Vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium sample and using method and collecting system of vertical oxidation combustion device

Abstract

The invention relates to a vertical oxidizing combustion device for sediment or biological radioactive organic carbon tritium samples, a using method of the vertical oxidizing combustion device and a collecting system of the vertical oxidizing combustion device. Comprising a combustion oxidation module which comprises a vertical separable combustion pipe, at least two air inlet pipes, an air entraining part and a heater; the combustion tube comprises a base and a fixed part, the base can be separated from or combined with the fixed part in a lifting mode, and a combustion chamber is arranged in the combustion tube; the gas inlet pipes extend into the combustion chamber from the upper part and the lower part respectively and are used for introducing combustion-supporting gas into the combustion chamber in the vertical direction respectively, so that the combustion-supporting gas forms vortex to promote sufficient combustion of a sample; the air entraining part is arranged at the top of the fixing part and is used for leading out gas formed by sample combustion; the heater sleeves the combustion tube and is used for heating the sample to reach an ignition point and combusting the sample; the system further comprises an oxidation catalysis module and a three-way catalysis module. The combustion device is thorough in combustion and high in gas harmlessness degree.

Description

Technical Field

[0001] The invention relates to a sample combustion collection technology, and in particular to a vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples, a use method thereof and a collection system. Background Art

[0002] Nuclear facilities engaged in radioactive research and production may, under certain circumstances, release a certain amount of tritium (T or 3 H) and 14 C, and cause certain pollution to the environment. Tritium and carbon entering the environment 14 C is mainly composed of HTO and carbon dioxide ( 14 CO2) in the form of natural water and carbon cycles, global biogeochemical cycles and all metabolic processes. 14 C is absorbed by plants and animals and transported here by these animal and plant foods. It is usually measured by monitoring tritium and 14 The content of C is used to assess the area affected by tritium and 14 C. The degree of pollution.

[0003] In recent years, with the development of my country's nuclear energy industry, the tritium and 14 The impact of C on the environment and the public has attracted increasing attention. Therefore, it is necessary to conduct research on environmental organic tritium and 14 C measurement. Currently commonly used tritium and 14 Among the C analysis methods, the analysis of organic tritium carbon is relatively difficult. Usually, the most effective method is to convert the sample into a liquid state and measure it using a liquid scintillation counter. 14 The content of C is low, so it needs to be converted into water and carbon dioxide for enrichment to increase tritium and 14 The existing sample preparation device not only takes a long time to prepare samples, but also has difficulty in taking into account both organic tritium and 14 In order to detect the tritium in sediment or biological radioactive organic carbon samples, 14 The C and tritium content is generally determined by oxidizing and burning the sample under high temperature conditions and collecting the fully oxidized and burned gases, which include carbon dioxide and water.

[0004] The utility model patent "Oxidation Combustion Device for Preparing Organic Tritium Carbon Samples" announced on May 26, 2023 announced an oxidation combustion device for preparing organic tritium carbon samples, including an oxidation combustion furnace, a heating device and an absorption device. The internal space of the oxidation combustion furnace is divided into a sample placement area and a catalytic reaction area. The sample placement area is divided into a first space and a second space. The sample is placed in the first space. The first space has a vent. Oxygen enters the first space through the air inlet pipe, the secondary combustion air inlet, the second space, and the vent in turn, so that the pyrolysis products of the sample in the first space are burned, and the products after combustion enter the catalytic reaction area. However, the oxygen in the device is not in sufficient contact with the gas after the first combustion of the sample, and the combustion is not yet complete. Summary of the invention

[0005] In order to solve the problems existing in the above-mentioned prior art, the object of the present invention is to provide a vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples.

[0006] The present invention discloses a vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples, comprising: a combustion oxidation module, the combustion oxidation module comprising a vertical detachable combustion tube, at least two air inlet pipes, an air inlet portion and a heater; the combustion tube comprises a base and a fixed portion, the base can be separated or combined with the fixed portion by lifting, and the combustion tube is provided with a combustion chamber opened and closed by lifting the base and the fixed portion; the air inlet pipes extend into the combustion chamber from the top and bottom respectively, and are used to respectively introduce combustion-supporting gas into the combustion chamber along the up and down directions, so that the combustion-supporting gas forms a vortex to promote full combustion of the sample; the air inlet portion is arranged at the top of the fixed portion, and is used to draw out the gas formed by the combustion of the sample; the heater is sleeved on the outside of the combustion tube, and is used to make the sample reach the ignition point and burn by heating; an oxidation catalytic module, the oxidation catalytic module is connected to the air inlet portion, and is used to further oxidize and catalyze the first product to form a second product; a three-way catalytic module, the three-way catalytic module is connected to the oxidation catalytic module, and is used to further render the second product harmless through a redox reaction.

