CN104165921A - Intermittent ultra-low pressure surface reaction apparatus - Google Patents
Intermittent ultra-low pressure surface reaction apparatus Download PDFInfo
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- CN104165921A CN104165921A CN201310187501.0A CN201310187501A CN104165921A CN 104165921 A CN104165921 A CN 104165921A CN 201310187501 A CN201310187501 A CN 201310187501A CN 104165921 A CN104165921 A CN 104165921A
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Abstract
The invention provides an intermittent ultra-low pressure surface reaction apparatus. The intermittent ultra-low pressure surface reaction apparatus mainly comprises a reaction chamber, a gas source, a gas storage bottle, a vacuum pump, a temperature controller, a pressure sensor, a mass spectrometry detector, etc. Each part in the reaction apparatus is mutually connected through a leak valve. Samples are placed in the reaction chamber, and vacuumization of or introduction of gas with certain pressure into the reaction chamber can be realized through cooperation of the leak valve. During introduction of gas, gas in the gas source diffuses into the gas storage bottle at first and is then introduced into the reaction chamber for sample pretreatment or reaction; during a reaction, a part of gas products in the reaction chamber are introduced into the mass spectrometry detector for on-line analysis; and thus, determination of reaction performance of samples with low reaction activity is completed. The apparatus provided by the invention has an ingenious design and a simple structure, is convenient to operate and shows wide practical values and application prospects in the field of research on catalyst surfaces, especially in determination of reaction performance of samples with low activity.
Description
Technical field
The present invention relates in general to the instrument field of catalyst reaction performance test, is specifically to provide a kind of intermittent reaction device with ultralow surface reaction activity that can be used for measuring.
Background technology
Intermittent reaction device is a kind of integration type reactor, and with respect to differential expression reactor, intermittent reaction device is having unique advantage aspect the reactivity worth mensuration for the low especially sample of activity.In catalyst surface research field, sometimes due to the restriction of catalyst surface area, reactivity is very low, sometimes for the course of reaction on Study of Catalyst surface, need under very low pressure condition, carry out, to get rid of the impact of chemical kinetics factor, so all can cause product amount little, therefore product need to be accumulated.In intermittent reaction device, the product of reaction is along with the reaction time is accumulated, and after being accumulated to a certain degree, desirable portion of product is measured, but at this moment can only carry out the sampling of off-line, and can not carry out on-line analysis to reaction product.In fact, we often wish to adopt mass spectrum to carry out the on-line analysis of product, and simultaneously owing to being subject to the impact of mass spectrographic working pressure, mass spectrographic sample size is very low, and (pressure of injection port generally will be lower than 10
-6torr), this has limited mass spectrographic application widely, and traditional structure and method not yet can solve the mensuration of the reactivity worth of active low sample, yet there are no so far the report of relevant solution in patent.
The invention provides a kind of brand-new intermittent reaction device that can be used for the reactivity worth of measuring the sample with ultralow surface reaction activity, this device has solved the series of problems such as distribution, reaction generation, product detection of reaction gas, really realizes the mensuration of the reactivity worth to low reaction activity sample.This device design is ingenious, simple in structure, easy to operate, and in catalyst surface research field, particularly the mensuration aspect of the reactivity worth of low activity sample has practical value and application prospect widely.
Summary of the invention
The present invention has designed a kind of brand-new can be used for and has measured the intermittent reaction device with ultralow surface reaction activity, and considers emphatically the problem existing in design.For example to consider rationality and the operability of each steps such as distribution, introducing, reaction generation, collection of products and the detection of reaction gas and link, therefore the structure of this batch reactor be carried out to special design.
Specifically, discontinuous formula reaction unit of the present invention is mainly made up of parts such as reaction chamber, source of the gas, gas bomb, vacuum pump, temperature controller, pressure transducer, mass detectors.All parts in reaction unit connects by multiple leak valves.In reaction chamber, place sample, can carry out heat treated to sample, can introduce gas or vacuumize processing.Vacuum pump is for vacuumizing processing to reaction chamber.Temperature in reaction chamber shows by temperature controller and controls, and pressure is shown by pressure transducer, is vacuumized or introduced the gas of certain pressure by the cooperation of leak valve.While introducing gas, in source of the gas, gas first diffuses in gas bomb, carries out the distribution of reaction gas, and the reaction gas of then introducing certain pressure by gas bomb is to reaction chamber, for sample pretreatment or reaction.In course of reaction, part gaseous product in reaction chamber can be introduced in mass spectrum, carry out the on-line analysis of product, can complete like this mensuration of the reactivity worth to low reaction activity sample.
Be elaborated below in conjunction with accompanying drawing
Fig. 1 is the framework schematic diagram of the batch (-type) low pressure surface reaction unit of patent of the present invention;
Fig. 2 is the structural representation of the batch (-type) low pressure surface reaction unit of a kind of embodiment of patent of the present invention.
