CN100336598C - Self heat exchanging type catalyst rate recactor - Google Patents
Self heat exchanging type catalyst rate recactor Download PDFInfo
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- CN100336598C CN100336598C CNB2005100137772A CN200510013777A CN100336598C CN 100336598 C CN100336598 C CN 100336598C CN B2005100137772 A CNB2005100137772 A CN B2005100137772A CN 200510013777 A CN200510013777 A CN 200510013777A CN 100336598 C CN100336598 C CN 100336598C
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Abstract
本发明公开了一种自换热式催化剂评价反应器，属于催化剂评价反应装置。该反应器包括密封头、密封头内的直角梯形橡胶密封垫圈和反应管，所述的密封头由连接体及与其上部连接的上密封帽、与其下部连接的下密封套组成；下密封套内侧设置一个下45°直角梯形橡胶密封垫圈；上密封帽内侧设置一个上45°直角梯形橡胶密封垫圈；所述的反应管由三根同心石英玻璃管组成，其中外层石英玻璃管与中间层石英玻璃管的环形间隙为反应气体流入通道，中间层石英玻璃管底部开设气体通孔，内置反应催化剂，它与内层石英玻璃管的环形间隙为反应生成气体流出通道。该发明强化了反应气与生成气之间的热交换，具有反应生成气体温度低，拆卸方便，气密性好，死体积小等优点。
The invention discloses a self-heat exchange catalyst evaluation reactor, which belongs to catalyst evaluation reaction devices. The reactor includes a sealing head, a right-angled trapezoidal rubber sealing washer in the sealing head and a reaction tube. The sealing head is composed of a connecting body, an upper sealing cap connected to its upper part, and a lower sealing sleeve connected to its lower part; the inner side of the lower sealing sleeve A lower 45° right-angled trapezoidal rubber sealing gasket is set; an upper 45° right-angled trapezoidal rubber sealing gasket is arranged on the inside of the upper sealing cap; the reaction tube is composed of three concentric quartz glass tubes, wherein the outer layer of quartz glass tube and the middle layer of quartz glass The annular gap of the tube is the inflow channel of the reaction gas, the bottom of the middle quartz glass tube is provided with a gas through hole, and the reaction catalyst is built in, and the annular gap between it and the inner quartz glass tube is the outflow channel of the reaction gas. The invention strengthens the heat exchange between the reaction gas and the generated gas, and has the advantages of low temperature of the reaction gas, convenient disassembly, good air tightness, small dead volume and the like.
Description
Technical field:
The present invention relates to a kind ofly, belong to the evaluating catalyst reaction unit from heat exchange type evaluating catalyst reactor.
Background technology:
The performance evaluation of catalyst plays important directive function as the important means of catalyst characterization in catalyst research.The reactor that present laboratory is used for the catalytic perfomance evaluation mainly contains two kinds: a kind of is U type tubular reactor, and another kind is a straight tubular reactor.The reaction tube volume of U type tubular reactor is less, is mainly used in to estimate the granular pattern catalyst, and the reaction tube material is generally quartz glass; The straight tubular reactor volume is bigger, is used to estimate integral catalyst or granular pattern catalyst, and the reaction tube material is generally metal or quartz glass.In the use, traditional U type pipe reactor and straight tubular reactor are extruded with following shortcoming: the first, and the temperature of reactor outlet reactant is very high, is generally 300-500 ℃.Often need the special cooling device of assembling to reduce the temperature of outlet reactant,, increased the cost of system to reduce the damage of high-temperature gas to sealing rubber ring, downstream pipeline and the checkout equipment of reactor exit; The second, traditional reactor is realized its sealing by extruding O type rubber ring or cutting ferrule usually, and the loading and unloading trouble through regular meeting the improper and leakage of the reactor that causes of O type rubber ring or cutting ferrule loading and unloading takes place, and is difficult to guarantee the air-tightness of reactor assembly; The 3rd, traditional reactor dead volume is big, and the back-mixing of can induce reaction thing and product, back-mixing can make the concentration data result of reactant and product depart from its actual concentration, increases the systematic error of reactor, causes the catalyst performance assessment to lack accuracy.
