JP2012194001A - Evaluation apparatus for adsorptivity and/or reactivity of gas - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an evaluation apparatus for adsorptivity and/or reactivity of gas, in which the adsorptivity and/or reactivity of gas in an evaluation target can be evaluated even when a high-concentration gas is used.SOLUTION: An evaluation apparatus comprises a reaction unit 1 within which an evaluation target is provided, a heating unit 2 which heats the evaluation target, a gas supply channel 3 which allows gas to flow into the reaction unit 1, a gas discharge channel 4 which allows the gas to flow out of the reaction unit 1, a flow rate adjusting unit 5 which is provided inside the gas supply channel 3, and a detection unit 7 which is provided in the gas discharge channel 4. An analysis unit 8 which analyzes adsorptivity and/or reactivity of the gas in the evaluation target is connected to the detection unit 7 and the reaction unit 1, an inert gas injection unit 9 which injects an inert gas into the gas discharge channel 4 is provided in the gas discharge channel 4, and the detection unit 7 detects a component contained in a mixed gas of the gas flowing out of the reaction unit 1 and the inert gas.

Description

  The present invention relates to an apparatus for evaluating gas adsorption and / or reactivity.

  Conventionally, a temperature-programmed desorption (TPD) method has been known as a method for evaluating gas adsorption and reactivity on the surface of a catalyst material or the like. A conventional apparatus for evaluating gas adsorption and reactivity has a structure as shown in FIG.

In order to operate the conventional gas absorptive and reactive evaluation apparatus 110 shown in FIG. 2, first, a gas supplied from a gas cylinder (gas storage unit) 106 via a gas supply channel 103 (for example, He, N ₂ , O ₂ , H _2, etc.) are adjusted to an appropriate flow rate by using a mass flow controller (MFC, flow rate adjustment unit) 105, and in some cases, a plurality of gases are mixed and the sample unit (reaction unit) 101 Distribute and pre-process. At this time, if necessary, a sample such as a catalyst material is heated using a heater (heating unit) 102 surrounding the sample unit 101. The gas that has passed through the sample unit 101 is discharged out of the system from the exhaust port via the gas discharge channel 104 (usually not supplied to the detection unit 107).

After the pretreatment, at a desired temperature, the probe gas is circulated through the gas supply channel 103 using the MFC 105 and is adsorbed on the catalyst sample by the sample unit 101. Here, the probe gas refers to a gas containing a gas component for which interaction (adsorbability, reactivity, etc.) with a catalyst sample is to be evaluated. After adsorption of the probe gas to the catalyst sample, the sample unit 101 is heated by the heater 102 while a carrier gas such as He or N ₂ is circulated through the gas supply channel 103 using the MFC 105. At this time, the carrier gas that has passed through the sample portion 101 flows out to the exhaust port via the gas discharge channel 104 along with the gas component desorbed from the catalyst sample. A part of the gas is introduced into the detection unit 107 (mass spectrometer) by a splitter, so that the reaction desorption gas accompanying the temperature rise is continuously analyzed. By installing the data acquisition unit (analysis unit) 108, the gas analysis data and the heater output are acquired on the same time axis, and the TPD curves as shown in FIG. 3 can be acquired by correlating each later. .

FIG. 3 shows the TPD curve of NH ₃ , where A is no steam treatment, B is one steam treatment, C is two steam treatments, and D is three steam treatments. ing. In FIG. 3, NH ₃ -TPD is evaluating surface acid properties. At low temperature, NH ₃ on the weak acid is replaced by water and disappears by steam treatment. On the other hand, at high temperature, it is not affected by the steam treatment. This indicates that the low temperature desorption component of the NH ₃ -TPD curve in the measurement without steam treatment corresponds to a weak acid or a physical adsorption species, and the high temperature desorption component corresponds to a chemisorption species.

