CN204269615U - A kind of catalyst test apparatus - Google Patents

A kind of catalyst test apparatus Download PDF

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Publication number
CN204269615U
CN204269615U CN201420542163.8U CN201420542163U CN204269615U CN 204269615 U CN204269615 U CN 204269615U CN 201420542163 U CN201420542163 U CN 201420542163U CN 204269615 U CN204269615 U CN 204269615U
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China
Prior art keywords
reactor
communicated
gas
tail gas
delivery outlet
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Expired - Fee Related
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CN201420542163.8U
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Chinese (zh)
Inventor
李春启
李德炳
陈爱平
陈元应
冯巍
梅长松
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Datang International Chemical Technology Research Institute Co Ltd
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Datang International Chemical Technology Research Institute Co Ltd
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Abstract

The utility model relates to a kind of catalyst test apparatus, comprising: protective gas feedway (2), methanol tank (3), deionized water storage tank (4), the first reactor (18) being filled with the catalyzer carrying out preparing dimethyl ether from methanol reaction, the second reactor (19) being filled with the catalyzer carrying out methyl alcohol and dimethyl ether olefine reaction, gas chromatograph (24).The utility model adopts the mode of double-reactor series connection, experimentally object, rely on the switching of three-way switch valve, on same device, realize catalyzer decatize (hydrothermal treatment consists), the evaluation of DME catalyst activity first, simulate the processes such as industrial MTP evaluating catalyst and catalyst regeneration, solve the problem of tail gas safe discharge simultaneously.

Description

A kind of catalyst test apparatus
Technical field
The utility model relates to coal chemical technology, in particular to a kind of Chemical Manufacture simulating-estimating device, and particularly a kind of multi-functional catalyst test apparatus for the differential responses such as preparing propylene by methanol transformation and methanol conversion preparing dimethy ether and modification.
Background technology
Propylene is a kind of important Organic Chemicals.In recent years, along with the ongoing shortage of petroleum resources and the requirement of the strategy of sustainable development, in the world the research institution of many countries all endeavour to develop non-petroleum synthesizing low-carbon alkene technology path wherein with the methyl alcohol of coal-based or rock gas base synthesis for raw material, the chemical process technology (being called for short " MTP ") of main production propylene receives publicity day by day, comparatively abundant according to coal resources in China, and the feature of relative low price, adopt coal not only can reduce China's depending on unduly petroleum resources through low-carbon alkenes such as preparing propylene from methanol, and meet the demand of national economy sustainable growth and realize strategic reserve.
Do not consider its circulation technology, now strange (the L ü rgi) process for preparing propylene from methanol in the Shandong of successful commercialization adopts fixed bed reactors, alkene is obtained through two-step approach, namely material benzenemethanol is after preparing dimethyl ether from methanol (DME) catalyzer reacts, and the methyl alcohol of generation and dimethyl ether potpourri generate the organic product of C1 ~ C9 after MTP catalyst reaction.Therefore, complete MTP technique needs the respective performance simultaneously investigating MTP catalyzer and DME catalyzer.In addition, according to the study, MTP catalyzer is generally parent with ZSM-5 molecular sieve, and the modified techniques such as suitable water treatment are conducive to the hydro-thermal reaction performance improving catalyzer.
Current, catalyst for producing propylene with methanol itself is paid close attention in most invention and research, to the device used needed for the preparing dimethyl ether from methanol in MTP technological process and methanol-to-olefin catalyst performance evaluation pay close attention to relatively less.Can only be applied to for evaluating apparatus at present and evaluate single catalytic reaction, the kinds of experiments demands such as preparing dimethyl ether from methanol catalyzer, preparing propylene from methanol and MTP catalyzer hydrothermal treatment consists can not be realized simultaneously, therefore a kind of easy and simple to handle, multiduty catalyst test apparatus of research is for the reaction of simulation actual condition, reduces the tools such as plant investment and has very great significance.In addition, the reaction end gas amount of the catalytic evaluation reaction under high-speed is large, if directly discharge often blocks offgas duct because of the condensation of high-carbon component, but also indoor pollutant can be caused to exceed standard.
