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CN112117020B - Method for treating tritium water by photo-thermal concerted catalysis - Google Patents

Method for treating tritium water by photo-thermal concerted catalysis Download PDF

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CN112117020B
CN112117020B CN202010944213.5A CN202010944213A CN112117020B CN 112117020 B CN112117020 B CN 112117020B CN 202010944213 A CN202010944213 A CN 202010944213A CN 112117020 B CN112117020 B CN 112117020B
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catalyst
water
reactor
photo
tritium
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CN112117020A (en
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岳磊
李佳懋
肖成建
龚宇
侯京伟
付小龙
冉光明
陈超
王和义
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
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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
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/42—Platinum
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44—Palladium
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
    • B01J23/8913—Cobalt and noble metals
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • 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
    • G21F9/04—Treating liquids
    • G21F9/20—Disposal of liquid waste

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Abstract

The invention discloses a method for treating tritiated water by photo-thermal concerted catalysis, which adopts a semiconductor material with response to ultraviolet light as a catalyst carrier such as TiO 2 ，Co 3 O 4 And the like, a light source is introduced to assist thermal catalysis, so that the reaction temperature is reduced, and the tritium water is quickly treated at a lower temperature. The method can be applied to the places where tritium water is generated, such as fusion devices, nuclear power plants and the like.