[0007] Preferably, the heater includes at least one heating part and an air cooling part, the heating part is sleeved on the outer side of the combustion tube, and is used to make the sample reach the ignition point and burn by heating, the air cooling part includes a shell and an air cooler, the shell is sleeved on the outer side of the combustion tube, is a double-layer shell with a cavity between the double layers, and the air outlet and air inlet of the air cooler are connected to the cavity between the double-layer shells.

[0008] Preferably, a sample placement component is fixedly or detachably provided on the base, and the sample placement component is a sample tube or a crucible.

[0009] Preferably, there are two air intake pipes, one of which extends into the combustion chamber from the top of the fixing portion or extends into the combustion chamber from the side of the fixing portion, and the other air intake pipe extends into the combustion chamber from the base.

[0010] Preferably, the oxidation catalytic module includes a foam copper mesh whose surface component is copper oxide, and a first quartz filter. The foam copper mesh is located in the channel where the first product flows from the air inlet portion to the three-way catalytic module, and is used to allow the first product to be catalytically oxidized by copper oxide to form the second product when passing through the heated foam copper mesh. The first quartz filter is located between the foam copper mesh and the combustion chamber, and is used to prevent the foam copper mesh and copper oxide from falling into the combustion chamber.

[0011] Preferably, the heater further comprises another heating part, which is sleeved on the outer side of the air ducting part and is used to form copper oxide on the surface of the foam copper mesh by heating; the temperature of each heating part is independently controlled.

[0012] Preferably, the three-way catalytic module includes a platinum-rhodium-palladium three-way catalyst, a second quartz filter and a quartz catalytic tube, one end of the quartz catalytic tube is connected to the air induction portion, the platinum-rhodium-palladium three-way catalyst is located in the quartz catalytic tube, and the second quartz filter is located at one end of the platinum-rhodium-palladium three-way catalyst close to the air induction portion, for preventing the platinum-rhodium-palladium three-way catalyst from moving along the quartz catalytic tube toward the air induction portion.

[0013] The present invention also provides a method for using the vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples as described in any of the above-mentioned technical solutions, characterized in that it includes the following steps: Step 1, lowering the base, placing the sample, and then raising the base so that it is combined with the fixed part into one; Step 2, making the oxidation catalytic module have oxidation catalytic ability, making the three-way catalytic module have oxidation-reduction ability, and introducing the combustion-supporting gas from the top and bottom of the combustion tube through the air inlet pipe and heating the sample to the ignition point through the heater or the heating part for heating the sample; Step 3, continuously heating or maintaining a constant temperature, oxidizing, catalyzing, and reducing until the gas formed by the combustion of the sample is harmlessly rendered.

[0014] Preferably, in step one, the sample is placed in a sample placement component and fixed to the base, or the sample is placed on the sample placement component fixed to the base; in step two, the heating temperature of the heater or the heating part for heating the sample is 400°C-1200°C, the oxidation catalytic module includes a foam copper mesh whose surface material is copper oxide, and the method for making the foam copper mesh have oxidation catalytic activity is to heat the foam copper mesh and maintain the heating temperature at 400°C-1200°C; the three-way catalytic module is a platinum-rhodium-palladium three-way catalytic converter, and the method for making the three-way catalytic module have redox activity is to heat the platinum-rhodium-palladium three-way catalytic converter 310 and maintain the heating temperature at 400°C-800°C.

[0015] The present invention also provides an oxidation combustion collection system for sediment or biological radioactive organic carbon tritium samples, comprising a vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples as described in any of the above technical solutions.

[0016] The vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium sample described in the present invention has the advantages that, taking oxygen as the combustion-supporting gas, the sample on the base is heated by oxygen, and after reaching the ignition temperature, it burns rapidly, and the oxidation produces gas (mainly including carbon monoxide (CO, containing 14 CO), hydrocarbons (CH n , incompletely burned hydrocarbons (CH n , including 14 C Hydrogen Compounds 14 CH n , Carbon tritium compound CT n , 14 C tritium compounds 14 CT n , where the subscript n represents the number of atoms, the same below), carbon dioxide (CO2, containing 14 CO2), water or tritium water (HTO, DTO or T2O)) and particulate matter (mainly incompletely burned hydrocarbons C n H m O k , including 14 C n H m O k , C n T m O k and 14 C n T n O ketc. particles; wherein the subscripts n, m and k represent the atomic number, the same below); in the middle of the above-mentioned combustion tube: the gas and particles rise with the airflow, continue to burn under the action of oxygen, release a large amount of heat to accelerate combustion; in the upper part of the above-mentioned combustion tube, a pure oxygen airflow flowing downward is added through the air intake pipe to intersect with the rising airflow, which can effectively supplement oxygen to accelerate combustion; at the same time, the pure oxygen airflow flowing downward intersects with the rising airflow, which will inevitably form a vortex microenvironment in the upper and middle areas of the above-mentioned combustion tube, and some unburned particles will also boil and burn like the ups and downs of the airflow, which is more conducive to the complete combustion of the sample. In addition to oxygen, in systems where other combustion-supporting gases exist, such as hydrogen, alkanes are the combustion-supporting gas or one of the combustion-supporting gases, the above-mentioned vortex environment can also be formed by the scheme of the present invention to promote the combustion of the corresponding system sample. The present invention is based on a three-stage cascade modular oxidation catalytic design, which effectively overcomes the shortcomings of incomplete dual-zone combustion, tritium water and 14 The conversion efficiency of C carbon dioxide is higher, the vertical double-path oxygen combustion-supporting design based on the boiling combustion principle has high heat utilization efficiency and more complete combustion. In addition, the present invention also provides a method for using the device and a collection system, which is simple, the sample is fully burned, the gas is highly harmless, and the collection is convenient. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 The structure of the vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium sample of the present invention is shown in FIG. Figure 1 ;