Utility model content
The purpose of this utility model is to overcome above-mentioned deficiency of the prior art, provides a kind of catalyst test apparatus for the differential responses such as preparing propylene by methanol transformation and methanol conversion preparing dimethy ether and modification easy and simple to handle, multiduty.
The utility model is achieved by following technical proposals:
A kind of catalyst test apparatus, comprising: protective gas supply fills 2, methanol tank 3, deionized water storage tank 4, be filled with the first reactor 18 of the catalyzer carrying out preparing dimethyl ether from methanol reaction, be filled with the second reactor 19, the gas chromatograph 24 of the catalyzer carrying out methyl alcohol and dimethyl ether olefine reaction;
Described protective gas feedway 2 and methanol tank 3 are communicated with described first reactor 18 respectively;
The delivery outlet of described first reactor 18 is communicated with described second reactor 19, gas chromatograph 24 respectively;
Described deionized water storage tank 4 is communicated with described second reactor 19;
The delivery outlet of described second reactor 19 is communicated with described gas chromatograph 24.Preferably, described gas chromatograph 24 has ten two-port valves, to realize the combination gas composition analyzing the first reactor 18 and the output of the second reactor 19 simultaneously.
The protective gas that described protective gas feedway 2 supplies be selected from helium, neon, argon gas, Krypton, xenon and nitrogen one or more, be preferably nitrogen.
According in an embodiment of the present utility model, described device also comprises air or oxygen feedway 1, and described air or oxygen feedway 1 is communicated with described first reactor 18
According in an embodiment of the present utility model, described device also comprises the first preheating mixer 17, described protective gas feedway 2, methanol tank 3 is communicated with described first reactor 18 via described first preheating mixer 17 respectively, that is, protective gas feedway 2, methanol tank 3 is communicated with the first preheating mixer 17 respectively, then, protective gas after preheating and methanol gas are passed in the first reactor 18 by the first preheating mixer 17 again, the protective gas that such protective gas feedway 2 provides and the methyl alcohol that methanol tank 3 provides can in this preheatings.
According in an embodiment of the present utility model, described device also comprises the second preheating mixer 21, and the delivery outlet of described first reactor 17, described deionized water storage tank 4 are communicated with described second reactor 19 via described second preheating mixer 21 respectively.That is, the reaction end gas that the first reactor 18 exports and the deionized water that provides of deionized water storage tank 4 are input in the second preheating mixer 21 by pipeline, then, are input in the second reactor 19 through the combination gas of preheating and/or water vapour again.
According in another embodiment of the present utility model, air or oxygen feedway 1 is communicated with the first reactor 18 via the first preheating mixer 17; And be communicated with described second reactor 19 via the second preheating mixer 21.The regeneration of the catalyzer in the first reactor 18 and/or the second reactor 19 can be realized by passing into air or oxygen in device.
According in another embodiment of the present utility model, described catalyst test apparatus also comprises knockout drum 31, and described knockout drum 31 is communicated with the delivery outlet of the first reactor 18, the delivery outlet of the second reactor 19 respectively.
According in another embodiment of the present utility model, described device also comprises for leaving that the material of described first reactor 18 with described second reactor 19 carries out heat exchange and condensation, that be connected successively heat interchanger 29, condenser 30, the reaction end gas that first reactor 18 or the second reactor 19 export, successively through described heat interchanger 29 and condenser 30, then enters described knockout drum 31.
According in another embodiment of the present utility model, the top of described knockout drum 31 can also be provided with counterbalance valve 32, controls with the system pressure realizing the first reactor 18.
According in another embodiment of the present utility model, described catalyst test apparatus also comprises tail gas processing mechanism, this tail gas processing mechanism is communicated with the delivery outlet of gas chromatograph 24, tail gas processing mechanism can comprise first tail gas bottle 25 and the second tail gas bottle 26 of connecting successively, preferably, splendid attire deionized water in described first tail gas bottle 25, splendid attire liquid soap or the liquid containing surfactant in described second tail gas bottle 26.
According in another embodiment of the present utility model, high-temperature filter can be provided with on the pipeline be communicated with the input port of described gas chromatograph 24.
