CN105561886A - Experiment system for studying gas-solid reaction kinetics - Google Patents

Experiment system for studying gas-solid reaction kinetics Download PDF

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Publication number
CN105561886A
CN105561886A CN201610038538.0A CN201610038538A CN105561886A CN 105561886 A CN105561886 A CN 105561886A CN 201610038538 A CN201610038538 A CN 201610038538A CN 105561886 A CN105561886 A CN 105561886A
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gas
temperature
solid reaction
studying
solid
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CN105561886B (en
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吴龙
周怀祖
孙永才
刘斌
刘红艳
周琦
周大鹏
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Shanghai Yao Xing Management Of Investment Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796Details of the reactor or of the particulate material
    • B01J2208/00893Feeding means for the reactants

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The invention provides an experiment system for studying gas-solid reaction kinetics. The system comprises a gas-solid reacting unit, a steam generating unit, a reacting gas supply unit and a product gas processing unit. The gas-solid reacting unit comprises a gas-solid reactor and a temperature closed-loop control device. A steam generator of the steam generating unit is connected with a gas inlet. The reacting gas supply unit comprises a first gas steel cylinder set, a second gas steel cylinder set, an electromagnetic valve set, a delay controller and a gas preheater. The first gas steel cylinder set and the second gas steel cylinder set are connected with the electromagnetic valve set which controls the transient switch of reacting gas through the delay controller. The gas preheater is connected with the gas inlet. The product gas processing unit comprises a first tar trap and a second tar trap which are connected with each other. The first tar trap is connected with a product gas outlet. The system has the advantages of being precise in temperature control, high in heating speed, precise in reacting gas control, capable of easily separating gas products and the like.

Description

For studying the experimental system of gas-solid reaction kinetic
Technical field
The invention belongs to field of chemical engineering, specifically, the present invention relates to the experimental system of research gas-solid reaction kinetic.
Background technology
The gas solid reactor experiment porch of traditional experiment room scale is due to shortcomings such as its firing rate are low, temperature control accuracy is poor, reaction atmosphere condition is single, product is not easily separated, truly can not reflect the reaction condition in commercial plant, cause the narrow and experiment condition of experimental result range of application not representative etc.Therefore, a kind of experimental system being suitable for studying gas-solid reaction kinetic is urgently developed.
Summary of the invention
The present invention is intended to solve one of technical problem in correlation technique at least to a certain extent.For this reason, one object of the present invention is to propose a kind of experimental system for studying gas-solid reaction kinetic.This experimental system has the features such as temperature controls accurately, firing rate is fast, reaction gas controls accurately, gaseous product is easily separated.
According to an aspect of the present invention, the present invention proposes a kind of experimental system for studying gas-solid reaction kinetic, comprising:
Gas-solid reaction unit, described gas-solid reaction unit comprises gas solid reactor and temperature closed-loop control device, described gas solid reactor has housing, reaction chamber is limited in described housing, described housing has gas feed and product gas outlet, there is in described reaction chamber the sample stage being suitable for gas-solid reaction, it is outer and be connected with described sample stage with electrode by compensation lead of thermocouple, to be suitable for monitoring the temperature of described sample stage and regulating and controlling that described temperature closed-loop control device is arranged on described housing;
Steam generating unit, described steam generating unit comprises the steam generator, reciprocating pump and the aqua storage tank that are connected successively, and described steam generator is connected with described gas feed;
Reaction gas feed unit, described reaction gas feed unit comprises the first gas bomb group, second gas bomb group, magnetic valve group, delay controller and gas preheater, described first gas bomb group is connected with described magnetic valve group respectively with the second gas bomb group, described magnetic valve group is connected with described gas preheater with described delay controller respectively, described gas preheater is connected with described gas feed, described magnetic valve group and delay controller are suitable for switching instantaneously the first gas bomb group and the second gas bomb group, to switch the question response gas passed in described gas solid reactor, and
Product gas processing unit, described product gas processing unit comprises the first connected tar trap and the second tar trap, and described first tar trap exports with described product gas and is connected.
