CN115254032A - Ionic liquid immobilized activated carbon and preparation method thereof - Google Patents
Ionic liquid immobilized activated carbon and preparation method thereof Download PDFInfo
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- CN115254032A CN115254032A CN202210395129.1A CN202210395129A CN115254032A CN 115254032 A CN115254032 A CN 115254032A CN 202210395129 A CN202210395129 A CN 202210395129A CN 115254032 A CN115254032 A CN 115254032A
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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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/02—Treating gases
Abstract
The invention belongs to the technical field of nuclear air purification, and relates to ionic liquid immobilized activated carbon and a preparation method thereof. The preparation method comprises the following steps: preparing an ionic liquid; (2) pretreating an active carbon carrier; and (3) loading the ionic liquid. By utilizing the ionic liquid immobilized activated carbon and the preparation method thereof, the prepared adsorbing material can be used in14CO2When the catalyst is used for trapping, the catalyst has excellent high-temperature stability and high acid atmosphere tolerance, and has good trapping effect.
Description
Technical Field
The invention belongs to the technical field of nuclear air purification, and relates to ionic liquid immobilized activated carbon and a preparation method thereof.
Background
Under the normal operation condition of the nuclear power station, the radioactive waste gas released to the environment contains Ar, kr, xe, I, sr, cs,3H、14C, etc. nuclides of which14C and3the discharge amount of H is maximum and reaches 1012Bq/a.14C has become the nuclear plant operating normally with the radioactive effluent having the largest contribution to the surrounding public annual effective dose, with a dose contribution ratio exceeding 50%.
14C has a half-life of 5730a and will persist for a long time after entering the ecosystem. Because the carbon has the same physical and chemical properties with common carbon and has stronger mobility in natural environment,14c can be widely involved in the biological chain and food chain in nature; in addition, the method14C is a pure beta nuclide, has large internal irradiation hazard, can be accumulated in the body through inhalation or ingestion, participates in the metabolic process of the human body and enters tissue molecules to cause cell mutation and/or cell death, and poses serious threat to the health safety of the public.
14The C gaseous effluent exists mainly in two forms: to be provided with14CO2Predominantly of carbon oxides and14CH4predominantly paraffinic compounds. For the14CH4Isoalkanes are generally oxidized to give them14CO2Then the oxidation product is treated again14CO2And (4) collecting. Therefore, the number of the first and second electrodes is increased,14CO2is that14C final to-be-treated form of gaseous effluent.
At present, no gas state is equipped in domestic under-construction and on-transport units14C radioactive effluent treatment plants, and the related treatment technologies are also less studied. Although the nuclear facilities are in the normal operation process at the present stage14The annual emission of C meets the limit value specified in the national standard 'environmental radiation regulations of nuclear power plants', but the long-term operation of nuclear facilities is considered14The cumulative effect of C, the long term non-intervention discharge, necessarily causes "chronic" toxic effects on the environment and organisms surrounding the nuclear facility. In addition, hundreds of tons of post-treatment plants are about to be constructed in China, and a great amount of high-concentration spent fuel rods are released in the shearing and dissolving processes of post-treatment14C, gaseous effluent, expected to far exceed the limits imposed by the existing standards.
Compared with a chemical reaction method and a liquid absorption method, the solid adsorption method has simple principle, high trapping efficiency and easy disposal of waste, and is ideal14CO2And (4) a trapping process. The solid adsorbent is the key of a solid adsorption method, and is a targeted research and development method for high-temperature and high-acid environments possibly occurring in nuclear power plants and post-treatment plants14CO2An adsorbent material is necessary.
Disclosure of Invention
The invention aims to provide a preparation method of ionic liquid immobilized activated carbon, so that the prepared adsorbing material can be used for14CO2When the catalyst is used for trapping, the catalyst has excellent high-temperature stability and high acid atmosphere tolerance, and has a good trapping effect.
