CN104383917A - Preparation method of catalyst for removing tritium in tritium-containing air - Google Patents
Preparation method of catalyst for removing tritium in tritium-containing air Download PDFInfo
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Abstract
A disclosed preparation method of a catalyst for removing tritium in tritium-containing air comprises: (1) adding aluminium isopropoxide into distilled water and stirring for hydrolysis; (2) adding a peptizing agent to enable the hydrolysis solution to be colloidal, and performing stirring refluxing to obtain an aluminium oxide sol; (3) using honeycomb ceramic as a catalyst matrix and immersing in a diluted nitric acid solution, and then taking out, cleaning and baking; (4) mixing active aluminium oxide powder and the aluminium oxide sol, and performing ball milling to form a slurry; (5) uniformly coating the catalyst matrix with the slurry, and then baking and weighing; (6) repeating the step (5) until the weight gain of the catalyst matrix is 12%-20%; (7) adding diluted nitric acid into a noble metal solution, and mixing with stirring; and (8) immersing the catalyst matrix in the mixed solution to enable the catalyst matrix to absorb the mixed solution to reach a saturation state, and then roasting, so as to obtain the catalyst. The preparation method helps to substantially improve the processing capacity of the catalyst on gases without increasing the gas resistance of the tritium-removal system.
Description
Technical field
The present invention relates to a kind of catalyst, that be specifically related to is a kind of preparation method for the catalyst containing tritium air detritiation.
Background technology
Tritium belongs to the one of hydrogen isotope, and it is a kind of strategic material, not only expensive, and is not easy to obtain; Meanwhile, tritium is the radionuclide that a kind of animal migration is very strong, and its leakage not only to environment, and can also have very large harm to human body.So every technique relating to tritium operation must perform strict radiation protection and environmental emission requirement.According to current security concepts, tritium facility should set up triple containing system, adopts physical shielding and the mode that combines except tritium cleaning to solve the problem that tritium is inclusive with validity simultaneously.Purifying containing tritium gas atmosphere, is the necessary means setting up safety in production, and meanwhile, the tritium reclaimed wherein also can improve the utilization ratio of tritium.At present, no matter be that built or in design planning large-scale tritium facility, mostly adopt catalytic oxidation to add the technique of absorption detritiation, wherein catalyst performance is the key factor realizing efficient detritiation.
At present, in detritiation field, what substantially still adopt both at home and abroad is the noble metal catalyst such as spherical particle type palladium (Pd), platinum (Pt) using activated alumina as carrier, such catalyst has a wide range of applications in civilian industry, past is for containing the purification of tritium air or all kinds of design except tritium system, just directly have employed ready-made technique and technology, do not develop the catalyst of special tritium cleaning.
Traditional containing tritium air except the catalyst of tritium system is the activated alumina (γ-Al of 3 ~ 4mm usually by diameter
2o
3) bead is as carrier, the load of Pt, Pd isoreactivity component is on carrier.Such catalyst have mechanical strength high, manufacture simple, cheap, load the advantages such as easy.But, because pellet type catalyst thermal capacity is large and adopt closs packing type of feed, thus also increases the vapour lock except tritium system, cause gas processing capability to decline.Meanwhile, pelleted substrate is easy to efflorescence of wearing and tearing, and Long-Time Service easily causes the blocking except tritium system, further increases system vapour lock so especially.
Summary of the invention
The object of the present invention is to provide a kind of preparation method for the catalyst containing tritium air detritiation, mainly solve the problem that existing detritiation catalyst easily causes detritiation system vapour lock to increase.