Thus, for the experimental system studying gas-solid reaction kinetic, there is the features such as temperature controls accurately, firing rate is fast, reaction gas controls accurately, gaseous product is easily separated by what adopt the above embodiment of the present invention.Adopt this system effectively to study the catalytic reaction etc. of the Chemical Kinetics of solid material, the gas absorption effect of adsorbent and solid catalyst, experimental result repeatability is high, representative strong.
In addition, the experimental system for studying gas-solid reaction kinetic according to the above embodiment of the present invention can also have following additional technical characteristic:
According to some embodiments of the present invention, described temperature closed-loop control device has electrode and temperature signal collection thermocouple wire, and described electrode is connected with described sample stage respectively with temperature signal collection thermocouple wire.
According to some embodiments of the present invention, described temperature scaling factor utensil has infrared temperature sensor, and described infrared temperature sensor is connected with described sample stage.
According to some embodiments of the present invention, described temperature closed-loop control device has centralised temperature controller, described centralised temperature controller is suitable for the heating rate of sample stage described in the temperature adjusting that monitors according to described temperature signal collection thermocouple wire or infrared temperature sensor, to control operating temperature in real time.
According to some embodiments of the present invention, described sample stage has cooling water jecket.
According to some embodiments of the present invention, the perisporium of described housing is formed by quartz or pressure tight metal, and the bottom surface of described housing is formed by metal.
According to some embodiments of the present invention, described first tar trap adopts sleeve structure, and filling has stainless steel cloth in the inner layer pipe in described sleeve pipe, the inner layer pipe in described sleeve pipe and be cooling-water duct between outer layer pipe;
Described second tar trap adopts water-bath structure, and the pipeline of filling stainless steel cloth is placed in sea water bath, has dry ice and/or liquid nitrogen in described sea water bath;
Counterbalance valve is provided with between described first tar trap and the second tar trap.Gas solid reactor outlet pressure is down to normal pressure by counterbalance valve.
According to some embodiments of the present invention, described first gas bomb group comprises multiple first gas bomb, described second gas bomb group comprises multiple second gas bomb, and the exit of described first gas bomb and the second gas bomb is provided with mass flow controller.
According to some embodiments of the present invention, the experimental system of above-described embodiment comprises the spinner flowmeter, flow totalizer, online detector and the torch that are connected successively further, described spinner flowmeter is connected with described second tar trap, and described battery valve group is connected with described torch.
According to some embodiments of the present invention, between described first tar trap and described counterbalance valve and between described online detector and described torch, be provided with safety-valve.
Accompanying drawing explanation
Fig. 1 is according to an embodiment of the invention for studying the structural representation of the experimental system of gas-solid reaction kinetic.
Detailed description of the invention
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not limitation of the present invention be interpreted as.
According to an aspect of the present invention, the present invention proposes a kind of experimental system for studying gas-solid reaction kinetic.The experimental system for studying gas-solid reaction kinetic of the specific embodiment of the invention is described in detail below with reference to Fig. 1.
Comprising for the experimental system studying gas-solid reaction kinetic according to the specific embodiment of the invention: gas-solid reaction unit 100, steam generating unit 200, reaction gas feed unit 300 and product gas processing unit 400.
According to a particular embodiment of the invention, gas-solid reaction unit 100 comprises gas solid reactor 110 and temperature closed-loop control device 120, described gas solid reactor 110 has housing 111, reaction chamber is limited in described housing, described housing 111 has gas feed 112 and product gas outlet 113, there is in described reaction chamber the sample stage 114 being suitable for gas-solid reaction, it is outer and be connected with described sample stage 114, to be suitable for monitoring the temperature of described sample stage 114 and regulating and controlling that described temperature closed-loop control device 120 is arranged on described housing 111.
Thus, gas solid reactor 110 is suitable for gas and solid reactant reaction.Temperature closed-loop control device 120 is suitable for monitoring the reaction temperature of gas solid reactor 110 and regulating and controlling, and particularly, can carry out real-time controlling and adjustment, and then effectively can improve the accuracy of experiment to the heating rate of sample stage and temperature.
