CN101279976A - Monitoring method for hot-spot temperature of gas-phase catalytic oxidation reaction in preparation of pyromellitic acid anhydride - Google Patents
Monitoring method for hot-spot temperature of gas-phase catalytic oxidation reaction in preparation of pyromellitic acid anhydride Download PDFInfo
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- CN101279976A CN101279976A CNA2008100251678A CN200810025167A CN101279976A CN 101279976 A CN101279976 A CN 101279976A CN A2008100251678 A CNA2008100251678 A CN A2008100251678A CN 200810025167 A CN200810025167 A CN 200810025167A CN 101279976 A CN101279976 A CN 101279976A
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Abstract
Disclosed is a temperature monitoring method during the gas-phase catalytic oxidation process in the preparation of pyromellific anhydride, belonging to the technical field of preparation of pyromellific anhydride. Each of the catalyst beds in three reaction tubes inside a reactor is provided with a multi-junction displaying thermocouple; the temperature induction areas of the lower parts of the multi-junction displaying thermocouples not fixed at the same position in the catalyst bed inside the reaction tube; the temperature sensed by the temperature induction areas at the lower parts of the multi-junction displaying thermocouples is converted into electric signals which are then transferred to a signal converter; the signal converter converts the electric signals of the three multi-junction displaying thermocouples into temperature values which are then fed back to a control system and are displayed on the screen of the control system for an operator to adjust. With the method, the temperature during the reaction can be accurately and timely measured and can be fed back to the control system, thus realizing adjustment to the condition of the process in time and ensuring the yield and quality of the oxidized crude pyromellific anhydride.
Description
Technical field
The invention belongs to the preparing technical field of pyromellitic acid anhydride, be specifically related to the catalytic gas phase oxidation hot(test)-spot temperature monitoring method in a kind of pyromellitic acid anhydride preparation.
Background technology
China's production that pyromellitic acid anhydride (PMDA) is developed in the seventies starting from last century is united tackling key problem at late nineteen seventies by Chinese Petroleum Company's tissue, does not form scale production all the time owing to be mainly used in military project originally and cost an arm and a leg.Yet, from middle nineteen nineties in last century, because powder coating industry develop rapidly increases sharply the demand of PMDA, greatly reduce the cost of producing PMDA after isolating durol by the C+10 heavy aromatic hydrocarbon raw material especially, more promoted the continuous expansion of PMDA output.But domestic production still exists small scale (minimum about 30T/; The most about 350T/), situations such as maturation are lost in the control of simple and crude, the processing condition of production equipment.
Preparing in the PMDA process through the Fixed Bed Gas Phase catalyzed oxidation by durol, catalyzer is after selecting, the catalytic gas phase oxidation processing condition, be cooperatively interacting and in time harmonizing of air speed (L/hL), load (g/hL), temperature of molten salt, hot(test)-spot temperature, the variation that can accurately monitor oxidation focus and hot spot region is in time adjusted to guarantee processing condition in optimum regime, just can reach yield height, purpose that selectivity is good.Wherein promptly to monitor and control be the key factor of adjusting other processing condition in the monitoring of hot(test)-spot temperature.At present, the domestic durol Fixed Bed Gas Phase catalyzed oxidation processing condition overview for preparing pyromellitic acid anhydride is as follows:
Air speed (L/hL): adopt spinner-type flowmeter that air is measured, owing to there is not the large vol spinner-type flowmeter, thereby adopt usually four or six spinner-type flowmeter parallel connections, thisly tend to occur following two kinds of unfavorable factors in the numerous spinner-type flowmeter mode of implementing metering in parallel, the one, when adjusting one of them the time can have influence on then that other are several; The 2nd, can not regulate simultaneously a plurality of.In addition, because spinner-type flowmeter generally all is located at the scene, when finding that going to regulate air flow quantity again after focus changes lags behind.
Load (g/hL): durol normal temperature is solid down, just be molten into liquid state more than 80 ℃, conveying for durol, usually use toothed gear pump, surge pump or ram pump, but definitely carry out the insulation protection when requiring pump to be in running condition, if durol will solidify very soon under temporary stoppage or day cold cooling situation, pump is resulted in blockage, and, often need pump dismounting to handle or, have a strong impact on production and normally carry out with the steam fusing of heating in order to determine block part.