Description

Method for treating tritium water through photo-thermal concerted catalysis
Technical Field
The invention belongs to the field of radioactive waste treatment, and particularly relates to a method for treating tritium water by photo-thermal concerted catalysis.
Background
For tritium water treatment, VPCE, LPCE and CECE are currently commonly used treatment methods, and H is utilized as the core 2 And (3) replacing tritium in the tritium-containing water to finish tritium removal treatment of the tritium-containing water. However, to increase the efficiency of the replacement, H 2 The ratio to tritiated water is often 3: 1 or higher, so that tritium is displaced in H 2 Is diluted, resulting in an increased burden on the isotope separation unit. In addition, VPCE is generally operated at about 200 ℃, energy consumption is large, LPCE relates to preparation of a hydrophobic catalyst, the process is complicated, the catalyst is easily covered by liquid water to be deactivated, CECE needs to be introduced into electrolysis equipment, and energy consumption is also too high.
In recent years, scholars replace hydrogen isotope exchange reaction with water vapor exchange reaction without introducing H 2 So that the HT produced is not diluted. Water-vapor transformation reaction: HTO + CO → CO 2 And + HT, the reaction principle is that a certain amount of CO is introduced, and T of the tritiated water is replaced, so that tritium removal operation of the tritiated water is realized. The catalyst used in the reaction is a conventional hydrophilic catalyst, and has the advantages of simple preparation and high stability.
For the water-vapor shift reaction, the reaction is exothermic from a thermodynamic point of view, i.e., the equilibrium conversion decreases as the temperature increases, so that a lower reaction temperature is advantageous for obtaining a higher conversion. In addition, because tritium is radioactive, it easily permeates into the environment through the container wall under high temperature conditions, causing radioactive contamination, and thus lower operating temperatures are safer. However, from the aspect of dynamics, the temperature is reduced, the chemical reaction rate is reduced, and the high-efficiency treatment of the tritiated water is difficult to realize in engineering application. Therefore, the conventional technology at present cannot simultaneously meet the requirements of high conversion rate, low tritium permeation quantity and high reaction rate when the tritium water is treated by adopting a water-vapor shift reaction.
Disclosure of Invention
In order to overcome the problem of slow reaction rate under the low temperature condition (50-150 ℃), the invention provides a method for treating tritiated water by photo-thermal concerted catalysis.
The following technical scheme is adopted specifically:
a method for treating tritium water by photo-thermal concerted catalysis is characterized by comprising the following steps:
a. uniformly mixing a catalyst and an adsorbent, adding the mixture into a reactor, turning on a heater, and heating the reactor;
b. converting tritium water HTO into water vapor and CO through a gasifier, uniformly mixing, and introducing into a reactor;
c. arranging a xenon lamp above a transparent window at the central position of the upper end surface of the reactor, turning on the xenon lamp and providing a light source for the reactor;
when the light source irradiates the surface of the catalyst, a catalyst defect structure is formed, and water vapor activation is promoted; CO molecules activated on the surface of the catalyst and water molecules generate a water-vapor transformation reaction to generate a product CO 2 And HT; the reaction process is characterized in that xenon lamp irradiates the surface of the catalyst, electrons of the catalyst jump from a valence band to a conduction band position, and photo-generated electrons e are formed in the conduction band - Formation of photogenerated holes h in the valence band + And inducing the generation of oxygen vacancies O v (ii) a Photoproduction electrons are transferred to the surface of Pt to promote CO activation, tritium water molecules are adsorbed on oxygen vacancies to be activated, the activated CO and the tritium water molecules are combined to generate a formic acid intermediate, and the formic acid intermediate is heated to be decomposed into CO 2 And HT, product CO 2 And the product HT flows out of the reactor.
Further, the light source wavelength of the xenon lamp is 300-700 nm, and the power is 100-300W;
furthermore, the transparent window material of reactor is organic glass to the light source gets into inside the reactor.
Furthermore, the catalyst is a supported catalyst, and the carrier of the supported catalyst is TiO 2 Or Co 3 O 4 And the supported metal is Pt or Pd. For semiconductor carrier TiO 2 、Co 3 O 4 The light irradiation semiconductor carrier promotes the light irradiation semiconductor carrier to generate oxygen vacancy, the oxygen vacancy is greatly beneficial to the dissociation process of water molecules in the reaction rate determining step, and the activity of the catalyst can be obviously improved.
Further, the adsorbent is lithium orthosilicate or calcium oxide;
further, the temperature of the reactor in the step (a) is 50-150 ℃.
The invention uses a semiconductor material responsive to ultraviolet light as a catalyst support such as TiO 2 ，Co 3 O 4 And introducing a light source for assisting thermal catalysis, reducing the reaction temperature and realizing the rapid treatment of tritiated water at the temperature close to normal temperature. The method can be applied to the places where tritium water is generated, such as fusion devices, nuclear power plants and the like.
Drawings
FIG. 1 is a schematic view of an apparatus for photo-thermal concerted catalytic treatment of tritiated water according to the present invention;
FIG. 2 is a schematic diagram of photo-thermal concerted catalytic treatment of tritiated water according to example 1;
in the figure, 1, a heater 2, a vaporizer 3, a reactor 4, a xenon lamp 5, a catalyst 6 and an adsorbent.
Detailed Description
The invention is explained in more detail below with reference to the figures and the examples.
Based on the device for treating tritium water by photo-thermal concerted catalysis shown in figure 1, the method for treating tritium water by photo-thermal concerted catalysis comprises the following steps:
a. uniformly mixing a catalyst 5 and an adsorbent 6, adding the mixture into a reactor 3, turning on a heater 1, and heating the reactor;
b. converting tritium water HTO into water vapor and CO through a gasifier 2, uniformly mixing, and introducing into a reactor 3;
c. arranging a xenon lamp 4 above a transparent window at the central position of the upper end surface of the reactor 3, turning on the xenon lamp 4 and providing a light source for the reactor 3; when the light source irradiates the surface of the catalyst 5, a catalyst defect structure is formed, and water vapor activation is promoted; CO molecules and moisture activated on catalyst surfaceThe seed undergoes a water-gas shift reaction to produce CO 2 And HT; the reaction process is specifically that the xenon lamp 4 irradiates the surface of the catalyst 5, the catalyst electron jumps from a valence band to a conduction band position, and a photo-generated electron e is formed in the conduction band - Formation of photogenerated holes h in the valence band + And inducing the generation of oxygen vacancies O v (ii) a Photoproduction electrons are transferred to the surface of Pt to promote CO activation, tritium water molecules are adsorbed on oxygen vacancies to be activated, the activated CO and the tritium water molecules are combined to generate a formic acid intermediate, and the formic acid intermediate is heated to be decomposed into CO 2 And HT, product CO 2 Is adsorbed and removed after contacting with the adsorbent 6, and a product HT flows out of the reactor 3.
The invention employs a semiconductor material responsive to ultraviolet light as a catalyst support such as TiO 2 ，Co 3 O 4 And introducing a light source for assisting thermal catalysis, reducing the reaction temperature and realizing the rapid treatment of tritiated water at the temperature close to normal temperature. The method can be applied to places where tritium water is generated, such as fusion devices, nuclear power stations and the like.
Further, the light source wavelength of the xenon lamp 4 is 300-700 nm, and the power is 100-300W;
further, the transparent window of the reactor 3 is made of organic glass, so that the light source can enter the reactor.
Further, the catalyst 5 is a supported catalyst, and the carrier of the supported catalyst is TiO 2 Or Co 3 O 4 And the supported metal is Pt or Pd. For semiconductor carrier TiO 2 、Co 3 O 4 The light irradiation semiconductor carrier promotes the light irradiation semiconductor carrier to generate oxygen vacancy, the oxygen vacancy is greatly beneficial to the dissociation process of water molecules in the reaction rate determining step, and the activity of the catalyst can be obviously improved.
Further, the adsorbent 6 is lithium orthosilicate or calcium oxide;
further, the temperature of the reactor in the step a is 50-150 ℃.
The method of the invention can obviously improve the activity of the water-gas shift reaction catalyst. Oxygen vacancies, a common defect structure of catalysts, can be used to activate water molecules, which then participate in chemical reactions with them. Conventional thermal catalysis, which requires high temperatures of greater than 1000 ℃ to generate oxygen vacancies in metal oxides, is clearly not applicable in the field of tritium water treatment. The catalyst can generate a large amount of oxygen vacancies at the temperature of between 50 and 150 ℃ after the light source is introduced. The invention realizes the water-vapor transformation reaction at the near normal temperature by means of light source assisted thermal catalysis, and can realize safe, efficient and rapid treatment of tritium water.
Example 1
With Pt/TiO 2 The catalyst is used for example for photo-thermal concerted catalysis treatment of tritiated water, and the specific principle is as shown in figure 2, wherein the method comprises the following steps:
a. catalyst Pt/TiO 2 Uniformly mixing with lithium orthosilicate adsorbent according to the ratio of 2: 1, adding into a reactor (3), turning on a heater (1), heating the reactor, and setting the temperature at 100 ℃;
b. tritiated water HTO is changed into water vapor through a gasifier (2), and is uniformly mixed with CO according to the ratio of 1: 1, and then the mixture is introduced into a reactor (3);
c. arranging a xenon lamp above the transparent window at the central position of the upper end surface of the reactor, turning on the xenon lamp and providing a light source for the reactor (3); when the light source irradiates on the catalyst Pt/TiO 2 When the surface is coated, a catalyst defect structure is formed, and water vapor activation is promoted; CO molecules activated on the surface of the catalyst and HTO molecules generate water-vapor transformation reaction to generate a product CO 2 And HT. The reaction process is concretely that a xenon lamp (4) irradiates on a catalyst Pt/TiO 2 (5) Surface, catalyst support TiO 2 The electrons transit from the valence band to the conduction band position to form a photogenerated electron e in the conduction band - Formation of photogenerated holes h in the valence band + And inducing the generation of oxygen vacancies O v The reaction formula is TiO 2 →TiO 2-x +O v +x/2O 2 (ii) a Photoproduction electrons are transferred to the surface of Pt to promote CO activation, and HTO molecules are adsorbed on TiO 2 Activating oxygen vacancy, combining CO and HTO molecules after activation to generate formic acid intermediate HCOOT, and decomposing into CO by heating 2 And HT, product CO 2 Is adsorbed and removed after contacting with the adsorbent lithium orthosilicate (6), and a product HT flows out of the reactor (3).
Under the condition, the reaction conversion rate is 80.4 percent, the reaction rate of tritium water is 42mmol/min, and the tritium permeation rate is highCalculated rate was 3.95X 10 -11 mol·m -2 ·s -1
Example 2
The xenon lamp in the step c of example 1 was turned off, the other conditions were unchanged, the reaction conversion rate was 1.8%, the tritium-water reaction rate was 0.9mmol/min, and the calculated tritium permeation rate was 3.95 × 10 -11 mol·m -2 ·s -1 。
Example 3
The reaction temperature in example 2 was adjusted to 300 ℃ and the other conditions were unchanged, resulting in a reaction conversion of 30.6%, a tritium-water reaction rate of 16mmol/min and a calculated tritium permeation rate of 3.41X 10 -8 mol·m -2 ·s -1 。
Therefore, the invention can realize higher tritium-water conversion rate at lower temperature, and simultaneously keep lower tritium permeation rate.