To achieve the object, in a basic embodiment, the present invention provides a method for preparing an ionic liquid immobilized activated carbon, the method comprising the steps of:
(1) Preparing an ionic liquid: adding amine substances into a reaction vessel, introducing protective gas nitrogen, then adding an acidic solution for reaction, and cooling to room temperature to obtain ionic liquid for loading;
(2) Pretreatment of an activated carbon carrier: mixing activated carbon and deionized water according to a certain volume ratio, ultrasonically cleaning, filtering, and drying the obtained cleaned activated carbon to obtain an activated carbon carrier;
(3) Loading ionic liquid: and (2) uniformly mixing the ionic liquid for loading prepared in the step (1) with an organic solvent according to a certain mass ratio, then adding the activated carbon carrier prepared in the step (2) for further uniform mixing, and drying to obtain the ionic liquid immobilized activated carbon.
In a preferred embodiment, the present invention provides a method for producing an ionic liquid-supported activated carbon, wherein in step (1),
adding amine substances into a reaction vessel, and introducing protective gas nitrogen at the temperature of 0-30 ℃;
adding acid solution to react at 10-100 deg.c for 0.5-30 hr.
In a preferred embodiment, the present invention provides a method for preparing an ionic liquid immobilized activated carbon, wherein in step (1),
the amine substance is selected from one or more of triethylene diamine, hexamethylene tetramine, trimethylene tetramine, diethanol amine and N-dimethyl-p-phenylenediamine;
the acidic solution is selected from one or more of lysine, nitric acid, lactic acid, fluoroboric acid and hydrofluoric acid.
In a preferred embodiment, the present invention provides a method for preparing an ionic liquid immobilized activated carbon, wherein in the step (1), the molar ratio of the amine substance to the acid in the acidic solution is 1.
In a preferred embodiment, the invention provides a preparation method of ionic liquid immobilized activated carbon, wherein in the step (2), the activated carbon and deionized water are mixed according to a certain volume ratio, ultrasonically cleaned and filtered for one or more times; the volume ratio of the activated carbon to the deionized water is 1.
In a preferred embodiment, the present invention provides a method for preparing an ionic liquid immobilized activated carbon, wherein in the step (2), the drying temperature is 80-200 ℃.
In a preferred embodiment, the invention provides a preparation method of ionic liquid immobilized activated carbon, wherein in the step (3), the organic solvent is selected from one or more of methanol, ethanol and acetone.
In a preferred embodiment, the present invention provides a method for producing an ionic liquid-supported activated carbon, wherein in step (3),
mixing the ionic liquid for loading and the organic solvent according to the mass ratio of 1.05-200 to obtain a mixed solution;
the mass ratio of the active carbon carrier to the mixed solution is 1;
the drying temperature is 5-200 ℃.
In a preferred embodiment, the invention provides a preparation method of ionic liquid immobilized activated carbon, wherein the ash content of the activated carbon carrier prepared in the step (2) is less than 10%, the strength is more than 90%, the water content is less than 10%, the particle size is less than 4 meshes, and the ignition point is higher than 400 ℃.
The second purpose of the invention is to provide an ionic liquid immobilized activated carbon which can be used in14CO2When the catalyst is used for trapping, the catalyst has excellent high-temperature stability and high acid atmosphere tolerance, and has good trapping effect.
To achieve this object, in a basic embodiment, the present invention provides an ionic liquid-supported activated carbon prepared by the preparation method according to the foregoing.
The invention has the beneficial effects that the prepared adsorbing material can be used for preparing the ionic liquid immobilized activated carbon and the preparation method thereof14CO2When collected, has an excellent heightTemperature stability and high acid atmosphere tolerance, and has good trapping effect.
The preparation method of the invention loads the amino ionic liquid on the active carbon, is simple and easy to implement, has easily obtained raw materials, and has wide industrial application prospect.
Drawings
FIG. 1 shows CO before and after the ionic liquid immobilized active carbon2Adsorption and desorption curves.
FIG. 2 shows the ultra-low partial pressure (0.01P)0Below) CO before and after the ionic liquid immobilized activated carbon2Adsorption profile.
FIG. 3 shows CO before and after irradiation of ionic liquid immobilized activated carbon2Adsorption and desorption curves.
Fig. 4 is a graph of adsorption performance of ionic liquid immobilized activated carbon under different NO concentration conditions.