Summary of the invention:
The object of the present invention is to provide a kind of self heat exchanging type catalyst rate recactor, characteristics such as this is answered, and utensil has that exchange capability of heat is strong, good airproof performance, easy accessibility and reactor dead volume are little.
The present invention by following technical proposals as to realize, a kind of self heat exchanging type catalyst rate recactor, this reactor comprises right-angled trapezium rubber gasket and the reaction tube in seal head, the seal head, it is characterized in that: reaction tube is made up of three concentric quartz glass tubes, the annular gap of its ectomesoderm quartz glass tube and intermediate layer quartz glass tube is the reacting gas flow channel, and its gap is 0.1-2mm; Gas via-hole is offered in quartz glass tube bottom in intermediate layer, built-in catalysts, and it is reaction generation gas flow pass with the annular gap of internal layer quartz glass tube, its gap is 0.1-2mm.Internal layer quartz glass tube hub inserts thermocouple, with the monitoring reaction bed temperature.Described seal head is made up of the connector of connecting thread section and the last sealing cap that is connected with connector top, the lower sleeve gasket that is connected with the connector bottom the two ends of a hollow.Wherein, following 45 ° of right-angled trapezium rubber gaskets are set between lower sleeve gasket and inboard, connector lower surface, are used for the sealable outer quartz glass tube; Last 45 ° of right-angled trapezium rubber gaskets are set between last sealing cap and the inboard, connector upper surface, are used to seal the intermediate layer quartz glass tube; The connector middle part is established through hole and is communicated with the annular gap of outer quartz glass tube and middle quartz glass tube, as reaction gas inlet; Connector upper surface sidepiece is established through hole and is communicated with the annular gap of intermediate layer quartz ampoule and internal layer quartz ampoule, generates gas vent as reaction; Connector upper surface central authorities establish through hole, connect galvanic couple sealed screw and fixing seal thermocouple.
Above-mentioned quartz glass length of tube is 100-500mm, and outer quartz glass tube diameter is 18-40mm.
Because the countercurrent heat-transfer process between reactant and the product, the present invention has strengthened the heat exchange between cold reactant and the hot product, need not to assemble special cooling device, can effectively reduce the temperature of exit product, reduce product to the aging of gas outlet rubber washer, pipeline and to the infringement of checkout equipment; Compare with extruding O type rubber ring or cutting ferrule, the right-angled trapezium rubber washer seals the linear sealing that substitutes traditional O type circle with face, and being flexible coupling with rubber has substituted the hard connection of cutting ferrule, has reduced the dismounting difficulty of reactor, has improved the air-tightness of reactor; The rubber ring seal of employing right-angled trapezium has reduced the requirement to metal parts and quartz glass tube machining accuracy, and Practical Performance is better; The concentric installation of outer quartz glass tube, intermediate layer quartz glass tube and internal layer quartz glass tube has reduced the dead volume of reactor, has avoided the back-mixing between product and the reactant, has reduced the systematic error of reactor.
Description of drawings:
Fig. 1 is a structural representation of the present invention.
Among the figure: 1 is last sealing cap; 2 is air inlet; 3 is connector; 4 is lower sleeve gasket; 5 is outer quartz glass tube; 6 is the intermediate layer quartz glass tube; 7 is the internal layer quartz glass tube; 8 is the silica wool supporting layer; 9 is catalyst layer; 10 is the silica wool cover layer; 11 is thermocouple; 12 is following 45 ° of right-angled trapezium rubber gaskets; 13 is last 45 ° of trapezoidal seal washers of right angle rubber; 14 is the gas outlet; 15 is the galvanic couple sealed screw; 16 is the galvanic couple hermetic collar.