  As an application of the TPD method, the probe gas is heated while being continuously circulated, and the probe gas and the reaction product gas on the catalyst sample are measured to evaluate the gas adsorption and reaction on the surface of the object. A temperature-programmed reaction (TPR) method is also known.

In addition to the mass spectrometer, the detection unit includes an inexpensive thermal conductivity detector, various gas analyzers (NDIR, FT-IR, chemiluminescence NOx meter, apparatus using a sO ₂ meter, etc.), or device combining them further observed catalytic surface adsorbed species at the desorption temperature at the same time as the TPD curve by connecting the spectral analyzer, such as FT-IR to the sample unit Various arrangement TPD devices are known, such as devices capable of doing so.

For example, Non-Patent Document 1 describes evaluation of gas adsorption, reactivity, etc., which are constituted by a gas supply flow path, a flow rate adjustment unit, a reaction unit, and a detection unit (thermal conductivity detector / TCD). The device (initial type) is shown. Further, Non-Patent Document 2 discloses an evaluation apparatus (spreading type, commercially available) for gas adsorption, reactivity, etc., which includes a gas supply channel, a gas flow rate adjustment unit, a reaction unit, and a detection unit (mass spectrometer). Product). Further, Non-Patent Document 3, an example using a variety of gas analyzer (chemiluminescence type NOx meter or SO ₂ meter UV fluorescence method, etc.) in the detection portion is shown.

R. J. Cvetanovic and Y. Amenomiya, Application of a Temperature-Programmed Desorption Technique to Catalyst Studies, Adv. Catal., 17, p.103-149, (1967) Miwa Niwa and Naobu Katada, “Solid Acid Properties of Zeolite and Metal Oxide Thin Layer by Ammonia Thermal Desorption”, Surface Science, Vol.24, No.10, p.635-641, (2003) Evangelos A. Efthimiadis et.al., Selective catalytic reduction of NO with C3H6over Rh / alumina in the presence and absence of SO2 in the feed, Appl. Catal., B 22, p.91-106, (1999)

  However, in the evaluation devices such as gas adsorbability and reactivity shown in Non-Patent Documents 1 and 2, since the detection concentration range depends on the detection unit, a wide range of concentrations, particularly high concentrations exceeding the detection upper limit. It is difficult to use for a test in which gas is continuously circulated. Further, when the gas adsorbed on the catalyst sample is detected while circulating a carrier gas such as He, when a high concentration gas exceeding the detection upper limit is generated, the component of the gas cannot be detected, There is a problem that it is not possible to evaluate gas adsorption and reactivity in the catalyst sample. In addition, the method disclosed in Non-Patent Document 3 is not intended to evaluate gas adsorbability, reactivity, and the like.

  The present invention has been made in view of the above-described conventional problems, and the object thereof is to achieve gas adsorption and / or reaction in an evaluation object even when a high-concentration gas exceeding the detection upper limit of the detector is used. It is an object of the present invention to provide a gas adsorption and / or reactivity evaluation apparatus capable of evaluating the properties.

  In view of the above-mentioned problems, the present inventors evaluated the gas adsorption property, reactivity, etc. in the evaluation object in the evaluation device for gas adsorption property, reactivity, etc. shown in Non-Patent Documents 1 and 2. The method to do was examined. The evaluation devices for gas adsorption and reactivity shown in Non-Patent Documents 1 and 2 have a configuration in which the gas exiting the reaction part is directly introduced into the detection part. For this reason, in order to reduce the amount of gas adsorbed to and desorbed from the evaluation object in the reaction unit in advance so that the gas has a concentration equal to or lower than the detection upper limit of the detection unit. It is necessary to reduce the weight of the evaluation object.