Detailed Description
The following description will further describe embodiments of the present invention with reference to the accompanying drawings.
Example 1: preparation of ionic liquid immobilized active carbon
The temperature was controlled at 5 ℃ while introducing a protective gas, nitrogen, into the reaction vessel. 1mol of trimethylenetetramine is put into a reaction vessel, 1mol of nitric acid is dripped into the reaction vessel at a constant speed, and the solution is uniformly mixed by magnetic stirring. After the dropwise addition of the acidic solution was completed, the temperature was raised to 25 ℃ and the reaction was carried out for 10 hours. And naturally cooling to room temperature after the reaction is finished to obtain the ionic liquid for loading.
Uniformly mixing activated carbon and deionized water according to the volume ratio of 1.5, filtering the activated carbon after ultrasonic cleaning, and repeatedly carrying out ultrasonic cleaning-filtering steps for multiple times. Then placing the activated carbon in a container for drying at 150 ℃ to prepare the activated carbon carrier.
And uniformly mixing the ionic liquid for loading with anhydrous methanol according to a mass ratio of 1. Then uniformly mixing the mixed solution with an activated carbon carrier according to the mass ratio of 114CO2The ionic liquid of (3) is immobilized with active carbon.
Example 2: detection of ionic liquid immobilized activated carbon
The ionic liquid immobilized activated carbon prepared in the embodiment 1 is subjected to related detection, and the detection method and the detection result are as follows:
determination of adsorbent CO by utilizing Kangta Autosorb iQ full-automatic gas adsorption analyzer2The adsorption capacity, before the adsorption and desorption isotherm measurement, the adsorbent sample is degassed for 12h at 403K0Values were determined by Station mode. P0The value was 91.92kpa (698 mm hg), the test temperature was 273K, and this was achieved by filling a dewar with an ice-water mixture.
FIG. 1 shows CO before and after loading of activated carbon with ionic liquid2The adsorption and desorption curve shows that although the adsorption capacity of the pure activated carbon is higher, the adsorption and desorption curve is completely closed, namely the activated carbon is used for CO2The adsorption of (2) belongs to physical adsorption; after the active carbon is loaded with the ionic liquid, the adsorption performance of the ionic liquid immobilized active carbon is 0-0.2P0Internal significant promotion, and is in the range of 0.2-1P0The internal adsorption performance is slightly reduced (mainly related to the blockage of partial pore structures of the activated carbon caused by the ionic liquid loading), but the absorption and desorption curves have obvious non-coincidence phenomenon (the absorption and desorption curves are not closed mainly because of the ionic liquid and CO2Chemical reaction occurs between the two to generate CO2Gas can not be completely desorbed, namely the non-closed region corresponds to the part of the composite material subjected to chemical adsorption), the chemical adsorption capacity of the activated carbon is increased from 0 to 25cc/g after the ionic liquid is loaded, and the ionic liquid is used for loading the activated carbon at 0-0.2P0The increase in adsorption performance is largely due to the dominance of chemisorption.
In addition, the ionic liquid immobilized activated carbon is mainly chemisorbed and has ultralow partial pressure of 0.01P0Adsorption Performance of (P)0The value was 91.92kpa (698 mm hg) and the test temperature was 273K) which was more than 10 times that of activated carbon (figure 2), which is an extremely low concentration in adsorption core facilities14CO2Is extremely critical.
Meanwhile, in order to investigate the irradiation stability of the ionic liquid immobilized active carbon, the ionic liquid immobilized active carbon is utilized60Co is subjected to 106Irradiation at Gy doseAnd analyzed for before and after irradiation (P)0The value was 91.92kpa (698 mm hg) and the test temperature was 273K). The result shows that the loaded irradiation dose value is high and belongs to a relatively extreme condition, the performance of the composite material is reduced after irradiation, but the adsorption performance can still be kept about 60 percent, which indicates that the ionic liquid immobilized active carbon has good irradiation resistance stability (figure 3) and has good adsorption radioactivity14CO2The capacity of the gas.
