuth nitrate solution is a bismuth nitrate glycol solution, and the concentration of the bismuth nitrate glycol solution is 0.05-0.1 mol/L.
Further, the solid-liquid separation in the step 4) is performed by centrifugation or filtration.
Step 1) -step 5) for removing radioactivity I - The halloysite-based high-efficiency adsorbent.
Compared with the prior art, the invention has the following advantages:
1. the halloysite used as the carrier is a natural nano tubular mineral and has the advantages of stable structure, low cost and easy obtainment; in addition, the method does not use a strong pollution chemical reagent, and the used bismuth nitrate glycol solution can be reused, so that the method has the advantages of low preparation cost, short reaction time and the like.
2. The method comprises the steps of firstly, evacuating water vapor and air in a halloysite nano pipeline through vacuum drying and vacuumizing, so that a bismuth nitrate glycol solution enters a nano pore channel; removing the bismuth nitrate glycol solution on the outer surface of the halloysite through solid-liquid separation; further heating and calcining the bismuth nitrate to generate Bi in the halloysite nanotube 2 O 3 And (3) nanoparticles. Compared with the prior art that active ingredients (such as silver oxide, bismuth oxide and the like) in the adsorbent mainly exist on the outer surface of the carrier, Bi in the halloysite-based efficient adsorbent prepared by the invention 2 O 3 The nanoparticles are present in the nano-tubes of halloysite, and the Bi in the nano-tubes 2 O 3 The high-efficiency adsorbent prepared by the invention has better structural stability; in addition, the high efficiency adsorbent can fix the radiation I due to shielding effect of the halloysite nanotube wall - And will then be less radioactive.
3. The halloysite-based efficient adsorbent prepared by the method has stable structure, high speed of removing iodide ions and high removal rate (0.1g of halloysite-based efficient adsorbent is about 1h for 10mL of the halloysite-based efficient adsorbent containing I - The highest removal rate of the solution can reach 94 percent), and the like.
Description of the drawings:
FIG. 1 is an X-ray diffraction pattern of the halloysite used in the examples and the radioactive I-removed halloysite-based high performance adsorbent prepared in example 1.
FIG. 2 is a transmission electron micrograph of the halloysite used in examples and the radioactive I-removed halloysite-based high efficiency adsorbent prepared in example 1. Wherein, the image (a) is a transmission electron micrograph of halloysite used in the examples; FIG. (b) is a graph for removing radioactivity I prepared in example 1 - Transmission electron microscopy of the halloysite-based high-efficiency adsorbent.
The specific implementation mode is as follows:
the following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Example 1
1) Putting 1g of halloysite in a vacuum drying oven, and drying for 12h at 120 ℃ under a vacuum condition;
2) placing the halloysite dried in the step 1) into a vacuum filtration bottle, connecting a side port of the vacuum filtration bottle with a vacuum pump, placing a magnetic stirring magneton in the vacuum filtration bottle, connecting the upside of the vacuum filtration bottle with a separating funnel through a ground port, sealing the ground port, turning on the vacuum pump, and vacuumizing for 3 hours;
3) adding 100mL of 0.1mol/L bismuth nitrate glycol solution into a separating funnel, opening a cock of the separating funnel to drip the bismuth nitrate glycol solution, mixing and stirring the bismuth nitrate glycol solution and halloysite under the condition that the vacuum degree is-0.08 Mpa, completely opening the cock of the separating funnel when the bismuth nitrate glycol solution is about to drip completely, allowing air to enter, and continuing stirring for 2 hours;
4) centrifuging the suspension obtained in the step 3);
5) putting the solid obtained in the step 4) into a tubular furnace, heating to 500 ℃ at a heating speed of 1 ℃/min in the air atmosphere, calcining for 6h, and cooling to room temperature to obtain the radioactivity I removed - The halloysite-based high-efficiency adsorbent.
The structure of the radioactive iodide ion-removing halloysite-based high-efficiency adsorbent prepared in this example was measured by X-ray diffraction, and the results showed that the radioactive iodide ion-removing halloysite-based high-efficiency adsorbent exhibited X-ray diffraction patterns attributed to metamorphite and Bi 2 O 3 Characterized in that (see FIG. 1, FIG. 1 is measured by X-ray diffractometer model D/Max-2200 of Pasacaceae, Netherlands), and the halloysite is generated by removing the structural hydroxyl groups and losing the crystal structure of the halloysite during the calcination. Analysis by a transmission electron microscope shows that in the halloysite-based high-efficiency adsorbent for removing radioactive iodide ions, Bi is contained 2 O 3 The nanocrystals were present in halloysite nanotubes (compare FIG. 2-b with FIG. 2-a), and FIG. 2 was measured using a FEI Tecnai G2F 20S-TWIN TMP type transmission-scanning electron microscope.