Hot-spot temperature of gas-phase catalytic oxidation reaction is very important to catalytic oxidation, and temperature crosses that low then oxidation is incomplete; Temperature is too high again can peroxidation.Have only the hot(test)-spot temperature of controlling optimum range, just can make yield height, the good product quality of oxidizing reaction, hot(test)-spot temperature is subjected to all multifactor influences in actual production.Listed as following table:
Usually adopt the hot(test)-spot temperature of three single-point thermocouple measurement reactors at present, three single-point thermopairs are placed in three different positionss of reactor respectively, in the vertical upper, middle and lower of reactor each one, the thermocouple location of middle part and lower position maintains static, and only moves up and down to determine the hot(test)-spot temperature position by top one.Because it can only be to carry out on the high temperature end socket of oxidation reactor at the scene that mobile galvanic couple is determined the operation of hot(test)-spot temperature position, therefore be easy to cause and burn, and the focus variation of temperature need show on the operation room panel board behind the mobile galvanic couple, is difficult to synchronously thereby cause Field adjustment and instrument to show; All can cause drift of oxidizing reaction focus and change under the situations such as the flow adjustment of air flow quantity and durol, the change of envrionment temperature and equipment operation are unusual, need redefine the hot(test)-spot temperature position, exactly because this loaded down with trivial details operating conditions, adjustment can not promptly and accurately cause gas phase catalytic oxidation reaction to be difficult to remain under the top condition and carry out.
By above-mentioned explanation as can be known, have only hot(test)-spot temperature carried out and accurately and timely effectively monitor and adjust, just can make gas phase catalytic oxidation reaction avoid causing oxidizing reaction not exclusively or over oxidation fully, so that influence yield, quality product.
Summary of the invention
Task of the present invention is the monitoring method that a kind of hot(test)-spot temperature position that can accurately and timely monitor gas-phase catalyst oxidation reactor will be provided and the hot(test)-spot temperature that is monitored be fed back to the hot-spot temperature of gas-phase catalytic oxidation reaction in the pyromellitic acid anhydride preparation of remote console.
Task of the present invention is finished like this, the monitoring method of the hot-spot temperature of gas-phase catalytic oxidation reaction in a kind of pyromellitic acid anhydride preparation, it is respectively to settle a multiple spot to show thermopair to three reaction tubes beds of the position distribution triangular in shape that is arranged in gas-phase catalyst oxidation reactor, and make each multiple spot show that the position of temperature sense zone in corresponding reaction tubes beds of thermopair lower end keeps different, and then show that by each multiple spot the temperature transition in the gas-phase catalyst oxidation reactor of being sensed in the temperature sense zone of thermopair lower end is that electric signal transmission is given signal converter, by signal converter three multiple spots are shown that electrical signal conversion that thermopairs obtain becomes temperature value to feed back to Controlling System and shows, adjusts the catalytic gas phase oxidation processing condition according to temperature value shown on the screen for the operator on the screen of Controlling System.
In a specific embodiment of the present invention, on distributing, described trilateral is meant on the cross section of gas-phase catalyst oxidation reactor position distribution with three summits of equilateral triangle.
In another specific embodiment of the present invention, described multiple spot shows that thermopair is meant that the temperature sense zone has five temperature sensitive member, spacing between five temperature sensitive member is 2cm, and wherein: first multiple spot shows that a temperature sensitive member of the top in five temperature sensitive member of thermopair is 15cm from the distance of reaction tubes beds upper surface; The distance of a temperature sensitive member an of temperature sensitive member of the top in five temperature sensitive member of second multiple spot demonstration thermopair the top in five temperature sensitive member of first multiple spot demonstration thermopair is 12cm; The distance of a temperature sensitive member an of temperature sensitive member of the top in five temperature sensitive member of the 3rd multiple spot demonstration thermopair the top in five temperature sensitive member of first multiple spot demonstration thermopair is 24cm.
In another specific embodiment of the present invention, described temperature sensitive member is a temperature sensor.
In another specific embodiment of the present invention, the temperature in the described gas-phase catalyst oxidation reactor is the hot(test)-spot temperature of gas-phase catalyst oxidation reactor.
Go back in the specific embodiment of the present invention, described hot(test)-spot temperature is the top temperature of the reaction zone of gas-phase catalyst oxidation reactor.
More of the present invention and in specific embodiment, described Controlling System is the distributed control system that includes computer, communication network, automatic control equipment at least based on microprocessor.
In of the present invention and then specific embodiment, described catalytic gas phase oxidation processing condition are meant by durol Fixed Bed Gas Phase catalyzed oxidation and prepare air speed, load, temperature of molten salt and hot(test)-spot temperature in the pyromellitic acid anhydride process.
Again more and in specific embodiment, described air speed is 4800～5200L/hL described load is 65～70g/hL of the present invention, and described temperature of molten salt is 380～390 ℃, and described hot(test)-spot temperature is 435～445 ℃.
Technical scheme disclosed in this invention is owing to adopted three multiple spots of distribution triangular in shape to show thermopair, thereby can be accurately, in time, effectively the temperature of reaction in the gas-phase catalyst oxidation reactor is predicted, and feed back to Controlling System, realization is guaranteed the yield and the quality product of the thick pyromellitic acid anhydride of oxygenated products to the timely adjustment of processing condition.