The acid resistance of the ionic liquid immobilized activated carbon is researched through penetration experiments. Firstly, 2g of ionic liquid immobilized activated carbon sample is added into a quartz tube and supported by quartz cotton, and the outside of the quartz tube is wrapped by a heating belt to control the temperature. Introducing 500ppm NO and 5vol% CO at 303K2And balance N2The total flow rate of the mixed gas of (4) was controlled to be 20ml/min. Detection of CO in outlet gas by gas chromatograph2The concentration was calculated, and the sample adsorption amount was calculated according to the following formula.
Wherein q istIs CO2Adsorption capacity (mmol/g); m is the mass (g) of the ionic liquid immobilized active carbon sample; q is the flow rate (mL/min) of the mixed gas; t is a unit of0273K; t is 303K; vm22.4mL/mmol; c0And CtRespectively as inlet and outlet CO2Volume content. The results are shown in fig. 4, which shows that the increase in NO concentration has little effect on the adsorption performance of the ionic liquid-supported activated carbon.
The above-described embodiments are merely illustrative of the present invention, which may be embodied in other specific forms or in other specific forms without departing from the spirit or essential characteristics thereof. The described embodiments are, therefore, to be considered in all respects as illustrative and not restrictive. The scope of the invention should be indicated by the appended claims, and any changes that are equivalent to the intent and scope of the claims are also intended to be included within the scope of the invention.
Claims (10)
1. The preparation method of the ionic liquid immobilized activated carbon is characterized by comprising the following steps:
(1) Preparing an ionic liquid: adding amine substances into a reaction vessel, introducing protective gas nitrogen, then adding an acidic solution for reaction, and cooling to room temperature to obtain ionic liquid for loading;
(2) Pretreatment of an activated carbon carrier: mixing activated carbon and deionized water according to a certain volume ratio, ultrasonically cleaning, filtering, and drying the obtained cleaned activated carbon to obtain an activated carbon carrier;
(3) Ionic liquid loading: and (3) uniformly mixing the ionic liquid for loading prepared in the step (1) with an organic solvent according to a certain mass ratio, then adding the activated carbon carrier prepared in the step (2) for further uniform mixing, and drying to prepare the ionic liquid immobilized activated carbon.
2. The production method according to claim 1, characterized in that: in the step (1), the step (c),
adding amine substances into a reaction vessel, and introducing protective gas nitrogen at the temperature of 0-30 ℃;
adding acid solution to react at 10-100 deg.c for 0.5-30 hr.
3. The production method according to claim 1, characterized in that: in the step (1), the step (c),
the amine substance is selected from one or more of triethylene diamine, hexamethylene tetramine, trimethylene tetramine, diethanol amine and N-dimethyl-p-phenylenediamine;
the acidic solution is selected from one or more of lysine, nitric acid, lactic acid, fluoroboric acid and hydrofluoric acid.
4. The method of claim 1, wherein: in the step (1), the molar ratio of the amine substance to the acid in the acidic solution is 1.
5. The method of claim 1, wherein: in the step (2), mixing activated carbon and deionized water according to a certain volume ratio, ultrasonically cleaning, and filtering for one or more times; the volume ratio of the activated carbon to the deionized water is 1.
6. The method of claim 1, wherein: in the step (2), the drying temperature is 80-200 ℃.
7. The method of claim 1, wherein: in the step (3), the organic solvent is selected from one or more of methanol, ethanol and acetone.
8. The method of claim 1, wherein: in the step (3), the step (c),
mixing the ionic liquid for loading and the organic solvent according to the mass ratio of 1.05-200 to obtain a mixed solution;
the mass ratio of the active carbon carrier to the mixed solution is 1;
the drying temperature is 5-200 ℃.
9. The method of claim 1, wherein: the ash content of the activated carbon carrier prepared in the step (2) is less than 10%, the strength is more than 90%, the water content is less than 10%, the particle size is less than 4 meshes, and the ignition point is higher than 400 ℃.
10. An ionic liquid immobilized activated carbon is characterized in that: the ionic liquid immobilized activated carbon is prepared by the preparation method according to any one of claims 1 to 9.
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