To achieve these goals, the technical solution used in the present invention is as follows:
For a preparation method for the catalyst containing tritium air detritiation, comprise the following steps:
(1) aluminium isopropoxide is joined in distilled water and stir hydrolysis, form hydrating solution, then remove the alcohol that hydrolysis produces;
(2) add peptizing agent, make hydrating solution form glue, and its pH value is 2 ~ 2.5, then stirring and refluxing 2 ~ 3h, obtains alumina sol;
(3) ceramic honey comb is soaked 20 ~ 24h as catalyst matrix in the dilute nitric acid solution of 5% ~ 10%, then take out cleaning, dry;
(4) active alumina powder is become slurries with alumina sol mixing and ball milling;
(5) joined in ultrasonic cleaner together with slurries by the catalyst matrix after oven dry, and carry out ultrasonic wave added coating under ultrasonic vibration condition, slurries are evenly coated on catalyst matrix, then take out oven dry, catalyst matrix weight is increased;
(6) step (5) is repeated, until catalyst matrix weightening finish 12% ~ 20%;
(7) at mass fraction be 0.3% ~ 0.5% precious metal solution in add dust technology mix and blend, make the pH value of mixed liquor be adjusted to 1.5 ~ 2;
(8) catalyst matrix is immersed in the mixed liquor that step (7) prepares, until catalyst matrix sucks mixed liquor and the state that reaches capacity, then after oven dry catalyst matrix, is carried out roasting, obtain catalyst.
Further, the peptizing agent in described step (2) is dust technology.
Again further, the ceramic honey comb in described step (3) is cordierite honeycomb ceramic, and its pore structure is regular hexagon, and its hole density specification is 400cpsi.
Specifically, the preparation process of the active alumina powder in described step (4) is as follows:
A aluminum nitrate is dissolved in distilled water and stirs and be mixed with the solution that concentration is 0.1mol/L by (), and add dispersant successively and ammonia spirit mix and blend is precipitated, then standing, ageing 20 ~ 24h, wherein, the dispersant quality added is 0.5% ~ 2% of aluminum nitrate quality, ammoniacal liquor in ammonia spirit and the volume ratio of water are 1: 1, and the pH value of mixed liquor is 9 ~ 9.5;
B () utilizes distilled water precipitation to be cleaned, remove nitrate ion wherein, then the precipitation polyglycol solution obtained is soaked 20 ~ 24h;
C () utilizes distilled water precipitation to be cleaned again, remove polyethylene glycol wherein, then the precipitation obtained is carried out spraying dry;
D drying is deposited in roasting 2 ~ 3h under the condition of 500 ~ 550 DEG C, obtains active alumina powder by ().
Specifically, the dispersant in described step (a) is polyethylene glycol, and its PEG degree of polymerization is 4000 ~ 10000.
Further, the slurries in described step (4), its aluminum oxide grain size is 300 ~ 1000nm.
Further, the precious metal solution in described step (7) is palladium bichloride or platinum acid chloride solution.
Specifically, described step (8) comprises the following steps:
(8a) take the mixed liquor of precious metal solution and dust technology according to the specification of 2 ~ 4g/L, and catalyst matrix is immersed in the mixed liquor of taking, until this mixed liquor is all inhaled in catalyst matrix, then dry catalyst matrix;
(8b) repeat step (8a), the state until catalyst matrix reaches capacity, then oven dry catalyst matrix after under the condition of 500 ~ 550 DEG C roasting 2 ~ 3h, obtain catalyst.
Compared with prior art, the present invention has following beneficial effect:
(1) present invention process is reasonable, and simple operation is easy to prepare.
(2) the present invention adopts alumina sol as ball milling liquid, then carry out ball milling with active alumina powder and prepare coated carrier, coated carrier prepared by the method, alumina particle distribution rationally, strong with catalyst matrix adhesion, not easily drop, and there is larger specific area and suitable pore structure, the high degree of dispersion of catalyst activity component can be convenient to, increase the contact area containing tritium air and catalyst, thus improve the activity of catalyst, strengthen catalyst to the disposal ability of gas.
(3) the present invention adopts ceramic honey comb material as catalyst matrix, be fixed in the privileged site (catalytic converter) except tritium system in use, due to the design feature that ceramic honey comb has, under thus can bearing air atmosphere in operating conditions, air flow (is generally hundreds of m
3/ more than h) long-term impact, not only durable in use, significantly extend the service life of the catalyst of detritiation system aspects, and there will not be wearing and tearing efflorescence phenomenon.