The specific embodiment:
Should comprise right-angled trapezium rubber gasket and reaction tube in seal head, the seal head from heat exchange type evaluating catalyst reactor.Reaction tube is made up of three concentric quartz glass tubes, is respectively to grow to be the outer quartz glass tube 5 of 230mm, grows for the intermediate layer quartz glass tube 6 of 250mm and grow to be the internal layer quartz glass tube 7 of 210mm.Three quartz ampoules are installed with one heart, and its ectomesoderm quartz glass tube 5 is 0.25mm with the annular gap of intermediate layer quartz glass tube 6, and intermediate layer quartz glass tube 6 is 0.25mm with the annular gap of internal layer quartz glass tube 7.
The catalyst that is used to estimate places intermediate layer quartz glass tube 6 bottoms.When estimating the powder-type catalyst, its filling order is followed successively by from down to up: silica wool supporting layer 8, beds 9 and silica wool cover layer 10; When estimating integral catalyst, need not to load silica wool, only need to place beds 9 to get final product integer catalyzer.Galvanic couple 11 is inserted into beds 9 by the center of internal layer quartz glass tube 7.
Seal head is made up of the lower sleeve gasket 4 of the last sealing cap 1 of the connector 3 of the diameter phi 65mm of connecting thread section and the diameter phi 55mm that is connected with its top, the diameter phi 51mm that is connected with its underpart the two ends of a hollow.Wherein, last 45 ° of right-angled trapezium rubber gaskets 13 are set between last sealing cap 1 and the inboard, connector 3 upper surface, are used to seal intermediate layer quartz glass tube 6; Between lower sleeve gasket 4 and inboard, connector 3 lower surface, following 45 ° of right-angled trapezium rubber gaskets 12 are set, are used for sealable outer quartz glass tube 5.
Reacting gas enters reactor by air inlet 2, and the annular gap of the 0.25mm that constitutes along outer quartz glass tube 5 and intermediate layer quartz glass tube 6 flow to outer quartz glass tube 5 bottoms downwards, passes through beds by the aperture of intermediate layer quartz glass tube 6 bottoms.Through the catalytic action of catalyst, reaction generates gas upwards flow to intermediate layer quartz glass tube 6 along intermediate layer quartz glass tube 6 and the annular gap of the 0.25mm of internal layer quartz glass tube 7 formations top.Final gas outlet 14 outflow reactors along last sealing cap 1 upper surface sidepiece.
In the entire reaction course, the downward inflow reactor in annular gap of the 0.25mm that cold reacting gas is made of outer quartz glass tube 5 and intermediate layer quartz glass tube 6, and the reaction of the heat that generates through catalytic action generates the annular gap of the 0.25mm that gas is made of intermediate layer quartz glass tube 6 and internal layer quartz glass tube 7 outflow reactor that makes progress.Reacting gas is opposite with reaction generation gas flow direction, has finished the countercurrent heat-transfer process by the tube wall of intermediate layer quartz glass tube 6.This countercurrent heat-transfer process has realized the hot-swap feature of self heat exchanging type catalyst rate recactor.
1. adopt apparatus of the present invention to implement the H of granular pattern catalyst
2-TPR evaluation procedure:
(1) estimate the granular pattern catalyst,, 30mg catalyst 9 put thereon in the bottom of intermediate layer quartz glass tube 6 assembling silica wool supporting layer 8, on cover one deck silica wool 10, then reaction tube and seal head are assembled, connect air inlet 2 and gas outlet 14.Reaction tube bottom is placed the flat-temperature zone of heating furnace, and with the reaction tube upper exposed under room temperature condition to guarantee the heat exchange operate as normal.
(2) H of feeding 4% (volume fraction)
2/ He gas, by flow control system, the setting reaction velocity is 100000h
-1The heatable catalyst bed, the heating furnace heating rate is 10 ℃/min, is 50-900 ℃ between heating zone.Through the catalytic action of granular pattern catalyst, H
2Be converted into H
2O.Adopt the online detection of QMS H
2Concentration.Reaction temperature is by the galvanic couple 11 online detections of inserting in the catalyst layer 9.