As the framework schematic diagram of Fig. 1 batch (-type) low pressure surface reaction unit that is patent of the present invention.Discontinuous formula reaction unit of the present invention is mainly made up of parts such as reaction chamber 1, mass detector 2, gas bomb 3, source of the gas 4, vacuum pump 5, temperature controller 6, pressure transducers 7.The interior placement sample of reaction chamber 1, can carry out heat treated to sample, can introduce gas or vacuumize processing.Vacuum pump 5 is for carrying out application of vacuum to reaction chamber 1.Temperature in reaction chamber 1 shows and controlled by temperature controller 6, and pressure is shown by pressure transducer 7, can be vacuumized or be introduced by the cooperation of leak valve the gas of certain pressure.Introduce when gas, the interior gas of source of the gas 4 first diffuses in gas bomb 3, carries out the distribution of reaction gas, then introduces certain reaction gas to pre-service or the reaction of carrying out sample in reaction chamber 1 by gas bomb 3.When reaction, interior reaction chamber 1 part gaseous product can be introduced in mass spectrum 2, carry out the on-line analysis of product.
As the structural representation of the batch (-type) low pressure surface reaction unit of Fig. 2 a kind of embodiment that is patent of the present invention.All parts in reaction unit is connected with multiple leak valves 91～102 by three adjustable leak valves 81～83.For example reaction chamber 1, by leak valve 101 and 100 or be directly connected with vacuum pump 5 by leak valve 99, is connected with mass spectrum 2 with 102 by leak valve 101; Gas bomb 41～43 connects respectively leak valve 91～93, is connected with leak valve 97 by adjustable leak valve 82 with gas bomb 3, and 3 of gas bombs are connected with vacuum pump 5 by leak valve 94～96.Source of the gas 4 is made up of 3 gas bombs 41～43, and concrete quantity can require to select according to user.Pressure transducer 7 is made up of vacuum gauge 1 and vacuum gauge 2 72, is connected to reaction chamber 1 and gas bomb 3 respectively by leak valve 98 and leak valve 96, can be respectively used to the gaseous tension in detection reaction chamber 1 and gas bomb 3.This device organically combines source of the gas 4, gas bomb 3, vacuum pump 5, reaction chamber 1 and mass spectrum 2 by leak valve 91～102 and/or adjustable leak valve 81～83, by the adjusting of leak valve 91～102 and/or adjustable leak valve 81～83, can in gas bomb 3, carry out the distribution of definite composition gas, the reacting gas that can process and introduce to vacuumizing in reaction chamber 1 certain pressure carrys out realization response process, interior reaction chamber 1 portion gas can be introduced to the on-line analysis of carrying out product in mass spectrum 2.Specific operation process is as follows:
1. distribution process: close adjustable leak valve 81 and 82, open leak valve 91～97, vacuum pump 5 directly vacuumizes the pipeline of 91～97 of gas bomb 3 and leak valves.Rear stop-and-waste valve 91～97, open one and corresponding leak valve 91～93 in gas bomb 41～43, by the openings of sizes of the adjustable leak valve 82 of slow adjusting, to valve 81,82,95～97 and vacuum gauge 2 72 round pipeline in introduce the gas of certain pressure, the pressure of introducing gas shows by vacuum gauge 2 72.Open again leak valve 96 or 97, this gas in pipelines diffuses in gas bomb 3, can repeat successively above vacuumizing and gas replenishment process, by clean the pipeline cleaning between gas bomb 3 and leak valve 91～97, after 3～4 times, in one by gas upon adsorption from gas bomb 41～43, be incorporated in gas bomb 3, complete gas replenishment process.Other gas also can be incorporated in gas bomb 3 and be mixed by the same manner, obtains the hybrid reaction gas of definite composition ratio, treats adapted.
2. course of reaction: the temperature of reaction that interior reaction chamber 1 sample is heated to setting.Introduce before gas, open leak valve 96 or 97, the interior gas of gas bomb 3 diffuse to valve 81,82,95～97 and vacuum gauge 2 72 round pipeline in, by the slow adjusting of adjustable leak valve 81, make a certain amount of gas diffuse to further vacuum gauge 1, valve 81 and 98 round pipeline in, vacuum gauge 1 demonstrates the pressure of introducing gas.Open leak valve 98, gas quickly diffuses in reaction chamber 1 and reacts, and opens leak valve 98 and introduces the starting point that the moment of gas is reaction.