Description of drawings
Fig. 1 is an embodiment synoptic diagram of the inventive method.
Fig. 2 is another embodiment synoptic diagram of the inventive method.
Fig. 3 is the embodiment and the application examples synoptic diagram of the inventive method.
Embodiment
Embodiment 1:
See also Fig. 1 and in conjunction with Fig. 2, prepare in the pyromellitic acid anhydride process at the durol catalytic gas phase oxidation, on having, lower cover 1, position in 2 the gas-phase catalyst oxidation reactor 3 is in the beds 5 of three reaction tubess 4 that equilateral triangle distributes settles first respectively, second, the 3rd multiple spot shows thermopair 6,7,8, specifically be to realize installing by means of pagoda spring 10 by reaction tubes 4 bottom small porcelain rings 9, here the trilateral mentioned distributes and is meant that on the cross section of gas-phase catalyst oxidation reactor 3 position with three summits of equilateral triangle (referring to Fig. 2) is provided with three reaction tubess 4, because the position of reaction tubes 4 is determined, so, three first, second, the 3rd multiple spot shows thermopair 6,7,8 trilateral distributes and also determines thereupon.Three first, second, third multiple spots show that the position of thermopair 6,7,8 in the beds 5 of each reaction tubes 4 is different, and respectively have five temperature sensitive member 11.A temperature sensitive member 11 of the top in five temperature sensitive member 11 of first multiple spot demonstration thermopair 6 is 15cm from the distance of beds 5 upper surfaces of reaction tubes 4; Temperature sensitive member 11 in the top in five temperature sensitive member 11 of second multiple spot demonstration thermopair 7 is 12cm from the distance of a temperature sensitive member 11 of the top of first multiple spot demonstration thermopair 6; Temperature sensitive member 11 in the top in five temperature sensitive member 11 of the 3rd multiple spot demonstration thermopair 8 is 24cm from the distance of a temperature sensitive member 11 of the top of first multiple spot demonstration thermopair 6.
Hence one can see that, and first, second, third multiple spot shows that thermopair 6,7,8 has 15 temperature acquisition points, each other with 2cm separately.Temperature sensitive member 11 is a temperature sensor.By first, second, the 3rd multiple spot shows thermopair 6,7, temperature in the gas-phase catalyst oxidation reactor 3 of 11 perception of 15 temperature sensitive member on three temperature sense zones of 8 passes to signal converter 12, convert temperature value to numerary signal by signal converter 12 and feed back to the computer that includes based on microprocessor, communication network, the distributed control system of automatic control equipment (DCS), by operator according to hot(test)-spot temperature value shown on the DCS screen to catalytic gas phase oxidation processing condition such as air speed, load, temperature of molten salt is calibrated with the adjustment that hot(test)-spot temperature is done coadaptation mutually (cooperation).
Embodiment 2:
Ask for an interview Fig. 3 and settle first by embodiment 1, second, the 3rd multiple spot shows thermopair 6,7,8, first multiple spot shows thermopair 6, second multiple spot demonstration thermopair 7 and the 3rd multiple spot demonstration thermopair 8 influence value of totally 15 temperature inductors are the terminal display screen that temperature value is sent to the DCS Controlling System through signal converter 12 with electrical signal conversion, and temperature is respectively: 441.9 ℃, 446.3 ℃, 450.0 ℃, 448.5 ℃, 446.8 ℃, 435.4 ℃, 435.9 ℃, 433.2 ℃, 437.6 ℃, 438.6 ℃, 441.4 ℃, 419.5 ℃, 420.6 ℃, 411.3 ℃, 426.6 ℃.Wherein, the highest temperature of reaction is that the focus temperature is 450.0 ℃.Durol is introduced durol fusion jar 14 (volume 5m by raw material pipeline 13
3) after the fusion; Regulate valve position through variable valve 15, controlled oxidation reaction load enters vaporizer 17 after 16 meterings of adjusting built-in orificeplate transmitter through first more automatically at 70g/hL.Air 18 flow through air control valves 19 is by the road regulated valve position, the controlled oxidation reaction velocity is at 5000L/hL, after the second shell side heat exchange of flowing through second interchanger 21 and first interchanger 22 after automatically regulating 20 meterings of built-in orificeplate transmitter is successively promptly heated, enter vaporizer 17 again, and will enter vaporizer 17 and carry under one's arms through the durol of high-temperature evaporation and introduce the upper cover 1 of gas-phase catalyst oxidation reactors 3 through pipeline 23.Will the fused salt case in 24 with 25 heating of calrod group, controlled temperature is introduced the shell side of gas-phase catalyst oxidation reactors 3 at 385 ℃ fused salt through fused salt loop head pipeline 26, is drawn by the fused salt loop exit pipeline 27 of gas-phase catalyst oxidation reactor 3 to be back to fused salt case 24 again.Oxidation products is drawn through gas-phase catalyst oxidation reactor 3 outlet at bottom pipelines 28, is drawn by oxidation products pipeline 29 after the tube side heat exchange cooling of first interchanger 22 and second interchanger 21 again.Above-described first, second regulated built-in orificeplate transmitter 16, the 20 preferred transmitters of being produced and sold by Chinese Chongqing City Yokogawa river instrument company limited that adopt automatically.