[0018] Figure 2 The structure of the vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium sample of the present invention is shown in FIG. Figure 2 .

[0019] Description of reference numerals:

[0020] 110 combustion tube 111 base 112 fixing part

[0021] 113 combustion chamber 120 intake pipe 120 air intake part

[0022] 140 heater 140 heater 141 heating unit

[0023] 150 Sample placement component 210 Foam copper mesh 220 First quartz filter

[0024] 310 Platinum-rhodium-palladium three-way catalytic converter 320 Second quartz filter 330 Quartz catalytic tube DETAILED DESCRIPTION

[0025] like Figure 1 to Figure 2As shown, the vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples described in the present invention comprises: a combustion oxidation module, the combustion oxidation module comprises a vertical detachable combustion tube 110, at least two air inlet pipes 120, an air induction part 130 and a heater 140; the combustion tube 110 comprises a base 111 and a fixing part 112, the base 111 can be separated or combined with the fixing part 112 by lifting, and the combustion tube 110 is provided with a combustion chamber 113 which is opened and closed by lifting the base 111 and the fixing part 112; the air inlet pipe 120 extends into the combustion chamber 113 from the top and bottom respectively, and is used to respectively move along the upper and lower sides of the combustion chamber 113. A combustion-supporting gas is introduced into the combustion chamber 113 from below, so that the combustion-supporting gas forms a vortex to promote complete combustion of the sample; the air introduction portion 130 is arranged at the top of the fixing portion 112, and is used to introduce the gas formed by the combustion of the sample; the heater 140 is sleeved on the outside of the combustion tube 110, and is used to make the sample reach the ignition point and burn by heating; an oxidation catalytic module, the oxidation catalytic module is connected to the air introduction portion 130, and is used to further oxidize and catalyze the first product to form a second product; a three-way catalytic module, the three-way catalytic module is connected to the oxidation catalytic module, and is used to further render the second product harmless through a redox reaction.

[0026] In a specific implementation, the air inlet pipe 120 can be set to 2-4 pieces. For example, 1-2 pieces can be set at the upper part of the fixed part 112, all of which are introduced from the outside of the fixed part 112 through the shell of the fixed part 112 to the top of the combustion chamber 113 and make the combustion-supporting gas flow downward (that is, the fixed part 112 points to the direction of the base 111); 1-2 pieces can be set on the base 111, all of which are passed through the base 111 from the outside of the base 111 to enter the bottom of the combustion chamber 113 and make the combustion-supporting gas flow upward (that is, the base 111 points to the direction of the fixed part 112). Specifically, the sample burns under the support of oxygen in the air inlet pipe 120 set on the base 111, and is further fully burned after mixing with the oxygen in the air inlet pipe 120 at the upper part of the fixed part 112 to form the first product. The heater 140 can heat the sample by heat conduction. In order to realize the heating function of the heater 140, the heater 140 and the position where it is installed on the combustion tube 110 can adopt the heating components in the prior art and select the installation position in the prior art. Those skilled in the art can select the heating components and installation positions in the prior art according to actual needs. The first product is catalytically oxidized by the oxidation catalytic module to form the second product, and then further rendered harmless by the three-way catalytic module through oxidation-reduction reaction.

[0027] The combustion-supporting gas is preferably oxygen. Due to the high efficiency and thoroughness of the combustion and post-treatment (oxidation, catalysis, reduction), the sample processing volume is not less than 100g of biological radioactive samples, or 200g of sediment / soil samples each time.

