CN102789250B - Automatic control system for pressurization micro reaction experiment device - Google Patents
Automatic control system for pressurization micro reaction experiment device Download PDFInfo
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- CN102789250B CN102789250B CN201210262019.4A CN201210262019A CN102789250B CN 102789250 B CN102789250 B CN 102789250B CN 201210262019 A CN201210262019 A CN 201210262019A CN 102789250 B CN102789250 B CN 102789250B
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- primary heater
- programmable logic
- logic controller
- state relay
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Abstract
The invention discloses an automatic control system for a pressurization micro reaction experiment device, which includes a mass flowmeter, a pressure transmitter, a temperature sensor, a six-way valve, as well as a solid state relay used for controlling the electrification/diselectrification of an electric heating furnace, an electromagnetic valve for switching valve position of the six-way valve, a monitoring computer, an RS485/232 converter, an analog quantity input unit and a programmable logic controller, wherein the analog quantity input unit is connected with the mass flowmeter, the pressure transmitter and the temperature sensor and used for acquiring flow, pressure and temperature data; and the programmable logic controller is connected with the solid state relay and used for controlling the solid state relay, and is also connected with the electromagnetic valve and used for controlling the valve position switching of the six-way valve. The automatic control system can be used for automatically completing most operation and data detection during the pressurization micro reaction experiment, brings convenience for experimental personnel for experiment operation and data logging, facilitates simplifying the experiment procedures and greatly improves the accuracy of experiment data.
Description
Technical field
The present invention relates to a kind of automation control system, more specifically, relate to a kind of automation control system for micro-anti-experimental provision that pressurizes.
Background technology
Pressurization micro-reaction equipment is widely used in a plurality of fields such as Chemical Manufacture, scientific research and teaching, its nucleus equipment is fixed-bed tube reactor, in course of reaction, need the situation of change of observing response temperature and reaction pressure at any time, reaction product adopts chromatogram analysis conventionally.Due to general grow (more than 24 hours) consuming time of this type of reaction, and require once to sample at set intervals and stratographic analysis, adopt manually-operated method to have very large drawback.
Summary of the invention
For above-mentioned prior art, the invention provides a kind of automation control system for micro-anti-experimental provision that pressurizes, this control system not only can be monitored temperature of reaction and reaction pressure in real time, and the six-way valve that can also automatically switch, carries out on-line chromatograph analysis, overcome manually-operated deficiency, be conducive to experimenter and hold more accurately extent of reaction, control course of reaction, simultaneously, also greatly reduce experimenter's labour intensity, saved a lot of time.
In order to solve the problems of the technologies described above, the technical scheme that the present invention is achieved for the automation control system of micro-anti-experimental provision of pressurizeing is: comprise the measurement assembly that is arranged on the micro-anti-experimental provision of pressurization, described measurement assembly is included in the mass flowmeter that is arranged on gas piping, is arranged on the pressure unit in primary heater inlet ductwork and is separately positioned on primary heater and the temperature sensor in reactor, the six-way valve being connected with described chromatograph; Also comprise the solid-state relay for controlling preheating and reactor electric furnace current switching, the solenoid valve switching for six-way valve valve position; Also comprise monitoring host computer, RS485/232 converter, analog input device and Programmable Logic Controller; Wherein, described analog input device is connected with described mass flowmeter, pressure unit and temperature sensor, for obtaining gas flow, enter the internal temperature of pressure, primary heater and the reactor of the mixed gas of primary heater; The make-and-break time that described Programmable Logic Controller is connected with described solid-state relay and controls solid-state relay electric current for realizing; Described Programmable Logic Controller is also connected with described solenoid valve, switches, thereby realize the online automatic control detecting of chromatograph for controlling the valve position of six-way valve.
The present invention, for the automation control method of micro-anti-experimental provision that pressurizes, comprises the steps:
By the man-machine dialog interface of monitoring main frame, set the step of technological parameter, comprise and set preheat temperature and temperature of reaction;
By Programmable Logic Controller, realize the step of the make-and-break time of controlling solid-state relay electric current;
By analog input device, obtain the step of the internal temperature of gas flow, the pressure that enters the mixed gas of primary heater, primary heater and reactor on gas piping;
By the break-make of Controlled by Programmable Controller solenoid valve, realize the automatic switchover of six-way valve between sampling and analyzing two states, thereby automatically control the online detection of chromatograph.
Compared with prior art, the invention has the beneficial effects as follows:
Can automatically complete the execution of the major part operation in the micro-anti-experimentation of pressurization and the detection of data thereof, facilitate experimenter's experimental implementation and data recording, be conducive to simplify experimental procedure, greatly improve the accuracy of experimental data.