(4) catalyst that prepared by the present invention has regular alveolate texture, can for fluid by providing uniform duct, one piece of regular catalyst is also a catalytic reaction fixed bed simultaneously, and active constituent loading is on regular catalyst matrix, the high efficiency composition of micro-tritium oxygen under can realizing air atmosphere under normal temperature, its before the reaction gas do not need preheating, cooling is not needed after reaction, therefore, the present invention is applied to and can significantly simplifies its flow scheme design except in tritium system, and optimizes its overall performance.
(5) the present invention adopts cordierite honeycomb ceramic as catalyst matrix, because the matching of this kind of ceramic honey comb and various catalyst activity component is good, and have the advantages that hole wall is thin, geometrical surface is large, thermal coefficient of expansion is little and resistance to sudden heating is good, be thus very suitable for being used in the preparation containing tritium air detritiation catalyst.
(6) the every flow process of the present invention is closely connected, all linked with one another, its obtained catalyst, efficiently solve that existing detritiation system catalyst consumption is large, temperature control is difficult, system gas thwarts engineering problems such as reducing, and rely on the catalyst oxidation reactor of this kind of Catalyst Design, then be applicable to very much the efficient detritiation requirement under larger air speed, therefore, the present invention is adapted at extensive use in air detritiation field.
(7) cost performance of the present invention is high, it has prepared the skeleton catalyst with pellet type catalyst different structure, this kind of catalyst is when being applied in except tritium system, not only the disposal ability of gas is gone up not down, and the phenomenon that system vapour lock increases can not be there is because of Long-Time Service, therefore, the present invention compared with prior art, has outstanding substantive distinguishing features and significant progress.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Fig. 2 is the preparation flow schematic diagram of active alumina powder in the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described, and embodiments of the present invention include but not limited to the following example.
Embodiment
As shown in Figure 1, the invention provides a kind of process preparing catalyst containing tritium air detritiation, its obtained catalyst by active component, carrier and matrix three part form, wherein, matrix is the ceramic monolith block of ordered structure, active component and carrier then with the mode load of coating structure on the internal gutter wall inner surface of matrix, matrix is that coated catalysts plays supporter; Carrier adopts active alumina powder, rises and increases surface area, the effect of dispersion, supported catalyst active component.The process of Kaolinite Preparation of Catalyst of the present invention is as follows:
(1) aluminium isopropoxide is joined in distilled water and stir hydrolysis, form hydrating solution, then remove the alcohol that hydrolysis produces;
(2) add peptizing agent, make hydrating solution form glue, and its pH value is 2 ~ 2.5, then stirring and refluxing 2 ~ 3h, obtains alumina sol;
(3) ceramic honey comb is soaked 20 ~ 24h as catalyst matrix in the dilute nitric acid solution of 5% ~ 10%, then take out cleaning, dry;
(4) active alumina powder is become slurries with alumina sol mixing and ball milling, the aluminum oxide grain size in these slurries is 300 ~ 1000nm;
In this step, active alumina powder can adopt existing technique to obtain, and technique provided by the invention also can be adopted to obtain, and as shown in Figure 2, the process that the present invention prepares active alumina powder is as follows:
A aluminum nitrate is dissolved in distilled water and stirs and be mixed with the solution that concentration is 0.1mol/L by (), and add dispersant successively and ammonia spirit mix and blend is precipitated, then standing, ageing 20 ~ 24h, wherein, the dispersant quality added is 0.5% ~ 2% of aluminum nitrate quality, ammoniacal liquor in ammonia spirit and the volume ratio of water are 1: 1, and the pH value of mixed liquor is 9 ~ 9.5;