According in an embodiment of the present utility model; DME catalyzer is loaded in described first reactor; its one end by the first preheating mixer 17 respectively with parallel with one another after air or oxygen feedway 1, protective gas feedway 2 and methanol tank 3 be connected; the other end of described first reactor 18 is communicated with a three-way switch valve, by the switching of this three-way switch valve, the reaction end gas that the first reactor 18 exports is divided into two-way.Gas chromatograph 24 is directly entered after the reaction end gas that described first reactor 18 exports can be passed through the first high-temperature filter 23 under the control of three-way switch valve, the online full constituent analysis of dimethyl ether catalyst reaction end gas is carried out in gas chromatograph 24, this tail gas also can be passed through stop valve and heat interchanger 29, condenser 30 and is communicated with knockout drum 31 and carries out gas-liquid separation, the counterbalance valve 32 that can also be arranged by knockout drum 31 top controls the system pressure of the first reactor 18, carries out the evaluation of DME catalyst activity.
Gas in the first described reactor 18 enters the second preheating mixer 21, second preheating mixer 21 and is communicated with deionized water storage tank 4 by pipeline under three-way switch valve controls.The unstripped gas of described second preheating mixer 21 is reaction end gas that water vapour and the first reactor export, the second reactor 19 is entered after the reaction end gas that water vapour and the first reactor 18 export mixes, MTP catalyzer is loaded in this second reactor 19, can simulate and evaluate MTP reaction, also water vapour can be inputted separately the second reactor 19, carry out MTP catalyzer decatize (i.e. catalyzer hydrothermal treatment consists) technological process.
Reaction end gas in the second described reactor 19 can enter gas chromatograph 24 and carry out the analysis of product full constituent under the control of three-way switch valve; Reaction end gas in the second described reactor 19 also under the control of three-way switch valve, through heat interchanger 29, condenser 30, finally can enter knockout drum 31 and carries out gas-liquid separation.
Described gas chromatograph 24 has ten two-port valves, can realize analyzing two-way gas composition simultaneously.The tail gas that gas chromatograph 24 exports passes into two interconnective tail gas bottles 25,26 successively.Tail gas can direct safety dumping after twice bubbling process of described tail gas bottle 25,26, and wherein load deionized water in the first tail gas bottle, in the second tail gas bottle, filling can make the solution of the dissolving of the high-carbon component in reaction end gas.Such as, this solution can be the solution containing negative ion or cationic surfactant, is preferably liquid soap.
The beneficial effects of the utility model are: adopt four gas circuits, double-reactor and band ten gas chromatography of two-port valve, experimentally object, by the control of three-way switch valve, realize catalyzer decatize (i.e. hydrothermal treatment consists), the evaluation of DME catalyst activity, simulate industrial MTP evaluating catalyst and catalyst regeneration carries out on same device.In addition, the tail gas bottle by tail gas being passed into the solution being loaded with deionized water and be easy to dissolving high-carbon component efficiently solves the problem of tail gas safe discharge.
Accompanying drawing explanation
Below, describe embodiment of the present utility model in detail by reference to the accompanying drawings, wherein:
Fig. 1 is the structural representation of a better embodiment according to catalyst test apparatus of the present utility model.
description of reference numerals:
1-air or oxygen feedway; 2-protective gas feedway; 3-methanol tank; 4-deionized water storage tank; 5-first stop valve; 6-second stop valve; 7-first pump; 8-second pump; The first-class gauge of 9-; 10-second gauge; 11-first retaining valve; 12-the 3rd stop valve; 13-second retaining valve; 14-the 4th stop valve; 15-the 3rd retaining valve; 16-the 4th retaining valve; 17-first preheating mixer; 18-first reactor; 19-second reactor; 20-first three-way switch valve; 21-second preheating mixer; 22-second three-way switch valve; 23-first high-temperature filter; 24-gas chromatography; 25-first tail gas bottle; 26-second tail gas bottle; 27-second high-temperature filter; 28-the 5th stop valve; 29-heat interchanger; 30-condenser; 31-knockout drum; 32-counterbalance valve; 33-the 6th stop valve; 34-the 7th stop valve.
Embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is described in detail further.Should be appreciated that drawings and Examples only for explaining the utility model, not for limiting the claimed scope of the utility model.
embodiment 1
Fig. 1 shows a better embodiment according to catalyst test apparatus of the present utility model.First preheating mixer 17 is communicated with air or oxygen feedway 1, protective gas feedway 2 and methanol tank 3 respectively by pipeline, the pipeline of connection air or oxygen feedway 1 is provided with the first stop valve 5, first-class gauge 9 and the 3rd retaining valve 15, so that the air or oxygen of monitor and forecast input; The pipeline of connective protection gas supply device 2 is provided with the second stop valve 6, second gauge 10 and the 4th retaining valve 16, so that the protective gas of monitor and forecast input; The pipeline of connection methanol tank 3 is provided with the first pump 7 and the first retaining valve 11, the pipeline between the first pump 7 and the first retaining valve 11 can arrange the branch line with the 3rd stop valve 12, for detecting the charging situations such as the flow of methanol solution.The delivery outlet of the first preheating mixer 17 is communicated with the input port of the first reactor 18 by pipeline, the delivery outlet of this first reactor 18 is communicated with the first three-way switch valve 20, two other interface of this first three-way switch valve 20 is communicated with an input port of the second preheating mixer 21 and gas chromatograph 24 respectively by pipeline, and the pipeline being wherein communicated with gas chromatograph 24 is also provided with the second high-temperature filter 27.Another input port of second preheating mixer 21 is communicated with deionized water storage tank 4 with the pipeline of the second retaining valve 13 by being provided with the second pump 8, between the second pump 8 and the second retaining valve 13, the branch line with the 4th stop valve 14 can also be set, to detect the charging situations such as the flow of methanol solution.The delivery outlet of this second preheating mixer 21 is communicated with by the input port of pipeline with the second reactor 19, the delivery outlet of this first reactor 19 is communicated with the second three-way switch valve 22, two other interface of this second three-way switch valve 22 is communicated with the input port of gas chromatograph 24 and condenser 30 respectively by pipeline, wherein, the pipeline of the input port of connection gas chromatograph 24 is provided with the first high-temperature filter 23, the pipeline of connection condenser 30 is provided with heat interchanger 29.The delivery outlet of gas chromatograph 24 is communicated with the first tail gas bottle 25 of splendid attire deionized water by pipeline, after the second tail gas bottle 26 of the solution of the surfactants such as splendid attire suds is connected on the first tail gas bottle 25.The output terminal of condenser 30 is communicated with knockout drum 31 by pipeline, this knockout drum 31 arranges the 6th stop valve 33 and the 7th stop valve 34 respectively on the pipeline be communicated with liquid phase delivery outlet with its gas phase delivery outlet, is also provided with counterbalance valve 32 at the top of this knockout drum 31.The pipeline be communicated with high gas chromatograph 24 by first three-way switch valve 20 arranges branch line, this branch line is communicated with the pipeline being communicated with heat interchanger 29, and this branch line is provided with the 5th stop valve 28, the gas that the first reactor 18 can be produced like this is input in burbling tank 31 via heat interchanger 29, condenser 30.
Be to be understood that, reactor in the present embodiment is fixed bed reactors, any fixed bed reactors being applicable to methanol to olefins reaction are all applicable to the utility model, include but not limited to the types such as axial heat-insulating fixed bed reactors, radial adiabatic formula fixed bed reactors, calandria type fixed bed reactor.
Be to be understood that, although only used three-way switch valve in the present embodiment to control the flow direction of reaction end gas, but, obviously also by arranging valve on each pipeline, or the valvular delivery outlet of multiple tool can be set on reactor to control the flow direction of reaction end gas.
Although should be appreciated that the selection as the best in the present embodiment is provided with preheating mixer separately, also reactant directly can be passed in reactor without preheating mixer, or, also directly can carry out preheating reactant by pipeline installing heat exchange mechanisms.
The using method of the catalyst test apparatus that the utility model provides is as follows:
Application service condition of the present utility model (including but not limited to following condition):
1) gas handling system is reacted: nitrogen flow is 0 ~ 1000mL/min, as carrier gas; Air or oxygen flow 0 ~ 1000mL/min, as catalyst regeneration gas;
2) methyl alcohol and deionized water feed system: adopt constant-flux pump, flow is 0 ~ 10ml/min;
3) reactive system: preheating mixer temperature: 0 ~ 350 DEG C; First temperature of reactor: 0 ~ 600 DEG C, the second temperature of reactor: 0 ~ 600 DEG C;
4) refrigerated separation, adds the reagent such as ethylene glycol in cold-producing medium, and temperature controls at-10 ~ 5 DEG C;
5) pipeline insulation: 160 ~ 200 DEG C.