Accompanying drawing explanation
Fig. 1 is the formation schematic diagram of the automation control system of the micro-anti-experimental provision of pressurization;
Fig. 2 realizes the method flow diagram that the micro-anti-experimental provision robotization of pressurization is controlled.
In figure:
1-gas bomb 2-reduction valve 3-exsiccator 4-filtrator
5-mass flowmeter 6-check (non-return) valve 7-mixer 8-primary heater
9-reactor 10-condenser 11-chromatograph 12-gas-liquid separator
13-counterbalance valve 14-six-way valve 15-soap film flowmeter 16-sample collecting device
17-charge pump 18-safety valve 19-pressure unit 20-solenoid valve
21-solid-state relay 22-Programmable Logic Controller 24-analog input device 25-RS485/232 converter
26-monitoring host computer
Embodiment
As shown in Figure 1, conventionally, micro-anti-experimental provision that pressurizes comprises three gas bombs 1, are furnished with accordingly three reduction valve 2, three exsiccators 3, three filtrators 4, three mass flowmeters 5, three check (non-return) valves 6, in addition, also comprise mixer 7, primary heater 8, reactor 9, condenser 10, chromatograph 11, gas-liquid separator 12, counterbalance valve 13, six-way valve 14, soap film flowmeter 15, sample collecting device 16, charge pump 17, safety valve 18 and the pressure unit 19 connecting by pipeline successively order.
In order to realize, the micro-anti-experimental provision of above-mentioned pressurization is carried out to robotization control, wherein, data for direct-detection experimental provision, or the measuring sensor group that the experimentation of device is controlled includes: be located at three mass flowmeters 5 on gas piping, be located at the pressure unit 19 in the inlet ductwork of primary heater 8, be located at two temperature sensor TCI101 in primary heater 8 and the temperature sensor TCI103 in TI102 and reactor 9, for controlling the solid-state relay 21 of primary heater 8 and reactor 9 electric furnace current switchings, and for controlling the solenoid valve 20 of chromatograph 11, also comprise monitoring host computer 26, RS485/232 converter 25, analog input device 24 and Programmable Logic Controller 22, described monitoring host computer 26 is for receiving experimenter's manual intervention to monitor and control simulation amount input unit 24 and Programmable Logic Controller 22, described RS485/232 converter 25 is in order to connecting analog amount follower 24, Programmable Logic Controller 24 and monitoring host computer 26, to realize the communication between them.Wherein, described analog input device 24 is connected with described mass flowmeter 5, pressure unit 19 and temperature sensor, for obtaining gas flow, enter the internal temperature of pressure, primary heater 8 and the reactor 9 of the mixed gas of primary heater 8; The make-and-break time that described Programmable Logic Controller (22) is connected with described solid-state relay 21 and controls solid-state relay 21 electric currents for realizing; Described Programmable Logic Controller 22 is also connected with described solenoid valve 20, switches, thereby realize the online automatic control detecting of chromatograph 11 for controlling the valve position of six-way valve 14.
Realizing the pressurize robotization of micro-anti-experimental provision of the present invention controls and mainly to comprise: by the man-machine dialog interface of monitoring main frame 26, set the step of technological parameter, comprise and set preheat temperature and temperature of reaction; By Programmable Logic Controller 22, realize the step of the make-and-break time of controlling solid-state relay 21 electric currents; By analog input device 24, obtain the step of the internal temperature of gas flow, the pressure that enters the mixed gas of primary heater 8, primary heater 8 and reactor 9 on gas piping; The break-make of controlling solenoid valve 20 by Programmable Logic Controller 22, realizes the automatic switchover of six-way valve 14 between sampling and analyzing two states, thereby automatically controls the online detection of chromatograph 11.
Embodiment:
The present invention pressurizes in the automation control system of micro-anti-experimental provision, the equipment of its core is a fixed-bed tube reactor, reaction product adopts chromatograph to carry out sampling analysis, by controlling the supporting solenoid valve six-way valve valve position that can automatically switch, realizing artificial On-line Control detects, monitoring host computer is wherein the personal computer based on industrial configuration software, industrial configuration software is the special software of a kind of data acquisition and process control, be used widely, its using method and concrete function are well-known, do not elaborate here.Generally speaking, deviser can be according to existing process chart, and utilization configuration software reaches Experiments of Automatic Control process and obtains the object of monitoring result.