B () utilizes distilled water precipitation to be cleaned, remove nitrate ion wherein, then the precipitation polyglycol solution obtained is soaked 20 ~ 24h, so can further facilitate the pore-creating of subsequent technique;
C () utilizes distilled water precipitation to be cleaned again, remove polyethylene glycol wherein, then the precipitation obtained is carried out spraying dry;
D drying is deposited in roasting 2 ~ 3h under the condition of 500 ~ 550 DEG C, obtains active alumina powder by ();
(5) joined in ultrasonic cleaner together with slurries by the catalyst matrix after oven dry, and carry out ultrasonic wave added coating under ultrasonic vibration condition, slurries are evenly coated on catalyst matrix, then take out oven dry, catalyst matrix weight is increased;
(6) step (5) is repeated, until catalyst matrix weightening finish 12% ~ 20%;
(7) at mass fraction be 0.3% ~ 0.5% precious metal solution in add dust technology mix and blend, make the pH value of mixed liquor be adjusted to 1.5 ~ 2;
(8) catalyst matrix is immersed in the mixed liquor that step (7) prepares, until catalyst matrix sucks mixed liquor and the state that reaches capacity, then after oven dry catalyst matrix, is carried out roasting, obtain catalyst.This step can be soaked catalyst matrix in the following way:
(8a) take the mixed liquor of precious metal solution and dust technology according to the specification of 2 ~ 4g/L, and catalyst matrix is immersed in the mixed liquor of taking, until this mixed liquor is all inhaled in catalyst matrix, then dry catalyst matrix;
(8b) repeat step (8a), the state until catalyst matrix reaches capacity, then oven dry catalyst matrix after under the condition of 500 ~ 550 DEG C roasting 2 ~ 3h, obtain catalyst.The catalyst soakage mode that step (8a), (8b) adopt can make mixed liquor be fully utilized on the one hand, matrix then can be made on the other hand to be sucked by mixed liquor very equably, ensure that it follow-uply obtains homogeneous, good looking appearance and the good catalyst of result of use after roasting.
According to above-mentioned technological process, specifically set forth technical scheme of the present invention with several case study on implementation below, and embody excellent properties and the beneficial effect of catalyst prepared by the present invention by the testing experiment of case.
Case 1
Prepared by present case is palladium catalyst, and its preparation process is as follows:
(1) active alumina powder is prepared:
Be that the aluminum nitrate of 18.75g joins in 500mL distilled water and stirs and be made into the solution of 0.1mol/L by quality, then the polyethylene glycol (its PEG degree of polymerization is 4000) of 94mg is added as dispersant, and in whipping process, add ammonia spirit be mixed to get precipitation, the pH value of mixed liquor is adjusted to 9, then continuing stir about 1h makes precipitation even, then standing, ageing 20h.
After ageing, with distilled water by precipitation cleaning twice, and then with mass fraction be 2% polyglycol solution precipitation is soaked 20h, and clean one time with distilled water again, remove most polyethylene glycol in precipitation.Then, precipitation is carried out spraying dry, and under 500 DEG C of conditions roasting 3h, obtain active alumina powder.
(2) alumina sol is prepared:
10g aluminium isopropoxide is joined 90mL, temperature is stir hydrolysis 1h in the distilled water of 80 DEG C, then temperature is increased to 90 DEG C by open container mouth, and the alcohol volatilization that order hydrolysis produces, falls temperature after 1h and be back to 80 DEG C, then drip dust technology plastic, and its pH value is 2.Keep 80 DEG C of stirring and refluxing 3h, obtain the alumina sol of transparent and stable.
(3) catalyst matrix pretreatment:
According to the dimensions cutting cordierite honeycomb ceramic of Φ 10 × 20mm, the pore structure of this cordierite honeycomb ceramic is regular hexagon, and hole density is 400cpsi.The cordierite honeycomb ceramic of well cutting is placed in the dilute nitric acid solution of 5% and soaks 20h, then take out, clean with distilled water and be placed in vacuum drying chamber and dry.