  If the present inventors can introduce the gas into the detection part after diluting the gas exiting the reaction part and reducing the concentration, the case where a high concentration gas exceeding the detection upper limit of the detection part is used or adsorbed It has been found that even when components are desorbed at a time and a high-concentration gas exceeding the detection upper limit of the detection unit is generated, the adsorptivity and reactivity of the gas in the evaluation object can be evaluated. Then, the inventors have uniquely found that the gas can be diluted by mixing an inert gas with the gas exiting the reaction section, and have completed the present invention. According to the present invention, the gas can be detected using a gas having a concentration range that exceeds the detection upper limit of the detection unit, and the concentration that exceeds the detection upper limit of the detection unit from the evaluation object on which the gas is adsorbed. Even when the gas in the region is desorbed, the desorbed gas can be detected without adjusting the amount of the object to be evaluated. As a result, the present invention can evaluate the adsorptivity, reactivity, etc. of the gas in the evaluation object even when a high concentration gas is used.

  That is, the gas adsorption and / or reactivity evaluation apparatus according to the present invention includes a reaction unit in which an evaluation target is provided and a heating unit that heats the evaluation target in order to solve the above-described problems. A gas supply channel for allowing gas to flow into the reaction unit, a gas discharge channel for allowing gas to flow out from the reaction unit, a flow rate adjusting unit provided inside the gas supply channel, and the gas discharge channel A detection unit provided in the path, and an analysis unit for analyzing the adsorptivity and / or reactivity of the gas in the evaluation object is connected to the detection unit and the reaction unit, and the gas discharge An inert gas injection section for injecting an inert gas into the flow path is provided in the gas discharge flow path, and the detection section is configured to mix a gas that has flowed out of the reaction section with the inert gas. It is characterized by detecting contained components That.

  According to said structure, since the inert gas injection | pouring part which injects an inert gas into the said gas exhaust flow path is provided in the said gas exhaust flow path, an inert gas is mixed with the gas which flows out from a reaction part. can do. Thereby, the inert gas injection part can dilute the gas flowing out from the reaction part, and can reduce the concentration of the gas.

  Moreover, according to said structure, since the said detection part detects the component contained in the mixed gas of the gas which flowed out from the said reaction part, and the said inert gas, the gas after reducing a density | concentration Can be detected. Thereby, the said detection part can detect gas in the density | concentration range which does not exceed a detection upper limit.

  As a result, the gas adsorptivity and / or reactivity evaluation apparatus of the present invention can evaluate the gas adsorptivity and / or reactivity in the evaluation object even when a high-concentration gas is used.

  Here, Japanese Patent Application Laid-Open No. 2010-243180 discloses a gas analysis method in which a gas dilution device is incorporated into a gas analysis device such as a fuel cell or an exhaust gas treatment system to dilute the gas. In this gas analysis method, an inert gas is supplied only by incorporating a gas dilution device upstream from the flow rate adjustment unit of the supply gas, and the concentration of the gas immediately before flowing into the analyzer (detection meter) is reduced. Therefore, the gas concentration range that can be analyzed (detected) by the analyzer (detector) cannot be widened. In addition, this gas analysis method suppresses the condensation of moisture inside the mass flow controller for flow rate adjustment and suppresses the response delay of the analyzer due to the structure of the mass flow controller when performing the gas composition analysis. The temperature programmed desorption method is not used.

  Japanese Patent Application Laid-Open No. 2010-13989 discloses a gas evaluation apparatus that dilutes exhaust gas by incorporating a dilution gas channel into an evaluation apparatus for an exhaust gas aftertreatment device. This gas evaluation apparatus only incorporates a dilution gas flow path upstream of the detection gas flow rate adjustment unit and supplies an inert gas, and does not reduce the concentration of the gas immediately before flowing into the detector. Therefore, the gas concentration range that can be detected by the detector cannot be widened. Further, this gas evaluation apparatus is for detecting the components of the exhaust gas when evaluating the performance of the exhaust gas, and does not use the temperature programmed desorption method.

  The techniques described in the above two patent publications (Japanese Patent Laid-Open Nos. 2010-243180 and 2010-13989) provide an accurate and responsive response to component analysis of gas discharged from a drive system such as an internal combustion engine or a fuel cell. In order to perform well, the inert gas dilution part is provided in the gas analysis system, and it does not aim at evaluating the adsorptivity and reactivity between a specific object and gas.