[0028] The vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium sample described in the present invention has the advantages that, taking oxygen as the combustion-supporting gas, the sample on the base is heated by oxygen, and after reaching the ignition temperature, it burns rapidly, and the oxidation produces gas (mainly including carbon monoxide (CO, containing 14 CO), hydrocarbons (CH n , incompletely burned fuel components, including 14 CH n ), carbon tritium compounds (CT n , including 14 CT n )), carbon dioxide (CO2, containing 14 CO2), water or tritium water (HTO, DTO and T2O) and particulate matter (mainly incompletely burned hydrocarbons C n H m O k , including 14 C n H m O k , C n T m O k and 14 C n T n O k and other particles); in the middle of the combustion tube: the gas and particles rise with the airflow, continue to burn under the action of oxygen, release a large amount of heat to accelerate combustion; in the upper part of the combustion tube, a pure oxygen airflow flowing downward is added through the air inlet pipe to intersect with the rising airflow, which can effectively supplement oxygen to accelerate combustion; at the same time, the pure oxygen airflow flowing downward intersects with the rising airflow, which will inevitably form a vortex microenvironment in the upper and middle areas of the combustion tube, and some of the particles that are not fully burned will also boil and burn like the ups and downs of the airflow, which is more conducive to the complete combustion of the sample. In addition to oxygen, in systems where other combustion-supporting gases exist, such as hydrogen, alkanes are the combustion-supporting gas or one of the combustion-supporting gases, the above-mentioned vortex environment can also be formed by the scheme of the present invention to promote the combustion of the corresponding system samples. In addition, the present invention is based on a three-stage cascade modular oxidation catalytic design, which effectively overcomes the shortcomings of incomplete dual-zone combustion, tritium water and 14 The conversion efficiency of CO2-14 is higher, and the vertical dual-path oxygen-assisted combustion design is based on the principle of boiling combustion, with high heat utilization efficiency and more complete combustion.

[0029] Preferably, the heater 140 includes at least one heating part 141 and an air cooling part. The heating part 141 is sleeved on the outer side of the combustion tube 110, and is used to make the sample reach the ignition point and burn by heating. The air cooling part includes a shell and an air cooler. The shell is sleeved on the outer side of the combustion tube 110, is a double-layer shell with a cavity between the double layers, and the air outlet and air inlet of the air cooler are connected to the cavity between the double-layer shells.

[0030] In specific implementation, the heating part 141 is sleeved on the outer side of the combustion tube 110, and its sleeve position needs to achieve this function, that is, the sample reaches the ignition point and burns by heating. Those skilled in the art can select the heater used in the heating part and the sleeve position of the heating part 141 according to the existing technology and actual needs. After the air-cooling part (not shown in the figure) is started, air (such as cold air) returns to the air-cooling part from the air inlet (not shown in the figure) of the air-cooling part through the cavity between the double-layer shells and from the air outlet (not shown in the figure) of the air-cooling part, and is sent to the air inlet of the air-cooling part again after processing (such as cooling). The air-cooling part can adopt the air-cooling system in the prior art, and those skilled in the art can select the air-cooling system in the prior art according to actual needs.

[0031] Preferably, a sample placement component 150 is disposed on the base 111 , and the sample placement component 150 is a sample tube or a crucible.

[0032] In specific implementation, the sample placement component 150 can be directly fixed on the base 111, or a sample placement seat (not shown in the figure) can be provided on the base 111, and the sample placement component 150 can be fixed on the sample placement seat. The sample placement component 150 can be a sample tube or a crucible, and the sample tube or crucible can be a sample tube or a crucible in the prior art. Those skilled in the art can use a sample tube or a crucible in the prior art according to actual needs.

[0033] Preferably, there are two air intake pipes 120 , one of which extends into the combustion chamber 113 from the top of the fixing portion 112 or extends into the combustion chamber 113 from the side of the fixing portion 112 , and the other air intake pipe 120 extends into the combustion chamber 113 from the base 111 .

[0034] In a specific implementation, when one of the air intake pipes 120 extends from the top of the fixed portion 112 into the combustion chamber 113, and the other air intake pipe 120 extends from the base 111 into the combustion chamber 113, the sample burns to form gas and particulate matter under the action of the combustion-supporting gas (oxygen) in the air intake pipe 120 and the heater (heating the sample to the ignition point to cause the sample to burn), and the gas and the particulate matter rise to the middle of the combustion chamber for further combustion, and the gas and a small amount of particulate matter after further combustion form a vortex in the upper part of the combustion chamber with the combustion-supporting gas (oxygen) flowing from the top of the fixed portion 112 in the air intake pipe 120 toward the base 111, and are fully burned. When the air intake pipe 120 extends from the side of the fixed portion 112 into the combustion chamber 113, the principle is the same as above. When the intake pipe 120 extends into the combustion chamber 113 from the top of the fixed part 112, it can be extended into from the upper opening of the fixed part 112 and fixed by a sealing component such as a plug, a cover or a plug. The sealing component is provided with a through hole (not shown in the figure) that can accommodate the intake pipe 120 and the air induction part 130. The matching relationship and position relationship of the sealing component, the intake pipe 120 and the air induction part 130 at the upper opening of the fixed part 112 adopt the position relationship and matching relationship in the prior art. Those skilled in the art can select the position relationship and matching relationship in the prior art according to actual needs. For example, the air induction part 130 cooperates with a cover-like component through a through hole, and the cover-like component covers the upper opening of the fixed part 112 in a tight fit; the air induction part 130 and the intake pipe 120 cooperate with another cover-like component through two through holes, and the cover-like component covers the upper opening of the fixed part 112 and is located outside the previous cover-like component. When the air intake pipe 120 extends from the side of the fixing portion 112 into the combustion chamber 113 , a through hole needs to be opened on the double-layer shell.