According to a particular embodiment of the invention, temperature closed-loop control device 120 has electrode and temperature signal collection thermocouple wire, and described electrode is connected with described sample stage with temperature signal collection thermocouple wire.Temperature closed-loop control device 120 accurately can obtain the temperature of sample stage by temperature signal collection thermocouple wire thus, to regulate its temperature further.According to a particular embodiment of the invention, the electrode of temperature closed-loop control device 120 and temperature signal collection thermocouple wire, all through the housing of gas solid reactor, enter reaction chamber and are connected with sample stage.
According to another specific embodiment of the present invention, temperature scaling factor device 120 has infrared temperature sensor, and described infrared temperature sensor is connected with described sample stage.Temperature scaling factor device 120 accurately can obtain the temperature of sample stage by infrared temperature sensor thus, to regulate its temperature further.
According to a particular embodiment of the invention, described temperature closed-loop control device 120 has centralised temperature controller 121, described centralised temperature controller is suitable for the heating rate of sample stage described in the temperature adjusting that monitors according to described temperature signal collection thermocouple wire or infrared temperature sensor, to control operating temperature in real time.
According to a particular embodiment of the invention, sample stage 114 has cooling water jecket.Can lower the temperature to sample stage thus, to prevent sample stage in experimentation overheated, and then improve intellectuality and the applicability of experimental system, reach required experiment condition better, improve the representativeness of experimental data.Therefore, above-mentioned sample stage 114 can realize the controlled of heating rate and operating temperature, improves the accuracy of reaction condition, improves the reliability of experimental data.
According to a particular embodiment of the invention, by gas flowing, reacting gas product is departed from sample stage in time in reaction chamber, avoid the secondary response again of gaseous products and solid sample.
According to a particular embodiment of the invention, the perisporium of the housing 111 of gas solid reactor 110 can be formed by quartz or pressure tight metal, and the bottom surface of housing 111 is formed by metal.According to concrete example of the present invention, the perisporium of described housing and adopt O to enclose between upper bottom surface and bottom surface or the sealing means of embedding, can maintain the closed environment in reaction chamber thus better.
According to a particular embodiment of the invention, steam generating unit 200 comprises the steam generator 210, reciprocating pump 220 and the aqua storage tank 230 that are connected successively, and described steam generator 210 is connected with described gas feed 122.Thus by adopting above-mentioned steam generating unit 200 can provide steam to gas solid reactor 110.
According to a particular embodiment of the invention, reaction gas feed unit 300 comprises the first gas bomb group 310, second gas bomb group 320, magnetic valve group 330, delay controller 340 and gas preheater 350, described first gas bomb group 310 is connected with described magnetic valve group 330 respectively with the second gas bomb group 320, described magnetic valve group 330 is connected with described gas preheater 350 with described delay controller 340 respectively, and described gas preheater 350 is connected with described gas feed 122.
According to a particular embodiment of the invention, magnetic valve group 330 and delay controller 340 are suitable for switching instantaneously, to switch the question response gas passed in gas solid reactor 110 the first gas bomb group 310 and the second gas bomb group 320.According to concrete example of the present invention, when reaction needed in gas solid reactor 110 changes reaction gas, above-mentioned magnetic valve group 330 and delay controller 340 can be utilized to realize." switch instantaneously " and specifically refer to complete switching in 0.02 second, the fastest switch speed can be 0.005 second.Namely magnetic valve group 330 and delay controller 340 can realize the quick switching between the first gas bomb group 310 and the second gas bomb group 320 at 0.005 second, and then the moment switching of gas with various in experimentation is accurately controlled, and then significantly improve the flexibility of system and the accuracy of experiment.
According to a particular embodiment of the invention, gas preheater 350 is suitable for heating entering question response gas in gas solid reactor 110, and then can effectively control the initial temperature of the question response gas entered in reaction chamber in advance; In addition when containing steam in question response gas, steam condensation in reaction chamber can be prevented by opening gas preheater 350, affecting reaction condition.
According to a particular embodiment of the invention, described first gas bomb group 310 comprises multiple first gas bomb, described second gas bomb group 320 comprises multiple second gas bomb, and described first gas bomb and the second gas bomb exit are provided with mass flow controller 330.The contiguous gas outlet place of each gas bomb is provided with mass flow controller 360 thus, and then accurately can control the flow entering multiple reaction gas in gas solid reactor 110.