  Thus, conventionally, no technique has been found to widen the detectable gas concentration range by lowering the concentration of the detection gas using the temperature programmed desorption method.

  In contrast, the gas adsorptive and / or reactive evaluation apparatus of the present invention uses the temperature programmed desorption method to provide the detection gas by providing the inert gas injection part in the gas discharge channel. This is an apparatus that widens the detectable gas concentration range by lowering the concentration of gas.

  In the gas adsorption and / or reactivity evaluation apparatus according to the present invention, it is preferable that the inert gas injection unit has a second flow rate adjustment unit.

  Thereby, the gas adsorption property and / or reactivity evaluation apparatus of the present invention can adjust the injection amount of the inert gas. As a result, the gas adsorption and / or reactivity evaluation apparatus of the present invention can efficiently and quantitatively evaluate the gas adsorption and / or reactivity.

  In addition, the gas adsorption and / or reactivity evaluation apparatus of the present invention is preferably used for evaluating the gas adsorption and / or reactivity in an object having a catalytic function.

  Thereby, the gas adsorption property and / or reactivity evaluation apparatus of the present invention can be widely applied to the field using the object having a catalytic function.

  As described above, the gas adsorption and / or reactivity evaluation apparatus according to the present invention includes a reaction unit in which an evaluation object is provided, a heating unit that heats the evaluation object, and an interior of the reaction unit. A gas supply channel for flowing gas into the gas, a gas discharge channel for flowing gas from the reaction unit, a flow rate adjusting unit provided in the gas supply channel, and a gas discharge channel An analysis unit that includes a detection unit and analyzes gas adsorption and / or reactivity in the evaluation object is connected to the detection unit and the reaction unit, and an inert gas is provided in the gas discharge channel. An inert gas injection part for injecting gas is provided in the gas discharge flow path, and the detection part contains a component contained in a mixed gas of the gas discharged from the reaction part and the inert gas. It is a device to detect.

  Therefore, the gas adsorptivity and / or reactivity evaluation apparatus according to the present invention has an effect that the gas adsorptivity and / or reactivity in an evaluation object can be evaluated even when a high-concentration gas is used. Play. For example, gas reactivity evaluation (TPR method) when high-concentration gas is continuously circulated, and gas adsorption capacity evaluation (TPD method or TPR method) when high-concentration gas is generated as a result of excessive occlusion as a result of excessive occlusion ) Becomes possible.

It is sectional drawing which shows schematic structure of the evaluation apparatus of the gas adsorptivity and / or reactivity in one Embodiment of this invention. It is sectional drawing which shows schematic structure of evaluation apparatuses, such as the conventional gas adsorption property and reactivity. It is a graph which shows the relationship between the temperature and the amount of desorption gas in the evaluation apparatus, such as general gas adsorption property and reactivity.

  One embodiment of the present invention will be described in detail below, but the scope of the present invention is not limited to these explanations, and modifications other than the following exemplifications are made as appropriate without departing from the spirit of the present invention. Can be implemented.

(I) Configuration of Gas Adsorbency and / or Reactivity Evaluation Device in the Present Embodiment The gas adsorbability and / or reactivity evaluation device in the present embodiment is a reaction in which an evaluation object is provided. A heating section for heating the object to be evaluated, a gas supply flow path for flowing gas into the reaction section, a gas discharge flow path for flowing gas from the reaction section, and the gas supply flow path. A flow rate adjustment unit, and a detection unit provided in the gas discharge flow path, and an analysis unit for analyzing gas adsorption and / or reactivity in the evaluation object includes the detection unit and the An inert gas injection section that is connected to the reaction section and injects an inert gas into the gas discharge flow path is provided in the gas discharge flow path, and the detection section is caused to flow out of the reaction section. Included in the mixed gas of gas and inert gas The component which is present is detected.