[0035] Preferably, the oxidation catalytic module includes a foam copper mesh 210 whose surface component is copper oxide, and a first quartz filter 220. The foam copper mesh 210 is located in the channel through which the first product flows from the air inlet portion 130 to the three-way catalytic module, and is used to allow the first product to be catalytically oxidized by copper oxide to form the second product when passing through the heated foam copper mesh 210. The first quartz filter 220 is located between the foam copper mesh 210 and the combustion chamber 113, and is used to prevent the foam copper mesh 210 and copper oxide from falling into the combustion chamber 113. The first product flows from the air inlet portion 130 through the first quartz filter 220 to the foam copper mesh 210, and after forming the second product through the foam copper mesh 210, it flows to the three-way catalytic module.

[0036] In a specific implementation, the foam copper mesh 210 is oxidized at high temperature before the reaction to generate CuO on the surface. When the sample reacts, copper oxide plays the dual role of oxidant and catalyst, so that the sample burns to form a further combustible gas (carbon monoxide (CO, containing 14 CO), hydrocarbons (CH n , incompletely burned fuel components, including 14 CH n , CT n , 14 CT n ) accelerates combustion and generates carbon dioxide (CO2, containing 14 CO2), water (H2O, including HTO, T2O), its combustion rate reaches 90%. At the same time, at high temperature, copper oxide can also catalyze carbon monoxide (CO,, including 14 CO) is oxidized to carbon dioxide or carbon-14 carbon dioxide (CO2, containing 14 CO2), catalytic hydrocarbons (CH n , including 14 CH n , CT n , 14 CT n ) reacts with O2 to produce carbon dioxide (CO2, containing 14 CO2), (H2O, including HTO and T2O), or carbon monoxide (CO, including 14 CO) is oxidized by CuO to produce carbon dioxide (CO2, containing 14 CO2), at which point CuO is reduced to Cu. After further catalytic oxidation of CuO, the combustion rate of the sample can reach 90%, reducing the working pressure of the three-way catalytic module.

[0037] Preferably, the heater 140 further comprises another heating portion 141, which is sleeved on the outer side of the air ducting portion 130 and is used to form copper oxide on the surface of the foam copper mesh 210 by heating; the temperature of each heating portion 141 is independently controlled.

[0038] In specific implementation, the heating part 141 is sleeved on the outer side of the air inlet part 130, and its sleeve position needs to achieve this function, even if the foam copper mesh generates copper oxide at high temperature, those skilled in the art can select the heater used in the heating part and the sleeve position of the heating part 141 according to existing technology and actual needs. The temperature of each heating part 141 is independently controlled by a separate control unit, which is conducive to the selection of different sample reaction conditions.

[0039] Preferably, the three-way catalytic module includes a platinum-rhodium-palladium three-way catalyst 310, a second quartz filter 320 and a quartz catalytic tube 330, one end of the quartz catalytic tube 330 is connected to the air inlet portion 130, the platinum-rhodium-palladium three-way catalyst 310 is located in the quartz catalytic tube 330, and the second quartz filter 320 is located at one end of the platinum-rhodium-palladium three-way catalyst 310 close to the air inlet portion 130, and is used to prevent the platinum-rhodium-palladium three-way catalyst 310 from moving along the quartz catalytic tube 330 toward the air inlet portion 130.

[0040] In specific implementation, the platinum-rhodium-palladium three-way catalyst 42 provides a surface with a platinum-rhodium-palladium three-way catalyst, and the carrier for the platinum-rhodium-palladium three-way catalyst is a porous ceramic. The platinum-rhodium-palladium three-way catalyst allows the oxidation-reduction reaction of the gas oxidized and catalyzed by the oxidation catalytic module to be carried out efficiently at a relatively low temperature. In the oxidation-reduction reaction process, carbon monoxide (CO, containing 14 CO), hydrocarbons (CH n , incompletely burned fuel components, including 14 CH n ), carbon tritium compounds (CT n , including 14 CT n ) and nitrogen oxides (NO n These harmful gases are converted into relatively harmless carbon dioxide (CO2, containing 14 CO2), water (H2O, including tritium water HTO and T2O) and nitrogen (N2). 14 CO), hydrocarbons (CH n , including 14 CH n , CT n , 14 CT n ) is oxidized to generate carbon dioxide (CO, containing 14 CO), water (H2O, including HTO and T2O), nitrogen oxides (NO n ) is reduced to nitrogen (N2) under the action of the catalyst. This is a reduction process. Through this redox process, the oxidized catalytic gas is rendered harmless, easy to collect and avoids environmental pollution caused by gas leakage. And nitrogen oxides (NO n ) is converted into nitrogen (N2), which effectively reduces the acidity of water (tritium water) and the quenching effect and color effect of subsequent liquid scintillation, and improves the measurement efficiency of tritium carbon.