(3) with the temperature be abscissa, H
2Concentration be that ordinate is drawn H
2Concentration-temperature characteristics.
2. adopt apparatus of the present invention to implement the CO catalytic oxidation performance evaluation procedure of integral catalyst:
(1) estimate integral catalyst, evaluation procedure need not to assemble silica wool supporting layer 8 and silica wool cover layer 10, directly catalyst 9 is positioned over the bottom of intermediate layer quartz glass tube 6.Connect gas circuit, reaction tube bottom placed the flat-temperature zone of heating furnace, and with the reaction tube upper exposed under room temperature condition.
(2) feed the CO/N of 4% (volume fraction) simultaneously
2O with 2% (volume fraction)
2/ N
2Gas, by flow control system, the setting reaction velocity is 30000h
-1The heatable catalyst bed, the heating furnace heating rate is 10 ℃/min, is 50-800 ℃ between heating zone.The catalytic action of the integral catalyst of process heating, CO is converted into CO
2Adopt five component exhaust analyzers, online detection CO, CO
2, O
2Concentration.Reaction temperature is by the galvanic couple 11 online detections of inserting in the catalyst layer 9.
(3) calculate the conversion ratio of CO when different temperatures.With the temperature is abscissa, and conversion ratio is that ordinate is drawn CO conversion ratio-temperature characteristics.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100137772A CN100336598C (en) | 2005-06-13 | 2005-06-13 | Self heat exchanging type catalyst rate recactor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100137772A CN100336598C (en) | 2005-06-13 | 2005-06-13 | Self heat exchanging type catalyst rate recactor |
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| Publication Number | Publication Date |
|---|---|
| CN1724135A CN1724135A (en) | 2006-01-25 |
| CN100336598C true CN100336598C (en) | 2007-09-12 |
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| CNB2005100137772A Expired - Fee Related CN100336598C (en) | 2005-06-13 | 2005-06-13 | Self heat exchanging type catalyst rate recactor |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2470131B1 (en) | 2009-08-24 | 2014-11-12 | New Phase Ltd | Phase-change materials |
| CN103990421B (en) * | 2014-05-19 | 2016-11-23 | 中国科学院宁波材料技术与工程研究所 | Device and multiphase gas-solid reaction method for multiphase gas-solid reaction |
| EP3226819B1 (en) | 2014-11-25 | 2018-10-24 | New Phase Ltd. | Phase-change nanoparticle |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003078051A2 (en) * | 2002-03-12 | 2003-09-25 | Uop Llc | Process for evaporation in an array and an array of process vessels with integral evaporator |
| WO2004020084A1 (en) * | 2002-08-29 | 2004-03-11 | Uop Llc | Combinatorial catalytic reactor |
| CN1512911A (en) * | 2001-06-06 | 2004-07-14 | �����ɷ� | Reactor for testing catalyst systems |
| CN1579612A (en) * | 2004-05-19 | 2005-02-16 | 中国科学院山西煤炭化学研究所 | Reactor for catalytic reaction research |
-
2005
- 2005-06-13 CN CNB2005100137772A patent/CN100336598C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1512911A (en) * | 2001-06-06 | 2004-07-14 | �����ɷ� | Reactor for testing catalyst systems |
| WO2003078051A2 (en) * | 2002-03-12 | 2003-09-25 | Uop Llc | Process for evaporation in an array and an array of process vessels with integral evaporator |
| WO2004020084A1 (en) * | 2002-08-29 | 2004-03-11 | Uop Llc | Combinatorial catalytic reactor |
| CN1579612A (en) * | 2004-05-19 | 2005-02-16 | 中国科学院山西煤炭化学研究所 | Reactor for catalytic reaction research |
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| CN1724135A (en) | 2006-01-25 |
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