  That is, the gas adsorptive and / or reactive evaluation apparatus according to the present embodiment uses a member (inert gas injection unit) for adding an inert gas to a gas flowing out from a gas sample unit (reaction unit) as a sample. By providing it between the part (reaction part) and the detection part, even if the gas has a concentration exceeding the detection upper limit in the detection part, the component can be detected by using a mixed gas with the inert gas.

  Specifically, this will be specifically described with reference to FIG. FIG. 1 is a cross-sectional view showing a schematic configuration of a gas adsorption and / or reactivity evaluation apparatus 10 in the present embodiment.

  As shown in FIG. 1, the gas adsorption and / or reactivity evaluation apparatus 10 in this embodiment includes, for example, a reaction unit 1, a heating unit 2, a gas supply channel 3, a gas discharge channel 4, and a flow rate adjustment. Unit 5, detection unit 7, analysis unit 8, and inert gas injection unit 9. Further, the gas adsorption and / or reactivity evaluation apparatus 10 in this embodiment may further include a gas storage unit 6. In that case, one type of gas may be supplied with the gas supply channel 3, the flow rate adjusting unit 5, and the gas storage unit 6 as one set, and the gas supply channel 3, the flow rate adjusting unit 5, and the gas storage unit 6 are set. There may be multiple. Note that the gas adsorption and / or reactivity evaluation apparatus 10 in the present embodiment has a conventionally known evaluation apparatus for gas adsorption and reactivity other than the inert gas injection unit 9. What is necessary is just to have the structure of. Details of each member will be described below.

<Evaluation object>
In the gas adsorptive and / or reactive evaluation apparatus 10 in the present embodiment, the evaluation object (sample) is not particularly limited as long as it adsorbs at least one kind of gas component. Examples of the evaluation object include an object having a catalytic function (ceramics, silica, activated carbon, etc.), an object to be thermally decomposed (nitrate, sulfate, carbonate, phosphate, etc.), a gas storage alloy (hydrogen Occlusion alloys, etc.). Catalytic functions include oxidation-reduction properties and acid-basic properties.

<Gas adsorption and / or reactivity>
The gas adsorptivity and / or reactivity evaluation apparatus 10 in the present embodiment evaluates at least one of gas adsorptivity and reactivity in an evaluation object.

  Here, “adsorption and / or reactivity” refers to a physical reaction such as adsorption or desorption of a gas from an evaluation object (how much the gas component adsorbs and desorbs at what temperature. And all the interactions that occur between the evaluation object and the gas, such as chemical reactions that occur on the surface of the evaluation object (oxidation-reduction reaction, acid-base reaction, etc.).

<Reaction part>
In the gas adsorption and / or reactivity evaluation apparatus 10 in the present embodiment, the reaction part (sample part) 1 is a member in which an evaluation object is provided. Moreover, it is preferable that the reaction part 1 consists of material which has heat resistance.

  Here, the “reaction part in which the evaluation object is provided” means that in the reaction part, the evaluation object is in contact with the gas flowing in from the gas supply channel, and the gas after contact is Even if the evaluation object is provided in a part inside the reaction part, the evaluation object is in a configuration provided at a position where it can flow out to the gas discharge channel. The aspect provided in the whole inside of the reaction part may be sufficient. The aspect in which the evaluation object is provided in a part inside the reaction part means that the evaluation object is any part inside the reaction part, for example, the central part inside the reaction part, the reaction What is necessary is just to be provided in the part along the inner wall of a part.

<Heating section>
In the gas adsorption and / or reactivity evaluation apparatus 10 in the present embodiment, the heating unit 2 is a member that heats the evaluation object. Examples of the heating unit 2 include a heater.

  In addition, when the reaction part 1 has a heating function, even if the gas adsorption property and / or reactivity evaluation apparatus 10 in this embodiment is not provided with the heating part 2, it is included in the scope of this embodiment.