[0041] The present invention also provides a method for using the vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples described in any of the above technical solutions, comprising the following steps: step one, lowering the base 111, placing the sample, and then raising the base 111 so that it is combined with the fixing part 112 into one; step two, making the oxidation catalytic module have oxidation catalytic activity, making the three-way catalytic module have redox activity, and introducing the combustion-supporting gas from the top and bottom of the combustion tube 113 through the air inlet pipe 120 and heating the sample to the ignition point through the heater 140 or the heating part 141 for heating the sample; step three, continuously heating or maintaining a constant temperature, oxidizing, catalyzing, and reducing until the gas formed by the combustion of the sample is rendered harmless.

[0042] The above method is simple to operate. The sample is burned thoroughly during the first combustion process due to the presence of vortex gas. Through the design of multi-step catalysis, oxidation, reduction and combustion, the gas formed by the combustion of the sample is completely rendered harmless. The rendered gas is environmentally friendly and easy to collect.

[0043] Preferably, in the method of use, in step one, the sample is placed in the sample placement component 150 and fixed to the base 111, or the sample is placed on the sample placement component 150 fixed to the base 111; in step two, the heating temperature of the heating part 141 of the heater 140 used to heat the sample is 400°C-1200°C, the oxidation catalytic module includes a foam copper mesh 210 whose surface material is copper oxide, and the method for making the foam copper mesh 210 have oxidation catalytic activity is to heat the foam copper mesh 210 and maintain the heating temperature at 400°C-1200°C; the three-way catalytic module includes a platinum-rhodium-palladium three-way catalytic converter 310, and the method for making the three-way catalytic module have redox activity is to heat the platinum-rhodium-palladium three-way catalytic converter 310 and maintain the heating temperature at 400°C-800°C.

[0044] In a specific implementation, the sample placement component 150 can be set to be fixed on the base 111 or detachably set on the base 111. The sample placement component 150 can adopt the sample placement component and setting method in the prior art. Those skilled in the art can select the placement component and setting method in the prior art according to actual needs.

[0045] Embodiment 1 of the present invention, as Figure 1As shown, the vertical oxidation combustion device used includes: a combustion oxidation module, which includes a vertical detachable combustion tube 110, two air inlet pipes 120, an air entrainment part 130 and a heater 140; the combustion tube 110 includes a base 111 and a fixing part 112, and the base 111 can be separated or combined with the fixing part 112 by lifting, and the combustion tube 110 is provided with a combustion chamber 113 which is opened and closed by lifting the base 111 and the fixing part 112; the air inlet pipe 120 extends into the combustion chamber 113 from the top and bottom respectively, and is used to introduce combustion-supporting gas into the combustion chamber 113 along the up and down directions respectively. , so that the combustion-supporting gas forms a vortex to promote the complete combustion of the sample to form a first product; the air inlet portion 130 is arranged on the top of the fixing portion 112, and is used to lead out the first product; the heater 140 is sleeved on the outside of the combustion tube 110, and is used to make the sample reach the ignition point and burn by heating; an oxidation catalytic module, the oxidation catalytic module is connected to the air inlet portion 130, and is used to further oxidize and catalyze the first product to form a second product; a three-way catalytic module, the three-way catalytic module is connected to the oxidation catalytic module, and is used to make the second product further harmless through an oxidation-reduction reaction and become the product to be separated;

[0046] Of the two air intake pipes 120 , one air intake pipe 120 extends from the side of the fixing portion 112 into the combustion chamber 113 , and the other air intake pipe 120 extends from the base 111 into the combustion chamber 113 ;

[0047] The heater 140 includes two heating parts 141 and an air cooling part 142, wherein the heating part 141 is sleeved on the outer side of the combustion tube 110, and is used to make the sample reach the ignition point and burn by heating, and the air cooling part 142 includes a shell and an air cooler, the shell is sleeved on the outer side of the combustion tube 110, is a double-layer shell with a cavity between the double layers, and the air outlet and air inlet of the air cooler are connected to the cavity between the double-layer shells;