3. testing process: after question response a period of time, open leak valve 101, partial reaction product gas from reaction chamber 1 diffuse to leak valve 100～102 round pipeline, after close reveal valve 101.Adjustable leak valve 83 before mass spectrum 2 is semi-open state, in the time opening leak valve 102, due to leak valve 100～102 round pipeline and the front huge pressure differential of mass spectrum 2, the reaction product gas moment of deposit enters in mass spectrum 2 in this pipeline, realizes the analysis of product.After to be analyzed, shut and reveal valve 102, open and reveal valve 100, the gas of this pipeline remnants is taken away to (generalized case does not have remnants, and gas is easy to all enter in mass spectrum), detect in order to reaction product next time.In fact, can reveal the distance of valve 100～102 and change the thickness of this pipeline by adjusting, make the volume of this pipeline be far smaller than the volume of reaction chamber 1, the amount of the gas of so each detection is negligible than the amount of reactant gases in reaction chamber, the pressure of reaction chamber 1 reaction gases almost remains unchanged, and can realize like this gas sampling mass spectrophotometry of continuous several times.
On this batch (-type) ultralow pressure surface reaction device, the process such as distribution, introducing, reaction generation, collection of products and detection that can realization response gas, completes the mensuration of the reactivity worth of ultralow reactivity sample.This device design is ingenious, simple in structure, easy to operate, and in catalyst surface research field, particularly the mensuration aspect of the reactivity worth of low activity sample has practical value and application prospect widely.
Claims (3)
1. batch (-type) ultralow pressure surface reaction device.
2. according to batch (-type) ultralow pressure surface reaction device claimed in claim 1, it is characterized in that it is mainly made up of parts such as reaction chamber, source of the gas, gas bomb, vacuum pump, temperature controller, pressure transducer, mass detectors.
3. according to batch (-type) ultralow pressure surface reaction device claimed in claim 1, it is characterized in that placing sample in reaction chamber, can carry out heat treated to sample, can introduce gas or vacuumize processing.Vacuum pump is for vacuumizing processing to reaction chamber.Temperature in reaction chamber shows by temperature controller and controls, and pressure is shown by pressure transducer, is vacuumized or introduced the gas of certain pressure by the cooperation of leak valve.While introducing gas, in source of the gas, gas first diffuses in gas bomb, carries out the distribution of reaction gas, and the reaction gas of then introducing certain pressure by gas bomb is to reaction chamber, for sample pretreatment or reaction.When reaction, reaction intracavity gas can be introduced in mass spectrum, carry out product on-line analysis.
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| CN201310187501.0A CN104165921A (en) | 2013-05-20 | 2013-05-20 | Intermittent ultra-low pressure surface reaction apparatus |
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| CN201310187501.0A CN104165921A (en) | 2013-05-20 | 2013-05-20 | Intermittent ultra-low pressure surface reaction apparatus |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784917A (en) * | 2014-12-26 | 2016-07-20 | 中国科学院大连化学物理研究所 | Application of mass spectrometer to detection process of ionized intermediates in catalytic reaction |
| CN107663163A (en) * | 2016-07-27 | 2018-02-06 | 深圳市中核海得威生物科技有限公司 | One kind is used for13The unstripped gas fill method of C urea synthesizings |
| CN107870192A (en) * | 2017-01-23 | 2018-04-03 | 黄华 | Batch (-type) low-pressure surface reaction unit |
| CN113670701A (en) * | 2021-08-20 | 2021-11-19 | 中国科学院西北生态环境资源研究院 | Gas purification device, and rare gas isotope measuring equipment and method |
-
2013
- 2013-05-20 CN CN201310187501.0A patent/CN104165921A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784917A (en) * | 2014-12-26 | 2016-07-20 | 中国科学院大连化学物理研究所 | Application of mass spectrometer to detection process of ionized intermediates in catalytic reaction |
| CN105784917B (en) * | 2014-12-26 | 2018-06-29 | 中国科学院大连化学物理研究所 | Application of the mass spectrograph during detection is catalyzed reactive ion intermediate |
| CN107663163A (en) * | 2016-07-27 | 2018-02-06 | 深圳市中核海得威生物科技有限公司 | One kind is used for13The unstripped gas fill method of C urea synthesizings |
| CN107663163B (en) * | 2016-07-27 | 2020-06-30 | 深圳市中核海得威生物科技有限公司 | Is used for13Raw material gas filling method for C-urea synthesis |
| CN107870192A (en) * | 2017-01-23 | 2018-04-03 | 黄华 | Batch (-type) low-pressure surface reaction unit |
| CN113670701A (en) * | 2021-08-20 | 2021-11-19 | 中国科学院西北生态环境资源研究院 | Gas purification device, and rare gas isotope measuring equipment and method |
| CN113670701B (en) * | 2021-08-20 | 2024-01-23 | 中国科学院西北生态环境资源研究院 | Gas purification device, rare gas isotope measurement equipment and method thereof |
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