<Gas supply channel>
In the gas adsorption and / or reactivity evaluation apparatus 10 according to the present embodiment, the gas supply channel (gas supply unit) 3 is a member that allows gas to flow into the reaction unit 1. The gas to be introduced (probe gas) is a gas component to be evaluated for the gas adsorption and / or reactivity of the evaluation object, that is, the gas adsorption ability of the evaluation object and / or the reactivity between the evaluation object and the gas. Contains gas. For _example, He, include a gas containing a component such as _{N 2, O 2, H 2} . Specifically, He or N ₂ may be used as a carrier gas, and O ₂ or H ₂ may be used as a probe, or may be used for adsorption (reaction) before circulating the probe gas. .
Various probe gases for evaluating the interaction between the object to be evaluated and the gas are conceivable. Usually, NH ₃ , CO ₂ , CO, NOx, SO ₂ or the like is used.

<Flow adjustment unit>
In the gas adsorptive and / or reactive evaluation apparatus 10 in the present embodiment, the flow rate adjusting unit 5 is a member that is provided inside the gas supply channel 3 and adjusts the flow rate of the gas to be introduced. Examples of the flow rate adjusting unit 5 include a mass flow controller (MFC).

  If the gas supply flow path 3 has a flow rate adjustment function, the gas adsorption and / or reactivity evaluation apparatus 10 in this embodiment does not include the flow rate adjustment unit 5, but the scope of this embodiment. include.

<Gas storage unit>
In the gas adsorptive and / or reactive evaluation apparatus 10 in the present embodiment, the gas storage unit 6 is a member that stores a gas that flows into the reaction unit 1. Examples of the gas storage unit 6 include a gas cylinder. Further, as the gas storage unit 6, one gas cylinder or the like may be used, or a plurality of gas cylinders or the like may be used.

<Gas discharge flow path>
In the gas adsorptive and / or reactive evaluation apparatus 10 in the present embodiment, the gas discharge channel 4 is a member that allows gas to flow out of the reaction unit 1. Examples of the gas to be flowed out include a reaction desorption gas that is desorbed by heating after being adsorbed on the surface of the evaluation object.

  The gas discharge channel 4 is connected to an exhaust port, and gas can be discharged out of the system from the exhaust port.

<Detector>
In the gas adsorptive and / or reactive evaluation apparatus 10 in the present embodiment, the detection unit 7 is provided in the gas discharge channel 4, and a gas that has flowed out of the reaction unit 1 and an inert gas described later are provided. It is a member which detects the component contained in this mixed gas. Examples of the detection unit 7 include a mass spectrometer, a heat conduction detector, various gas analyzers (NDIR, FT-IR, chemiluminescence NOx meter, SO ₂ meter, etc.), or a device combining them. .

  In the gas adsorptive and / or reactive evaluation apparatus 10 in the present embodiment, the detection target gas is (i) a gas that is adsorbed on the evaluation target and then desorbed with or without increasing the temperature. (Ii) a gas that undergoes a chemical reaction and desorbs with or without an increase in temperature after being adsorbed by the evaluation object; (iii) from the reaction unit 1 without being adsorbed to the evaluation object and without a chemical reaction. Gas that flows out, (iv) Gas that does not adsorb to the evaluation object, causes a chemical reaction by contact with the evaluation object, and flows out of the reaction unit 1.

By detecting the above gas, the interaction between the surface of the object to be evaluated and the gas (physical reaction: adsorption / desorption, chemical reaction: oxidation / reduction, acid-base, etc.) (CO + 1 / 2O ₂ → CO ₂ etc.), etc.).

<Analysis Department>
In the gas adsorption and / or reactivity evaluation apparatus 10 in the present embodiment, the analysis unit 8 is a member that analyzes the gas adsorption and / or reactivity in the evaluation object. The analysis unit 8 is connected to at least the detection unit 7 and the reaction unit 1. The analysis unit 8 may be connected to a part other than the detection unit 7 and the reaction unit 1.