(4) matrix coating:
Using alumina sol as ball milling liquid, and with active alumina powder mixing and ball milling (rotating speed of ball mill is 350r/min), make slurries, then pretreated catalyst matrix is immersed in these slurries, and put in ultrasonic cleaner, under ultrasonic vibration condition, carry out ultrasonic coating 15min.Take out matrix after ultrasonic coating to dry, then weigh, matrix weight is now owing to being coated with slurries, and thus weight can increase.The flow process of this prepared slarry of iterative cycles and ultrasonic coating, until matrix weightening finish 12%.
(5) load active component:
Preparation mass concentration is the palladium bichloride (PdCl of 0.5%
2) solution, and add dust technology mix and blend, its pH value is adjusted to 2.0 stand-by.Then, take the mixed solution mixed up by the load capacity of 2g/L, and immersed in this mixed solution of taking by coated catalyst matrix, after about 15min, mixed liquor is sucked by matrix, then takes out matrix and dries.This step of iterative cycles, the state until catalyst matrix reaches capacity, now, the whole catalyzed matrix of mixed solution sucks.By catalyst matrix roasting 3h under 500 DEG C of conditions, obtain the palladium catalyst of ordered structure.
Shown in table 1 is the test result that the air of palladium catalyst to hydrogeneous (including tritium) prepared by present case carries out catalytic oxidation efficiency, in its test parameters, catalytic bed temperature is respectively 20,40,60,80,100,120 DEG C, Primordial Qi flow velocity is 1L/min, and the hydrogen concentration of Primordial Qi is 8400ppm:
Table 1
As can be seen from Table 1, palladium catalyst prepared by present case, it can reach 99% substantially to the catalytic oxidation efficiency of the air of hydrogeneous and isotope applications, and catalytic bed temperature is higher, stronger to the disposal ability of gas, be even close to 100%, fully met the requirement containing tritium purification of air.
Case 2
Be with the difference of case 1, (1), in the process preparing active alumina powder, the polyethylene glycol quality as dispersant is 300mg, and its PEG degree of polymerization is 10000, and the pH value of mixed liquor is adjusted to 9.5, and still aging 24h.(2) preparing in alumina sol process, drip dust technology plastic in hydrating solution, its pH value is adjusted to 2.5, and stirring and refluxing 2h.(3) in catalyst matrix preprocessing process, cordierite honeycomb ceramic is placed in the dilute nitric acid solution of 10% and soaks 24h.(4) in the process of matrix coating, matrix is applied weightening finish 16%.(5) and in the process of load active component, then prepare the palladium chloride solution of 0.3%, adding dust technology, to mix to PH be 1.5, and then taking mixed solution by the load capacity of 4g/L, is then finally by catalysis matrix roasting 2h under 550 DEG C of conditions.
Equally, shown in table 2 is palladium catalyst prepared by present case carries out catalytic oxidation efficiency test result to hydrogeneous (including tritium) air, in its test parameters, catalytic bed temperature is respectively 20,40,60,80,100,120 DEG C, Primordial Qi flow velocity is 1L/min, and the hydrogen concentration of Primordial Qi is 8400ppm:
Table 2
As can be seen from table 2 equally, palladium catalyst prepared by present case, it can reach 99% substantially to the catalytic oxidation efficiency of the air of hydrogeneous and isotope applications, because the technical specification of existing hydrogen detecting instrument self limits, when tail gas hydrogen concentration is less than 2.5ppm, reach the measurement lower limit of instrument, hydrogen detecting instrument cannot detect real tail gas hydrogen concentration, thus according to other test value, and through reasonable inferences, when catalytic bed temperature is 120 DEG C, the catalytic efficiency of catalyst must be infinitely close to 100%, even likely reaches 100%.Palladium catalyst prepared by present case, its catalytic effect is slightly better than case 1, and is that catalytic bed temperature is higher equally, stronger to the disposal ability of gas, thus equally fully meets the requirement containing tritium purification of air.