As shown in Figure 1; the micro-anti-experimental provision of pressurization involved in the present invention; comprise three gas bombs 1; one of them is nitrogen; effect is to provide nitrogen protection and pipeline purges; another two is unstrpped gas, is furnished with accordingly three reduction valve 2, three exsiccators 3, three filtrators 4, three mass flowmeters 5, three check (non-return) valves 6.Two-way unstripped gas enters primary heater 8 after mixer 7 mixes, and liquid charging stock is also squeezed in primary heater 8 via charge pump 17, be preheating to together temperature required after, can enter in reactor 9 and react.After reaction finishes, product is first via condenser 10 condensations, then enters in gas-liquid separator 12 and carry out gas-liquid separation, and the liquid obtaining is directly collected in sample collecting device 16; The gas obtaining can enter in chromatograph 11 after via counterbalance valve 13, six-way valve 14 and carry out analyzing and testing, is furnished with the automatic switchover that solenoid valve 20 can be realized six-way valve 14 valve position herein.In addition, being also furnished with 7 tensimeters in whole system, is respectively PI101, PI102, PI103, PI104, PI105, PI106, PI107, for showing on the spot the line pressure of corresponding position; Also have: soap film flowmeter 15 is for the flow of assaying reaction tail gas; A pressure unit 19 is for measuring mixture pressure; Three temperature sensors, respectively TCI101, TI102 and TCI103, be used for measuring primary heater 8 and reactor 9 internal temperatures, in addition, in primary heater 8 and reactor 9, be equipped with electric furnace (not shown in FIG.), supporting solid-state relay 21 can be realized temperature sensor TCI101 in primary heater 8 and the automatic control of the temperature sensor TCI103 in reactor 9.
The pyrolysis gasoline hydrogenation reaction commonly used of take below utilizes the pressurize experimentation of automation control system of micro-anti-experimental provision of the present invention as example explanation.
First open monitoring host computer 26, enter and control interface.
Experimental implementation is as follows:
1) Preparatory work of experiment: testing fixture impermeability, guarantees completely airtight; Guarantee that charge pump 17 and chromatograph 11 setting parameters are complete errorless; Guarantee to pressurize between micro-anti-experimental provision and automation control system be connected accurate.
2) gas circuit N
2purge, guarantee the clean of gas piping; The first water such as liquid road and reactor 8 cleans and cleans with absolute ethyl alcohol, uses N
2after purging is dry, catalyzer is packed in reactor 8.
3) open the general supply on the micro-anti-experimental provision of pressurization, connect the power supply of chromatograph 11.
4) by the man-machine dialog interface of monitoring main frame 26, set technological parameter, comprise and set preheat temperature (as 120 ℃) and temperature of reaction (as 200 ℃), then Programmable Logic Controller 22 according to design temperature and transient temperature difference output control signal that electric current connects to solid-state relay 21, thereby make electric furnace start heating, temperature rises; When reaching while being raised to set temperature value, the signal that failures of current are controlled in Programmable Logic Controller 22 outputs is to solid-state relay 21, thereby makes electric furnace stop heating, and temperature no longer rises.
5) determine after on-stream pressure (as 2.5MPa), by controlling the given nitrogen flow value in interface (as 100ml/min), corresponding nitrogen pipeline mass flowmeter is opened, and starts pressurising, reaches after required pressure, stops logical nitrogen.In whole process, all can by analog input device 24, obtain the internal temperature of gas flow, the pressure that enters the mixed gas of primary heater 8, primary heater 8 and reactor 9 on gas piping, also can on monitoring host computer interface, show flow, pressure and all Temperature numerical simultaneously.6) temperature and pressure all reaches after reaction desirable value, opens hydrogen pipeline valve, by controlling the given hydrogen stream value in interface (as 50ml/min), guarantees that hydrogen enters in reactor 8 reposefully; Open charge pump 17, liquid charging stock (pyrolysis gasoline) is squeezed in reactor 8, react.
7) in course of reaction, can time recording hydrogen gas storage flow by controlling interface, preheat temperature, temperature of reaction and reaction pressure data; Check each parameter real-time curve variation tendency; Adjust hydrogen flowing quantity, preheat temperature and temperature of reaction setting value;
8) after a period of time, can by Programmable Logic Controller 22, control the break-make of solenoid valve 20, realize the automatic switchover of six-way valve 14 between sampling and analyzing two states, thereby automatically control the online detection of 11 pairs of reaction end gas of chromatograph.
9) after experiment finishes, first stop charge pump 17 chargings, close chromatograph 11 power supplys, by controlling interface, turn down preheat temperature and temperature of reaction, solid-state relay 21 is controlled electrical heating failure of current, starts cooling.When temperature drops to below 70 ℃, close the micro-anti-experimental provision general supply of pressurization, stop hydrogen feed.Pass into nitrogen blowing, open counterbalance valve 13, slowly the pressure in system is bled off.