According to a particular embodiment of the invention, above-mentioned multiple gas bomb is suitable for splendid attire hydrogen, carbon dioxide, carbon monoxide, steam, oxygen, nitrogen, hydrocarbon, sulfur-containing compound, nitrogen-containing compound and inert gas etc.And then provide required reaction gas for the reaction in gas solid reactor 110.
Thus, by adopting above-mentioned reacting gas feed unit 300, can realize the accurate control to reacting gas in experimentation, the moment comprising differential responses gas in flow, component, temperature and experimentation switches.
According to a particular embodiment of the invention, product gas processing unit 400 comprises the first connected tar trap 410 and the second tar trap 420, and described first tar trap 410 exports 123 with described product gas and is connected.
Thus, the condensation utilizing above-mentioned first tar trap 410 effectively can realize higher boiling gaseous products (relative molecular weight is greater than 400Da) be separated; In utilizing the second tar trap 420 to realize low boiling gaseous products (relative molecular weight is less than 400Da and is greater than 78Da) condensation be separated.
According to a particular embodiment of the invention, described first tar trap 410 adopts sleeve structure, and filling has stainless steel cloth in the inner layer pipe in described sleeve pipe, the inner layer pipe in described sleeve pipe and be cooling-water duct between outer layer pipe; Described second tar trap 420 adopts water-bath structure, and the pipeline of filling stainless steel cloth is placed in sea water bath, has dry ice and/or liquid nitrogen in described sea water bath; Counterbalance valve 430 is provided with between described first tar trap 410 and the second tar trap 420.Gas solid reactor 110 outlet pressure is down to normal pressure by counterbalance valve 430.
According to a particular embodiment of the invention, above-described embodiment comprise for the experimental system studying gas-solid reaction kinetic the spinner flowmeter 500, flow totalizer 600, online detector 700 and the torch 800 that are connected successively further, described spinner flowmeter 500 is connected with described second tar trap 420.
Thus, by arrange spinner flowmeter 500, flow totalizer 600, online detector 700 can and bond quality flow controller 360 can effectively accurately control the flow of the various gases entered in reaction chamber.Finally be connected with torch 800, by the product gas that produces in experimentation before discharge air, can be processed by flare system, avoid contaminated environment.
According to a particular embodiment of the invention, described battery valve group 330 is connected with described torch 800.Residual gas in pipeline or pipeline can be omitted gas before discharge air thus, be processed by flare system, avoid contaminated environment.
According to a particular embodiment of the invention, safety-valve 900 is provided with between described first tar trap and described counterbalance valve.According to a particular embodiment of the invention, safety-valve 900 is provided with between described online detector and described torch.The security of system can be improved thus further.
In describing the invention, it will be appreciated that, term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", " counterclockwise ", " axis ", " radial direction ", orientation or the position relationship of the instruction such as " circumference " are based on orientation shown in the drawings or position relationship, only the present invention for convenience of description and simplified characterization, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore limitation of the present invention can not be interpreted as.
In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise one or more these features.In describing the invention, the implication of " multiple " is two or more, unless otherwise expressly limited specifically.
In the present invention, unless otherwise clearly defined and limited, the term such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or integral; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals or the interaction relationship of two elements.For the ordinary skill in the art, above-mentioned term concrete meaning in the present invention can be understood as the case may be.
In the present invention, unless otherwise clearly defined and limited, fisrt feature second feature " on " or D score can be that the first and second features directly contact, or the first and second features are by intermediary mediate contact.And, fisrt feature second feature " on ", " top " and " above " but fisrt feature directly over second feature or oblique upper, or only represent that fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " below " and " below " can be fisrt feature immediately below second feature or tiltedly below, or only represent that fisrt feature level height is less than second feature.
In the description of this description, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, to the schematic representation of above-mentioned term need not for be identical embodiment or example.And the specific features of description, structure, material or feature can combine in one or more embodiment in office or example in an appropriate manner.In addition, when not conflicting, the feature of the different embodiment described in this description or example and different embodiment or example can carry out combining and combining by those skilled in the art.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, and those of ordinary skill in the art can change above-described embodiment within the scope of the invention, revises, replace and modification.