Claims (5)

1. A method for treating tritium water by photo-thermal concerted catalysis is characterized by comprising the following steps:
a. uniformly mixing a catalyst (5) and an adsorbent (6), adding the mixture into a reactor (3), turning on a heater (1), and heating the reactor; the catalyst (5) is a supported catalyst, the carrier of the catalyst (5) is a TiO2 or Co3O4 semiconductor, and the supported metal is Pt or Pd;
b. tritium water HTO is changed into water vapor through a gasifier (2), and is uniformly mixed with CO and then is introduced into a reactor (3);
c. arranging a xenon lamp (4) above a transparent window at the central position of the upper end surface of the reactor (3), turning on the xenon lamp (4), and providing a light source for the reactor (3); when a light source irradiates the surface of the catalyst (5), the catalyst (5) forms a defect structure to promote water vapor activation; CO molecules activated on the surface of the catalyst and water molecules are subjected to water-vapor transformation reaction to generate a product CO 2 And HT; the reaction process is concretely characterized in that a xenon lamp (4) irradiates the surface of a catalyst (5), the electrons of the catalyst jump from a valence band to a conduction band position, and photo-generated electrons e are formed in the conduction band - Formation of photogenerated holes h in the valence band + And inducing the generation of oxygen vacancies O v (ii) a Photoproduction electrons are transferred to the surface of Pt or Pd to promote CO activation, tritiated water molecules are adsorbed on oxygen vacancies to be activated, CO and the tritiated water molecules are combined to generate a formic acid intermediate after activation, and the formic acid intermediate is heated to be decomposed into CO 2 And HT, product CO 2 Is adsorbed and removed after contacting with the adsorbent (6), and a product HT flows out of the reactor (3).
2. The photothermal concerted catalysis tritiated water treatment method according to claim 1, characterized in that the light source wavelength of the xenon lamp (4) is 300-700 nm, and the power is 100-300W.
3. The photo-thermal concerted catalysis tritium water treatment method according to claim 1, characterized in that the transparent window of the reactor (3) is made of organic glass so that a light source can enter the reactor.
4. Photothermal concerted catalytic treatment of tritiated water according to claim 1, characterized in that the adsorbent (6) is lithium orthosilicate or calcium oxide.
5. A method for treating tritium water by photo-thermal concerted catalysis according to claim 1, characterized in that the reactor temperature in step a is heated to 50-150 ℃.
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