  The analysis unit 8 analyzes the gas components detected by the detection unit 7 and the gas adsorption and / or reactivity of the evaluation object. At that time, for example, information on the gas that has flowed into the reaction unit 1 is obtained from the gas contained in the gas storage unit 6.

  In addition, when the detection part 7 has an analysis function, even if the gas adsorption property and / or reactivity evaluation apparatus 10 in this embodiment is not provided with the analysis part 8, it is included in the scope of this embodiment.

<Inert gas injection part>
In the gas adsorption and / or reactivity evaluation apparatus 10 according to the present embodiment, an inert gas injection unit (gas addition apparatus) 9 is provided in the gas discharge flow path 4, and is not provided in the gas discharge flow path 4. It is a member for injecting active gas. The material, size, etc. of the inert gas injection part 9 are not particularly limited as long as they can inject the inert gas into the gas discharge channel 4. As the inert gas inert gas injection unit 9 is injected, for example, He, include a gas containing a component such as N _2.

  The inert gas injection unit 9 preferably has a second flow rate adjustment unit. Thereby, the injection amount of the inert gas can be adjusted.

  The second flow rate adjusting unit is not particularly limited as long as it can adjust the injection amount of the inert gas. For example, the same one as the flow rate adjusting unit 5 can be used.

  The ratio of the inert gas in the mixed gas of the gas flowing out of the reaction section 1 and the inert gas is preferably in the range of 10% or more and 90% or less, and is 50% or more and 90% or less. More preferably, it is in the range of 80% or more and 90% or less. If the ratio of the inert gas is less than 50%, the gas flowing out from the reaction section 1 cannot be sufficiently diluted. On the other hand, if the ratio of the inert gas is more than 90%, the gas flowing out from the reaction unit 1 is too diluted and cannot be accurately detected by the detection unit 7.

<Other members>
The gas adsorption and / or reactivity evaluation apparatus 10 in this embodiment includes a reaction unit 1, a heating unit 2, a gas supply channel 3, a gas discharge channel 4, a flow rate adjustment unit 5, a detection unit 7, and an analysis unit. 8 and other members other than the inert gas injection part 9 may be provided.

(II) Method for Producing Gas Adsorbability and / or Reactivity Evaluation Device in the Present Embodiment The method for producing the gas adsorbability and / or reactivity evaluation device in the present embodiment includes an inert gas injection unit 9. Other than the provision, a conventionally known method for producing a gas adsorption and / or reactivity evaluation apparatus can be used. The process for manufacturing the inert gas injection part 9 may be a process after the gas discharge channel 4 is manufactured. The process of manufacturing the inert gas injection part 9 is not particularly limited except that the inert gas injection part 9 is manufactured to have the function of the inert gas injection part 9.

(III) Manufacturing Apparatus for Gas Adsorbing and / or Reactive Evaluation Apparatus in the Present Embodiment The manufacturing apparatus for the gas adsorbing and / or reactive evaluating apparatus in the present embodiment includes an inert gas injection unit 9. Other than the provision, a conventionally known apparatus for producing an evaluation apparatus for gas adsorption and / or reactivity can be used. The apparatus for manufacturing the inert gas injection section 9 is not particularly limited except that the apparatus is manufactured so as to have the function of the inert gas injection section 9.

(IV) Examples detector 7 of the adsorptive and / or reactive evaluation apparatus of the gas in the present embodiment, it is possible to use a NOx and SO ₂ meter. An inert gas introduction line is designed upstream of the detection unit 7 and an inert gas injection unit 9 is connected thereto. The role of the inert gas injecting unit 9 is to add an inert gas such as He or N ₂ to the high-concentration detection gas that flows out from the reaction unit (sample unit) 1 and exceeds the detection upper limit, and dilutes the detection unit. 7 to optimize within the detection range.