embodiment 2
The present embodiment uses the catalyst test apparatus of embodiment 1 to carry out the evaluation of DME catalyst activity:
Filling DME catalyzer 3.0g in first reactor, the temperature setting the first preheating mixer 17 is 100 DEG C, setting insulation belt temperature 100 DEG C; Open advection first pump 7, setting flow 0.12ml/min, regulates catalyst in reactor bed temperature to be 320 DEG C; Regulate the first three-way switch valve 20, close the 5th stop valve 28, then the DME reaction end gas that the first reactor 18 produces directly enters chromatogram and carries out on-line analysis.Should be appreciated that and can pass into the carrier gas such as nitrogen in evaluation procedure, with the pressure in equilibrium catalyst evaluating apparatus.
embodiment 3
The present embodiment uses the catalyst test apparatus of embodiment 1 to carry out MTP catalyzer hydrothermal treatment consists:
Filling DME catalyzer 3.0g in first reactor 18, load MTP catalyzer 3.0g in the second reactor 19, the temperature setting the first preheating mixer 17 and the second preheating mixer 21 is respectively 100 DEG C and 110 DEG C, setting insulation belt temperature 100 DEG C; Open constant-flux pump (the second pump) 8 and pump into deionized water by the second pump 8, setting flow 0.12ml/min; Close the 3rd stop valve 12, deionized water is vaporized in the second preheating mixer 21; Meanwhile, open the second stop valve 6 and pass into nitrogen, it is 20ml/min that second gauge 10 sets nitrogen flow; Regulate the first three-way switch valve 20, after nitrogen is mixed with the deionized water of vaporization in the second preheating mixer 21, enter the second reactor 19; Regulate the second three-way switch valve 22, make the tail gas in the second reactor 19 enter knockout drum 31 and carry out gas-liquid separation and discharge.
embodiment 4
The present embodiment adopts the catalyst test apparatus of embodiment 1 to carry out MTP catalyzer Simulation evaluation:
MTP catalyzer hydrothermal treatment consists: filling DME catalyzer 3.0g in the first reactor 18, MTP catalyzer 3.0g is loaded in second reactor 19, the temperature setting the first preheating mixer 17 and the second preheating mixer 21 is respectively 200 DEG C and 300 DEG C, setting insulation belt temperature 180 DEG C;
Open the first pump 7 and pump into methyl alcohol by methanol tank 3, setting flow 0.12ml/min, methyl alcohol enters the first reactor 18 after the first preheating mixer 17 is vaporized, and its tail gas enters the second preheating mixer 21 by control first three-way switch valve 20;
While pumping into methyl alcohol, open the second pump 7, setting flow 0.15ml/min; Close the 4th stop valve 14, after the tail gas mixing of deionized water after the second preheating mixer 21 is vaporized in above-mentioned first reactor 18, enter the second reactor 19.When needing to measure activity data, then by adjustment second three-way switch valve 22, make tail gas after filtrator, enter gas chromatograph 24 and carry out on-line analysis, its tail gas carries out safety dumping after twice bubbling by the first tail gas tank 25 and the second tail gas tank 26, wherein, the second tail gas tank 26 loads appropriate liquid soap; When not needing to measure activity data, open heat interchanger 29 by adjustment second three-way switch valve 22, make tail gas after heat interchanger 29 and condenser 30, enter knockout drum 31 and carry out gas-liquid separation, if necessary, the gas in knockout drum and liquid can be carried out sampling analysis respectively.
During catalyst regeneration, close the first pump 7 (such as constant-flux pump) and the second pump 8 (such as constant-flux pump) stops charging, then the second stop valve 6 is first opened, after passing into nitrogen purging, open the first stop valve 5 again under the oxygen of variable concentrations, temperature programme is made charcoal, and carries out catalyst regeneration.
Although be described in detail embodiment of the present utility model and described, will be appreciated that, the utility model is not by the restriction of described embodiment.When not departing from the utility model spirit and scope, various improvement, modification and change can be made to the utility model, and these improve, modify and change all within scope of the present utility model.