Case 3
With case 1,2 unlike, the platinum catalyst of prepared by present case is ordered structure, and be with the difference of case 1, (1) in the process preparing active alumina powder, polyethylene glycol quality as dispersant is 120mg, its PEG degree of polymerization is 6000, and the pH value of mixed liquor is adjusted to 9.3, and still aging 22h.(2) in the process of load active component, then platinum acid chloride solution (the H of 0.5% is prepared
2ptCl
66H
2o), adding dust technology, to mix to PH be 1.8, then takes mixed solution by the load capacity of 4g/L.
Shown in table 3 is platinum catalyst prepared by present case carries out catalytic oxidation efficiency test result to hydrogeneous (including tritium) air, in its test parameters, catalytic bed temperature is respectively 50,80,100,120,140,160 DEG C, Primordial Qi flow velocity is 4L/min, and the hydrogen concentration of Primordial Qi is 8400ppm:
Table 3
As can be seen from Table 3, platinum catalyst prepared by present case, when catalytic bed temperature is at least 50 DEG C, its to the catalytic oxidation efficiency of the air of hydrogeneous and isotope applications substantially more than 99%, and it is the same with case 2, when catalytic bed temperature is more than 140 DEG C, hydrogen detecting instrument cannot detect the actual concentration of tail gas hydrogen, but its rule is that catalytic bed temperature is higher equally, stronger to the disposal ability of gas, and be infinitely close to 100%, particularly after 120 DEG C, catalytic efficiency continues to remain between 99.9% ~ 100%, therefore, fully meet the requirement containing tritium purification of air.
Case 4
What present case was prepared equally is platinum catalyst, and be with the difference of case 1, (1) in the process preparing active alumina powder, polyethylene glycol quality as dispersant is 300mg, its PEG degree of polymerization is 10000, and the pH value of mixed liquor is adjusted to 9.5, and still aging 24h.(2) preparing in alumina sol process, drip dust technology plastic in hydrating solution, its pH value is adjusted to 2.5.(3) in catalyst matrix preprocessing process, cordierite honeycomb ceramic is placed in the dilute nitric acid solution of 10% and soaks 24h.(4) in the process of matrix coating, matrix is applied weightening finish 20%.(5) and in the process of load active component, then prepare the platinum acid chloride solution of 0.4%, adding dust technology, to mix to PH be 1.9, is then finally by catalysis matrix roasting 3h under 550 DEG C of conditions.
Shown in table 4 is platinum catalyst prepared by present case carries out catalytic oxidation efficiency test result to hydrogeneous (including tritium) air, in its test parameters, catalytic bed temperature is respectively 50,80,100,120,140,160 DEG C, Primordial Qi flow velocity is 4L/min, and the hydrogen concentration of Primordial Qi is 8400ppm:
Table 4
As can be seen from table 4 equally, platinum catalyst prepared by present case, when catalytic bed temperature is at least 50 DEG C, it is also maintain more than 99% to the catalytic oxidation efficiency of the air of hydrogeneous and isotope applications, its catalytic effect is slightly better than case 3, and is that catalytic bed temperature is higher equally, stronger to the disposal ability of gas, therefore, present case equally fully meets the requirement containing tritium purification of air.
Catalyst activity prepared by the present invention is high, vapour lock is little, mechanical strength is large, efficiently can remove the tritium containing leaking in tritium closed container, tritium glove box and tritium laboratory at normal temperatures, and therefore, the present invention has very high practical value and application prospect widely.
Case in above-described embodiment is only the several preferably embodiment of the present invention; case study on implementation of the present invention is too numerous to mention; and the detritiation effect after test is all very good; therefore; above-described embodiment is not applied to limit the scope of the invention; and every in any amendment done within spirit and principle, the technical scheme being equal to the improvement replacing and have no essential meaning of designing of the present invention, all should be included within protection scope of the present invention.