  The inert gas injection unit 9 may adjust the flow rate of the inert gas to be supplied using a mass flow controller (MFC). Therefore, the range in which dilution can be performed can be widened by increasing the capacity of the mounted MFC. In addition, various gas analyzers can be applied to the detection unit 7 according to the detected components, but the detection range can be expanded by using a more sensitive analyzer.

  Specifically, in many cases, the conventional TPD system uses a gas diluted to a low concentration in advance, or various gas cylinders and MFC at the same time, and distributes the diluted gas by mixing the circulating gas to the sample part. Let This is to optimize the concentration of the gas introduced into the detection unit within the detection range of the detection unit. In other words, in the conventional system, the measurable concentration of TPD or TPR measurement depends on the performance of the detection unit. For example, the detection range is about several ppb to 1 ppm order in the mass spectrometer which is a high sensitivity analyzer, and about several hundred ppb to 0.1% in the chemiluminescence type NOx meter.

In contrast, when using the inert gas injection method of the present embodiment, the lower limit of detection is determined by the performance of the detection unit, but by diluting the evaluation gas with an inert gas such as He or N ₂ , The detection upper limit can be expanded. For example, in the TPD system using the inert gas injection method of this embodiment, the maximum flow rate of the evaluation gas is 100 mL / min. In contrast, a maximum of 1200 mL / min. Therefore, when a chemiluminescent NOx meter with a detection range of several hundred ppb to 5000 ppm is used as the detection unit, the detection range that can be measured is several hundred ppb to 6.5% (the detection upper limit is , Which is about 13 times the upper limit of detection of the conventional TPD system). This detection range can be further expanded by using a more sensitive detector, increasing the MFC capacity mounted in the inert gas injection section, or the like. That is, in this embodiment, it becomes possible to analyze gas components under a wide range of gas concentration conditions that could not be handled conventionally.

(V) Use of gas adsorption and / or reactivity evaluation apparatus in this embodiment The gas adsorption and / or reactivity evaluation apparatus in this embodiment is used for various applications. For example, it is used for evaluating gas adsorption and / or reactivity in an object having a catalytic function. Thereby, the gas adsorption property and / or reactivity evaluation apparatus of the present invention can be widely applied to the field using the object having a catalytic function.

(VI) Other Embodiments The present invention is not limited to the above-described embodiments, and various modifications are possible within the scope of the claims. That is, embodiments obtained by combining technical means appropriately modified within the scope of the claims are also included in the technical scope of the present invention.

  The present invention can be used in a wide range of fields such as industrial chemistry-related, pharmaceutical-related, food-related, electrical / electronic-related, fuel cell-related, exhaust gas treatment-related, secondary battery (lithium ion battery, etc.)-Related.

DESCRIPTION OF SYMBOLS 1 Reaction part 2 Heating part 3 Gas supply flow path 4 Gas discharge flow path 5 Flow rate adjustment part 6 Gas storage part 7 Detection part 8 Analysis part 9 Inert gas injection part 10 Gas adsorption property and / or reactivity evaluation apparatus

Claims (3)

A reaction part in which an evaluation object is provided, a heating part for heating the evaluation object, a gas supply channel for allowing gas to flow into the reaction part, and a gas discharge channel for allowing gas to flow out from the reaction part A flow rate adjusting unit provided in the gas supply flow path, and a detection unit provided in the gas discharge flow path,
The analysis unit for analyzing the gas adsorption and / or reactivity in the evaluation object is connected to the detection unit and the reaction unit,
An inert gas injection part for injecting an inert gas into the gas discharge channel is provided in the gas discharge channel;
A gas adsorption and / or reactivity evaluation apparatus in which the detection unit detects a component contained in a mixed gas of the gas flowing out of the reaction unit and the inert gas.   The gas adsorption property and / or reactivity evaluation device according to claim 1, wherein the inert gas injection unit includes a second flow rate adjustment unit.   The gas adsorption property and / or reactivity evaluation apparatus according to claim 1 or 2, which is used for evaluating gas adsorption property and / or reactivity in an object having a catalytic function.

Images