Claims (9)

1. a catalyst test apparatus, comprising: protective gas feedway (2), methanol tank (3), deionized water storage tank (4), the first reactor (18) being filled with the catalyzer carrying out preparing dimethyl ether from methanol reaction, the second reactor (19) being filled with the catalyzer carrying out methyl alcohol and dimethyl ether olefine reaction, gas chromatograph (24); Wherein,
Described protective gas feedway (2) and methanol tank (3) are communicated with described first reactor (18) respectively;
The delivery outlet of described first reactor (18) is communicated with described second reactor (19), gas chromatograph (24) respectively;
Described deionized water storage tank (4) is communicated with described second reactor (19);
The delivery outlet of described second reactor (19) is communicated with described gas chromatograph (24).
2. device as claimed in claim 1, it is characterized in that, described device also comprises air or oxygen feedway (1), and described air or oxygen feedway (1) is communicated with described first reactor (18).
3. device as claimed in claim 2; it is characterized in that; described device also comprises the first preheating mixer (17), and described protective gas feedway (2), methanol tank (3) are communicated with described first reactor (18) via described first preheating mixer (17) respectively.
4. device as claimed in claim 3, it is characterized in that, described device also comprises the second preheating mixer (21), and delivery outlet, the described deionized water storage tank (4) of described first reactor (17) are communicated with described second reactor (19) via described second preheating mixer (21) respectively.
5. device as claimed in claim 4, it is characterized in that, described air or oxygen feedway is communicated with described first reactor (18) via described first preheating mixer (17); And be communicated with described second reactor (19) via described second preheating mixer (21).
6. the device according to any one of claim 1-5, it is characterized in that, described device also comprises knockout drum (31), and described knockout drum (31) is communicated with the delivery outlet of described first reactor (18), the delivery outlet of the second reactor (19) respectively.
7. device as claimed in claim 6, it is characterized in that, described device also comprises for leaving that the material of described first reactor (18) with described second reactor (19) carries out heat exchange and condensation, that be connected successively heat interchanger (29), condenser (30), and the material leaving described condenser (30) enters described knockout drum (31).
8. device as claimed in claim 7, it is characterized in that, described device also comprises the counterbalance valve (32) being arranged on described knockout drum (31) top.
9. the device according to any one of claim 1-5, it is characterized in that, described device also comprises tail gas processing mechanism, described tail gas processing mechanism is communicated with the delivery outlet of described gas chromatograph (24), described tail gas processing mechanism comprises the first tail gas bottle (25) and the second tail gas bottle (26) of connecting successively, splendid attire deionized water in described first tail gas bottle (25), in described second tail gas bottle (26), splendid attire contains the solution of surfactant.
CN201420542163.8U 2014-09-19 2014-09-19 A kind of catalyst test apparatus Expired - Fee Related CN204269615U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105116096A (en) * 2015-08-13 2015-12-02 中国石油化工股份有限公司 Hydrodeoxygenation catalyst evaluation device
CN106179131A (en) * 2016-06-27 2016-12-07 天津市鹏翔科技有限公司 Liquid feedstock high efficient mixed system
CN106770891A (en) * 2016-12-30 2017-05-31 神华集团有限责任公司 Catalyst test apparatus and evaluation method
CN107703251A (en) * 2017-11-22 2018-02-16 洛阳凯美胜石化设备有限公司 A kind of catalyst test apparatus and method
CN111974462A (en) * 2020-09-01 2020-11-24 大唐国际化工技术研究院有限公司 Method for recycling waste MTP catalyst

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105116096A (en) * 2015-08-13 2015-12-02 中国石油化工股份有限公司 Hydrodeoxygenation catalyst evaluation device
CN106179131A (en) * 2016-06-27 2016-12-07 天津市鹏翔科技有限公司 Liquid feedstock high efficient mixed system
CN106770891A (en) * 2016-12-30 2017-05-31 神华集团有限责任公司 Catalyst test apparatus and evaluation method
CN107703251A (en) * 2017-11-22 2018-02-16 洛阳凯美胜石化设备有限公司 A kind of catalyst test apparatus and method
CN111974462A (en) * 2020-09-01 2020-11-24 大唐国际化工技术研究院有限公司 Method for recycling waste MTP catalyst

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