As one implementation application, according to the solid-to-liquid ratio of 0.1g of the halloysite-based composite material for removing radioactive iodide/10 mL of iodide solution,adsorption experiments were performed at room temperature. When the initial concentration of the iodide ion solution is 10ppm, the halloysite-based composite material pair I for removing radioactive iodide ions after 1h - The removal rate of (2) was 94%.
Example 2
1) Putting 1g of halloysite in a vacuum drying oven, and drying for 24 hours at 120 ℃ under a vacuum condition;
2) placing the halloysite dried in the step 1) into a vacuum filtration bottle, connecting a side port of the vacuum filtration bottle with a vacuum pump, placing magnetic stirring magnetons into the vacuum filtration bottle, connecting the upper part of the vacuum filtration bottle with a separating funnel through a ground port, sealing the ground port, turning a cock of the separating funnel into a sealed state, opening the vacuum pump, and vacuumizing for 3 hours;
3) adding 100mL of 0.1mol/L bismuth nitrate glycol solution into a separating funnel, opening a cock of the separating funnel to drip the bismuth nitrate glycol solution, mixing with halloysite under the condition that the vacuum degree is-0.08 Mpa, stirring, completely opening the cock of the separating funnel when the bismuth nitrate glycol solution is about to drip, allowing air to enter, and continuously stirring for 2 hours;
4) centrifugally separating the suspension obtained in the step 3);
5) putting the solid obtained in the step 4) into a tube furnace, heating to 500 ℃ at a heating speed of 5 ℃/min in the air atmosphere, calcining for 6h, and cooling to room temperature to obtain the product with radioactivity I removed - The halloysite-based high-efficiency adsorbent.
As one practical application, adsorption experiments were performed at room temperature according to a solid-to-liquid ratio of 0.1g of a halloysite-based composite material for radioactive iodide ion removal/10 mL of an iodide ion solution. When the initial concentration of the iodide ion solution is 50ppm, the halloysite-based composite material pair I for removing radioactive iodide ions is obtained after 1h - The removal rate of (2) was 80%.
Example 3
1) 1g of halloysite is placed in a vacuum drying oven and dried for 16h at 120 ℃ under vacuum condition;
2) placing the halloysite dried in the step 1) into a vacuum filtration bottle, connecting a side port of the vacuum filtration bottle with a vacuum pump, placing magnetic stirring magnetons into the vacuum filtration bottle, connecting the upper part of the vacuum filtration bottle with a separating funnel through a ground port, sealing the ground port, turning a cock of the separating funnel into a sealed state, opening the vacuum pump, and vacuumizing for 5 hours;
3) adding 100mL of 0.08mol/L bismuth nitrate glycol solution into a separating funnel, opening a cock of the separating funnel to drip the bismuth nitrate glycol solution, mixing and stirring the bismuth nitrate glycol solution and halloysite under the condition that the vacuum degree is-0.08 MPa, completely opening the cock of the separating funnel when the bismuth nitrate glycol solution is about to drip completely, allowing air to enter, and continuously stirring for 6 hours;
4) centrifuging the suspension obtained in the step 3);
5) putting the solid obtained in the step 4) into a tubular furnace, heating to 480 ℃ at a heating speed of 5 ℃/min in an air atmosphere, calcining for 6h, and cooling to room temperature to obtain the radioactivity I removed - The halloysite-based high-efficiency adsorbent.
As one practical application, an adsorption experiment was performed at room temperature according to a solid-to-liquid ratio of 0.1g of the halloysite-based composite material for removing radioactive iodide/10 mL of an iodide solution. When the initial concentration of the iodide ion solution is 30ppm, the halloysite-based composite material pair I for removing radioactive iodide ions after 1h - The removal rate of (2) was 82%.
Example 4
1) Putting 1g of halloysite in a vacuum drying oven, and drying for 24h at 120 ℃ under a vacuum condition;
2) placing the halloysite dried in the step 1) into a vacuum filtration bottle, connecting a side port of the vacuum filtration bottle with a vacuum pump, placing magnetic stirring magnetons into the vacuum filtration bottle, connecting the upper part of the vacuum filtration bottle with a separating funnel through a ground port, sealing the ground port, turning a cock of the separating funnel into a sealed state, opening the vacuum pump, and vacuumizing for 10 hours;
3) adding 100mL of 0.05mol/L bismuth nitrate glycol solution into a separating funnel, opening a cock of the separating funnel to drip the bismuth nitrate glycol solution, mixing and stirring the bismuth nitrate glycol solution and halloysite under the condition that the vacuum degree is-0.07 MPa, completely opening the cock of the separating funnel when the bismuth nitrate glycol solution is about to drip completely, allowing air to enter, and continuously stirring for 10 hours;
4) filtering the suspension obtained in the step 3), and carrying out solid-liquid separation;
5) putting the solid obtained in the step 4) into a tubular furnace, heating to 450 ℃ at a heating speed of 10 ℃/min in an air atmosphere, calcining for 2h, and cooling to room temperature to obtain the radioactivity I removed - The halloysite-based high-efficiency adsorbent.