Claims (10)

1. for studying an experimental system for gas-solid reaction kinetic, it is characterized in that, comprising:
Gas-solid reaction unit, described gas-solid reaction unit comprises gas solid reactor and temperature closed-loop control device, described gas solid reactor has housing, reaction chamber is limited in described housing, described housing has gas feed and product gas outlet, have the sample stage being suitable for gas-solid reaction in described reaction chamber, it is outer and be connected with described sample stage, to be suitable for monitoring the temperature of described sample stage and regulating and controlling that described temperature closed-loop control device is arranged on described housing;
Steam generating unit, described steam generating unit comprises the steam generator, reciprocating pump and the aqua storage tank that are connected successively, and described steam generator is connected with described gas feed;
Reaction gas feed unit, described reaction gas feed unit comprises the first gas bomb group, second gas bomb group, magnetic valve group, delay controller and gas preheater, described first gas bomb group is connected with described magnetic valve group respectively with the second gas bomb group, described magnetic valve group is connected with described gas preheater with described delay controller respectively, described gas preheater is connected with described gas feed, described magnetic valve group and delay controller are suitable for switching instantaneously the first gas bomb group and the second gas bomb group, to switch the question response gas passed in described gas solid reactor, and
Product gas processing unit, described product gas processing unit comprises the first connected tar trap and the second tar trap, and described first tar trap exports with described product gas and is connected.
2. the experimental system for studying gas-solid reaction kinetic according to claim 1, it is characterized in that, described temperature closed-loop control device has electrode and temperature signal collection thermocouple wire, and described electrode is connected with described sample stage respectively with temperature signal collection thermocouple wire.
3. the experimental system for studying gas-solid reaction kinetic according to claim 1, is characterized in that, described temperature scaling factor utensil has infrared temperature sensor, monitors described sample stage temperature by described infrared temperature sensor.
4. the experimental system for studying gas-solid reaction kinetic according to Claims 2 or 3, it is characterized in that, described temperature closed-loop control device has centralised temperature controller, described centralised temperature controller is suitable for the heating rate of sample stage described in the temperature adjusting that monitors according to described temperature signal collection thermocouple wire or infrared temperature sensor, to control operating temperature in real time.
5. the experimental system for studying gas-solid reaction kinetic according to claim 1, is characterized in that, described sample stage has cooling water jecket.
6. the experimental system for studying gas-solid reaction kinetic according to claim 1, is characterized in that, the perisporium of described housing is formed by quartz or pressure tight metal, and the bottom surface of described housing is formed by metal.
7. the experimental system for studying gas-solid reaction kinetic according to claim 1, it is characterized in that, described first tar trap adopts sleeve structure, filling has stainless steel cloth in inner layer pipe in described sleeve pipe, the inner layer pipe in described sleeve pipe and be cooling-water duct between outer layer pipe;
Described second tar trap adopts water-bath structure, and the pipeline of filling stainless steel cloth is placed in sea water bath, has dry ice and/or liquid nitrogen in described sea water bath;
Counterbalance valve is provided with between described first tar trap and the second tar trap.
8. the experimental system for studying gas-solid reaction kinetic according to claim 1, it is characterized in that, described first gas bomb group comprises multiple first gas bomb, described second gas bomb group comprises multiple second gas bomb, and the exit of described first gas bomb and the second gas bomb is provided with mass flow controller.
9. the experimental system for studying gas-solid reaction kinetic according to claim 1, it is characterized in that, comprise the spinner flowmeter, flow totalizer, online detector and the torch that are connected successively further, described spinner flowmeter is connected with described second tar trap, and described battery valve group is connected with described torch.
10. the experimental system for studying gas-solid reaction kinetic according to claim 1, is characterized in that, is provided with safety-valve between described first tar trap and described counterbalance valve and between described online detector and described torch.
CN201610038538.0A 2016-01-20 2016-01-20 For studying the experimental system of gas-solid reaction kinetic Active CN105561886B (en)

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