[0048] The oxidation catalytic module comprises a foam copper mesh 210 whose surface component is copper oxide and a first quartz filter 220, wherein the foam copper mesh 210 is located in the passage of the first product flowing from the air induction portion 130 to the three-way catalytic module, and is used to make the first product catalytically oxidized by copper oxide to form the second product when passing through the heated foam copper mesh 210, and the first quartz filter 220 is located between the foam copper mesh 210 and the combustion chamber 113, and is used to prevent the foam copper mesh 210 and copper oxide from falling into the combustion chamber 113;

[0049] The heater 140 further includes another heating portion 141 , which is sleeved on the outer side of the air ducting portion 130 and is used to form copper oxide on the surface of the foam copper mesh 210 by heating; the temperature of each heating portion 141 is independently controlled.

[0050] The three-way catalytic module includes a platinum-rhodium-palladium three-way catalyst 310, a second quartz filter 320 and a quartz catalytic tube 330, one end of the quartz catalytic tube 330 is connected to the air inlet portion 130, the platinum-rhodium-palladium three-way catalyst 310 is located in the quartz catalytic tube 330, and the second quartz filter 320 is located at one end of the platinum-rhodium-palladium three-way catalyst 310 close to the air inlet portion 130, and is used to prevent the platinum-rhodium-palladium three-way catalyst 310 from moving along the quartz catalytic tube 330 toward the air inlet portion 130.

[0051] In specific implementation, the generation process of the product to be separated is as follows: lower the base 111, put the sample in, and then raise the base 111 to combine it with the fixing part 112; control the heating temperature of the other heating part 141 from room temperature to 800°C, with a heating rate of 10°C / min, and continuously heat the foam copper mesh 210 at a constant temperature, and use a heating device (not shown in the figure) to heat the platinum-rhodium-palladium three-way catalytic converter 310, the heating temperature is from room temperature to 600°C, and the heating rate is 10°C / min. When the foam copper mesh 210 and the platinum-rhodium-palladium three-way catalytic converter 310 reach 800°C and 600°C, the combustion-supporting gas is introduced from the top and bottom of the combustion tube 110 through the intake pipe 120, and the heating temperature of the heating part 141 is controlled from room temperature to 800°C, with a heating rate of 10°C / min, and then the sample is heated to the ignition point at a constant temperature, and the heating or constant temperature, oxidation, catalysis, and reduction are continued until the gas formed by the combustion of the sample is rendered harmless.

[0052] More specifically, of the two air inlet pipes 120, the oxygen flow rate of the air inlet pipe 120 extending from the base 111 into the combustion chamber 113 is 0.12L / min-0.5L / min, and the oxygen flow rate of the air inlet pipe 120 extending from the side of the fixing portion 112 into the combustion chamber 113 is 0.12L / min-0.5L / min. The oxygen flow rates in the two air inlet pipes 120 are independently controlled by two flow meters. (The flow rates of nitrogen and oxygen required for the specific experiment are adjusted according to the organic matter and oil content in the sample)

[0053] like Figure 2As shown, embodiment 2 of the present invention is different from embodiment 1 in that, of the two intake pipes 120, one intake pipe 120 extends from the top of the fixing portion 112 into the combustion chamber 113, and the other intake pipe 120 extends from the base 111 into the combustion chamber 113; the rest is the same as embodiment 1.

[0054] The present invention also provides an oxidation combustion collection system for sediment or biological radioactive organic carbon tritium samples, including the vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples described in any of the above technical solutions.

[0055] In the description of the present invention, it is necessary to understand that the directions or positional relationships indicated by directional words such as "front, back, up, down, left, right", "lateral, vertical, horizontal" and "top, bottom" are usually based on the directions or positional relationships shown in the drawings. They are only for the convenience of describing the present invention and simplifying the description. Unless otherwise specified, these directional words do not indicate or imply that the device or element referred to must have a specific direction or be constructed and operated in a specific direction. Therefore, they cannot be understood as limiting the scope of protection of the present invention.

[0056] For those skilled in the art, various other corresponding changes and deformations can be made according to the technical solutions and concepts described above, and all of these changes and deformations should fall within the protection scope of the claims of the present invention.

Claims

1. A vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples, characterized in that: include: A combustion oxidation module, the combustion oxidation module comprising a vertical detachable combustion tube (110), at least two air inlet pipes (120), an air induction part (130) and a heater (140); the combustion tube (110) comprises a base (111) and a fixing part (112); the base (111) can be separated from or combined with the fixing part (112) by lifting; the combustion tube (110) is provided with a combustion chamber (1111) which is opened and closed by lifting the base (111) and the fixing part (112). 3); the air inlet pipe (120) extends into the combustion chamber (113) from the top and bottom respectively, and is used to introduce the combustion-supporting gas into the combustion chamber (113) in the top and bottom directions respectively, so that the combustion-supporting gas forms a vortex to promote the full combustion of the sample to form a first product; the air introduction part (130) is arranged on the top of the fixing part (112) and is used to introduce the first product; the heater (140) is sleeved on the outside of the combustion tube (110) and is used to make the sample reach the ignition point and burn by heating; An oxidation catalytic module, the oxidation catalytic module being connected to the air induction portion (130) and used for further oxidizing and catalyzing the first product to form a second product; A three-way catalytic module is connected to the oxidation catalytic module and is used to further render the second product harmless through a redox reaction.