As one practical application, an adsorption experiment was performed at room temperature according to a solid-to-liquid ratio of 0.1g of the halloysite-based composite material for removing radioactive iodide/10 mL of an iodide solution. When the initial concentration of the iodide ion solution is 10ppm, the halloysite-based composite material pair I for removing radioactive iodide ions is obtained after 1h - The removal rate of (2) was 90%.
Claims (7)
1. Remove radioactivity I - Removing radioactivity I by halloysite-based high-efficiency adsorbent - The application is characterized in that the preparation method of the halloysite-based efficient adsorbent comprises the following steps:
1) putting halloysite into a vacuum drying oven, and drying for 12-24 h at 120 ℃ under a vacuum condition;
2) carrying out vacuum filtration on the halloysite dried in the step 1);
3) mixing bismuth nitrate and halloysite to react to obtain a suspension, specifically, loading a bismuth nitrate solution into a separating funnel, opening a cock of the separating funnel, dripping the bismuth nitrate solution according to the ratio of the mass of the halloysite to the volume of the bismuth nitrate solution of 1g/100mL, mixing the bismuth nitrate solution with the halloysite and stirring the mixture in a vacuum state, completely opening the cock of the separating funnel when the bismuth nitrate solution is about to drip, allowing air to enter, and continuously stirring for 2-10 hours;
4) carrying out solid-liquid separation on the suspension in the step 3);
5) putting the solid obtained in the step 4) into a tube furnace, heating to 450-500 ℃ at a heating speed of 1-10 ℃/min in an air atmosphere, calcining for 2-6 h, and cooling to room temperature to obtain the product with radioactivity I removed - The halloysite-based high-efficiency adsorbent.
2. Use according to claim 1, wherein the halloysite is halloysite with a purity of greater than 70 wt%.
3. The application of claim 1, wherein the vacuum filtration in step 2) comprises the specific process of placing halloysite in a vacuum filtration bottle, the side port of the vacuum filtration bottle is connected with a vacuum pump, a magnetic stirring magneton is placed in the vacuum filtration bottle, the upper part of the vacuum filtration bottle is connected with a separating funnel through a grinding port, the grinding port has a sealing effect, a cock of the separating funnel is in a sealing state, the vacuum pump is turned on, and the vacuum is pumped for 3-10 hours.
4. Use according to claim 1, characterized in that the vacuum is less than-0.07 MPa in the vacuum flask.
5. The use of claim 1, wherein the bismuth nitrate solution is one of a bismuth nitrate ethylene glycol solution, a bismuth nitrate glycerol solution, or a bismuth nitrate acetone solution.
6. The use according to claim 1, wherein the bismuth nitrate solution is a bismuth nitrate glycol solution having a concentration of 0.05 to 0.1 mol/L.
7. The use according to claim 1, wherein the solid-liquid separation in step 4) is performed by centrifugation or filtration.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103918711A (en) * | 2014-04-17 | 2014-07-16 | 常州大学 | Preparation of halloysite loaded nano-silver antibacterial material |
| CN103934008A (en) * | 2014-04-17 | 2014-07-23 | 常州大学 | Preparation method of halloysite loading phosphoric acid Silverlight catalyst |
| CN106076246A (en) * | 2016-06-20 | 2016-11-09 | 江苏大学 | A kind of have the compound except iodine material and preparation method of micro-nano hierarchy |
| CN108380175A (en) * | 2018-02-28 | 2018-08-10 | 中国科学院广州地球化学研究所 | A kind of carbonic acid gas lanthanum-halloysite composite material and its preparation method and application |
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| JP3136044B2 (en) * | 1994-03-07 | 2001-02-19 | 財団法人産業創造研究所 | Iodine ion adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103918711A (en) * | 2014-04-17 | 2014-07-16 | 常州大学 | Preparation of halloysite loaded nano-silver antibacterial material |
| CN103934008A (en) * | 2014-04-17 | 2014-07-23 | 常州大学 | Preparation method of halloysite loading phosphoric acid Silverlight catalyst |
| CN106076246A (en) * | 2016-06-20 | 2016-11-09 | 江苏大学 | A kind of have the compound except iodine material and preparation method of micro-nano hierarchy |
| CN108380175A (en) * | 2018-02-28 | 2018-08-10 | 中国科学院广州地球化学研究所 | A kind of carbonic acid gas lanthanum-halloysite composite material and its preparation method and application |
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