Claims (8)
1., for a preparation method for the catalyst containing tritium air detritiation, it is characterized in that, comprise the following steps:
(1) aluminium isopropoxide is joined in distilled water and stir hydrolysis, form hydrating solution, then remove the alcohol that hydrolysis produces;
(2) add peptizing agent, make hydrating solution form glue, and its pH value is 2 ~ 2.5, then stirring and refluxing 2 ~ 3h, obtains alumina sol;
(3) ceramic honey comb is soaked 20 ~ 24h as catalyst matrix in the dilute nitric acid solution of 5% ~ 10%, then take out cleaning, dry;
(4) active alumina powder is become slurries with alumina sol mixing and ball milling;
(5) joined in ultrasonic cleaner together with slurries by the catalyst matrix after oven dry, and carry out ultrasonic wave added coating under ultrasonic vibration condition, slurries are evenly coated on catalyst matrix, then take out oven dry, catalyst matrix weight is increased;
(6) step (5) is repeated, until catalyst matrix weightening finish 12% ~ 20%;
(7) at mass fraction be 0.3% ~ 0.5% precious metal solution in add dust technology mix and blend, make the pH value of mixed liquor be adjusted to 1.5 ~ 2;
(8) catalyst matrix is immersed in the mixed liquor that step (7) prepares, until catalyst matrix sucks mixed liquor and the state that reaches capacity, then after oven dry catalyst matrix, is carried out roasting, obtain catalyst.
2. a kind of preparation method for the catalyst containing tritium air detritiation according to claim 1, it is characterized in that, the peptizing agent in described step (2) is dust technology.
3. a kind of preparation method for the catalyst containing tritium air detritiation according to claim 2, it is characterized in that, ceramic honey comb in described step (3) is cordierite honeycomb ceramic, and its pore structure is regular hexagon, and its hole density specification is 400cpsi.
4. a kind of preparation method for the catalyst containing tritium air detritiation according to claim 3, it is characterized in that, the preparation process of the active alumina powder in described step (4) is as follows:
A aluminum nitrate is dissolved in distilled water and stirs and be mixed with the solution that concentration is 0.1mol/L by (), and add dispersant successively and ammonia spirit mix and blend is precipitated, then standing, ageing 20 ~ 24h, wherein, the dispersant quality added is 0.5% ~ 2% of aluminum nitrate quality, ammoniacal liquor in ammonia spirit and the volume ratio of water are 1: 1, and the pH value of mixed liquor is 9 ~ 9.5;
B () utilizes distilled water precipitation to be cleaned, remove nitrate ion wherein, then the precipitation polyglycol solution obtained is soaked 20 ~ 24h;
C () utilizes distilled water precipitation to be cleaned again, remove polyethylene glycol wherein, then the precipitation obtained is carried out spraying dry;
D drying is deposited in roasting 2 ~ 3h under the condition of 500 ~ 550 DEG C, obtains active alumina powder by ().
5. a kind of preparation method for the catalyst containing tritium air detritiation according to claim 4, it is characterized in that, the dispersant in described step (a) is polyethylene glycol, and its PEG degree of polymerization is 4000 ~ 10000.
6. a kind of preparation method for the catalyst containing tritium air detritiation according to claim 4 or 5, it is characterized in that, the slurries in described step (4), its aluminum oxide grain size is 300 ~ 1000nm.
7. a kind of preparation method for the catalyst containing tritium air detritiation according to claim 6, it is characterized in that, the precious metal solution in described step (7) is palladium bichloride or platinum acid chloride solution.
8. a kind of preparation method for the catalyst containing tritium air detritiation according to claim 7, it is characterized in that, described step (8) comprises the following steps:
(8a) take the mixed liquor of precious metal solution and dust technology according to the specification of 2 ~ 4g/L, and catalyst matrix is immersed in the mixed liquor of taking, until this mixed liquor is all inhaled in catalyst matrix, then dry catalyst matrix;
(8b) repeat step (8a), the state until catalyst matrix reaches capacity, then oven dry catalyst matrix after under the condition of 500 ~ 550 DEG C roasting 2 ~ 3h, obtain catalyst.
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| CN110152732A (en) * | 2019-07-01 | 2019-08-23 | 苏州大学 | Composite catalyst and its preparation and application based on conjugation microporous polymer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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Application publication date: 20150304 |