The pressurize automation control system of micro-anti-experimental provision of the present invention, can automatically complete the execution of the major part operation in the micro-anti-experimentation of pressurization and the detection of data thereof, facilitate experimenter's experimental implementation and data recording, be conducive to simplify experimental procedure, greatly improved the accuracy of experimental data
Although in conjunction with figure, invention has been described above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; rather than restrictive; those of ordinary skill in the art is under enlightenment of the present invention; in the situation that not departing from aim of the present invention, can also make a lot of distortion, within these all belong to protection of the present invention.
Claims (2)
1. for an automation control system for micro-anti-experimental provision that pressurizes, it is characterized in that,
Comprise and be arranged on the measurement assembly of pressurization in micro-anti-experimental provision, described measurement assembly comprises the mass flowmeter (5) that is arranged on gas piping, is arranged on the pressure unit (19) in primary heater (8) inlet ductwork and is separately positioned on primary heater (8) and the temperature sensor in reactor (9), the six-way valve (14) being connected with chromatograph (11); Also comprise the solid-state relay (21) for controlling primary heater (8) and reactor (9) electric furnace current switching, the solenoid valve (20) switching for six-way valve (14) valve position;
Also comprise monitoring host computer (26), RS485/232 converter (25), analog input device (24) and Programmable Logic Controller (22); Wherein, described analog input device (24) is connected with described mass flowmeter (5), pressure unit (19) and temperature sensor, for obtaining gas flow, the enter primary heater internal temperature of pressure, primary heater (8) and reactor (9) of mixed gas of (8); The make-and-break time that described Programmable Logic Controller (22) is connected with described solid-state relay (21) and controls solid-state relay (21) electric current for realizing; Described Programmable Logic Controller (22) is also connected with described solenoid valve (20), switches, thereby realize the online automatic control detecting of chromatograph (11) for controlling the valve position of six-way valve (14).
2. an automation control method that utilizes the automation control system for micro-anti-experimental provision that pressurizes as claimed in claim 1, is characterized in that: comprise the steps:
By the man-machine dialog interface of monitoring main frame (26), set the step of technological parameter, comprise and set preheat temperature and temperature of reaction;
By Programmable Logic Controller (22), realize the step of the make-and-break time of controlling solid-state relay (21) electric current;
By analog input device (24), obtain the step of the internal temperature of gas flow, the pressure that enters the mixed gas of primary heater (8), primary heater (8) and reactor (9) on gas piping;
The break-make of controlling solenoid valve (20) by Programmable Logic Controller (22), realizes the automatic switchover of six-way valve (14) between sampling and analyzing two states, thereby automatically controls the online detection of chromatograph (11).
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| CN201210262019.4A CN102789250B (en) | 2012-07-26 | 2012-07-26 | Automatic control system for pressurization micro reaction experiment device |
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| CN201210262019.4A CN102789250B (en) | 2012-07-26 | 2012-07-26 | Automatic control system for pressurization micro reaction experiment device |
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| CN105912057B (en) * | 2016-06-27 | 2017-11-21 | 中国科学院上海技术物理研究所 | A kind of gas automatic control system and control method |
| CN107390752A (en) * | 2017-08-23 | 2017-11-24 | 南京扬子精细化工有限责任公司 | A kind of real-time inspection and control system |
| CN107562100B (en) * | 2017-08-25 | 2020-11-24 | 山东豪迈化工技术有限公司 | Flow and temperature control method and system of micro-reaction equipment |
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| DE10312698A1 (en) * | 2003-03-21 | 2004-09-30 | Bosch Rexroth Ag | Device for replacing the pressure and flow rate of a hydraulic pressure medium |
| CN101477018B (en) * | 2008-12-30 | 2011-04-20 | 中国科学院上海微系统与信息技术研究所 | Full-automatic hydrogen storage material performance tester and its testing method |
| CN102103363B (en) * | 2009-12-22 | 2012-12-26 | 上海吴泾化工有限公司 | Method and device for detecting and controlling acetoacetic ester continuous reaction system on line |
| CN102353750B (en) * | 2011-06-03 | 2014-05-14 | 中国石油天然气股份有限公司 | Crude oil low-temperature oxidation experimental device for light oil reservoir air-injection oil extraction |
| CN102393313B (en) * | 2011-10-18 | 2013-11-13 | 中国石油化工股份有限公司 | Temperature pressure tracking method of simulation device in petrifaction device in emergency discharge process |
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