2. The vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples according to claim 1, characterized in that: The heater (140) includes at least one heating part (141) and an air cooling part. The heating part (141) is sleeved on the outer side of the combustion tube (110) and is used to make the sample reach the ignition point and burn by heating. The air cooling part includes a shell and an air cooler. The shell is sleeved on the outer side of the combustion tube (110) and is a double-layer shell with a cavity between the double layers. The air outlet and air inlet of the air cooler are connected to the cavity between the double-layer shells.

3. The vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples according to claim 1, characterized in that: A sample placement component (150) is fixedly or detachably arranged on the base (111), and the sample placement component (150) is a sample tube or a crucible.

4. The vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples according to claim 1, characterized in that: There are two air intake pipes (120), one of which extends from the top of the fixing portion (112) into the combustion chamber (113) or from the side of the fixing portion (112) into the combustion chamber (113), and the other air intake pipe (120) extends from the base (111) into the combustion chamber (113).

5. The vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples according to claim 2, characterized in that: The oxidation catalytic module comprises a foam copper mesh (210) whose surface component is copper oxide, and a first quartz filter (220); the foam copper mesh (210) is located in a channel through which the first product flows from the air induction portion (130) to the three-way catalytic module (300), and is used to allow the first product to be catalytically oxidized by copper oxide to form the second product when passing through the heated foam copper mesh (210); and the first quartz filter (220) is located between the foam copper mesh (210) and the combustion chamber (113), and is used to prevent the foam copper mesh (210) and the copper oxide from falling into the combustion chamber (113).

6. The vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium sample according to claim 5, characterized in that: The heater (140) further comprises another heating portion (141), which is sleeved on the outer side of the air ducting portion (130) and is used to form copper oxide on the surface of the foam copper mesh (210) by heating; the temperature of each heating portion (141) is independently controlled.

7. The vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples according to claim 1, characterized in that: The three-way catalytic module comprises a platinum-rhodium-palladium three-way catalytic converter (310), a second quartz filter (320) and a quartz catalytic tube (330); one end of the quartz catalytic tube (330) is connected to the air induction portion (130); the platinum-rhodium-palladium three-way catalytic converter (310) is located in the quartz catalytic tube (330); the second quartz filter (320) is located at one end of the platinum-rhodium-palladium three-way catalytic converter (310) close to the air induction portion (130) and is used to prevent the platinum-rhodium-palladium three-way catalytic converter (310) from moving along the quartz catalytic tube (330) toward the air induction portion (130).

8. A method for using the vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium sample according to any one of claims 1 to 7, characterized in that: The steps include: Step 1, lowering the base (111), placing the sample, and then raising the base (111) to combine it with the fixing part (112) into one body; Step 2: enabling the oxidation catalytic module to have oxidation catalytic capability, enabling the three-way catalytic module to have oxidation-reduction capability, and introducing the combustion-supporting gas from the upper and lower sides of the combustion tube (113) through the air intake pipe (120) and heating the sample to the ignition point through the heater (140) or the heating part (141) for heating the sample; Step 3: Continue heating or maintaining a constant temperature, oxidizing, catalyzing, and reducing until the gas generated by the combustion of the sample is rendered harmless.

9. The method for using the vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples according to claim 8, characterized in that: In step 1, the sample is placed in a sample placement component (150) and fixed to the base (111), or the sample is placed on the sample placement component (150) fixed to the base (111); In step 2, the heating temperature of the heating part (141) of the heater for heating the sample is 400°C-1200°C, the oxidation catalytic module includes a foam copper mesh (210) whose surface material is copper oxide, and the method for making the foam copper mesh (210) have oxidation catalytic activity is to heat the foam copper mesh (210) and maintain the heating temperature at 400°C-1200°C; the three-way catalytic module includes a platinum-rhodium-palladium three-way catalytic converter (310), and the method for making the three-way catalytic module have redox activity is to heat the platinum-rhodium-palladium three-way catalytic converter (310) and maintain the heating temperature at 400°C-800°C.

10. An oxidation combustion collection system for sediment or biological radioactive organic carbon tritium samples, characterized in that: A vertical oxidation combustion device for sediment or biological radioactive organic carbon tritium samples as described in any one of claims 1 to 7.

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