When hot(test)-spot temperature in the anti-process of above-mentioned catalytic gas phase oxidation is the trend of liter and reaches 450.0 ℃, then can regulate according to following scheme:
Scheme one, the valve position of regulating air control valve 19 is increased to 5200L/hL with air speed from 5000L/hL, and it is effective that the hot(test)-spot temperature ascendant trend is slowed down explanation air speed increasing amount, otherwise a little increases air speed again, remains on till 440 ℃ until hot(test)-spot temperature;
Scheme two, keep air speed 5000L/hL and load 70g/hL constant, the heating that reduces or stop 25 pairs of fused salts of calrod group makes temperature of molten salt reduce by 0.5 ℃, and the hot(test)-spot temperature ascendant trend is slowed down the explanation temperature of molten salt and reduced effectively, remains on till 440 ℃ until hot(test)-spot temperature;
Scheme three keeps air speed 5000L/hL and 385 ℃ of temperature of molten salt constant, regulates the valve position of variable valve 15 the oxidizing reaction load is reduced to 65g/hL from 70g/hL.The hot(test)-spot temperature ascendant trend is slowed down the explanation load and is reduced effectively, otherwise reduces load slightly again, remains on till 440 ℃ until hot(test)-spot temperature.
Embodiment 3
Only first multiple spot is shown thermopair 6, second multiple spot show thermopair 7 and the 3rd multiple spot show thermopair 8 influence value of totally 15 temperature inductors be that the temperature that temperature value is sent to DCS Controlling System terminal display screen changes into through signal converter 12 with electrical signal conversion: 421.7 ℃, 426.0 ℃, 420.6 ℃, 411.3 ℃, 426.6 ℃, 420.3 ℃, 428.4 ℃, 405.2 ℃, 430.0 ℃, 422.8 ℃, 413.6 ℃, 411.3 ℃, 418.5 ℃, 421.4 ℃, 419.5 ℃, hot(test)-spot temperature changes 430.0 ℃ in the durol gas phase catalytic oxidation reaction control condition, all the other are with the description of embodiment 2, when focus is the decline gesture and reaches 430.0 ℃ in the anti-process of oxidation under this condition, can regulate according to following scheme:
Scheme one, the valve position of regulating air control valve 19 is reduced to 4800L/hL with air speed from 5000L/hL, and it is effective that the hot(test)-spot temperature downtrending slows down explanation air speed reduction, otherwise a little reduces air speed again, remains on till 440 ℃ until hot(test)-spot temperature;
Scheme two, keep air speed 5000L/hL and load 70g/hL constant, the heating of increase or 24 pairs of fused salts of unlatching calrod group raises 0.5 ℃ temperature of molten salt, and it is effective that the hot(test)-spot temperature downtrending slows down the increase of explanation temperature of molten salt, remains on till 440 ℃ until hot(test)-spot temperature;
Scheme three keeps air speed 5000L/hL and 385 ℃ of temperature of molten salt constant, and the valve position of regulating variable valve 15 is increased to 72g/hL with the oxidizing reaction load from 70g/hL.The hot(test)-spot temperature downtrending slows down the explanation load and increases effectively, otherwise increases load slightly again, remains on till 440 ℃ until hot(test)-spot temperature.All the other are with the description to embodiment 2.
The foregoing description 1-3, adopt three promptly first, second, third multiple spot show that the hot(test)-spot temperature of 6,7,8 pairs of durol gas phase catalytic oxidation reactions of thermopair monitors, can determine the hot(test)-spot temperature in the reactor accurately and timely, and then by reaction parameter be air speed, temperature of molten salt and load online dynamic adjustments, the calibration adjust the reaction hot(test)-spot temperature at optimum range, with high yield and the highly selective of guaranteeing to react.
Claims (9)
1, in the preparation of a kind of pyromellitic acid anhydride the monitoring method of hot-spot temperature of gas-phase catalytic oxidation reaction, it is characterized in that it is respectively to settle a multiple spot to show thermopair to three reaction tubes beds of the position distribution triangular in shape that is arranged in gas-phase catalyst oxidation reactor, and make each multiple spot show that the position of temperature sense zone in corresponding reaction tubes beds of thermopair lower end keeps different, and then show that by each multiple spot the temperature transition in the gas-phase catalyst oxidation reactor of being sensed in the temperature sense zone of thermopair lower end is that electric signal transmission is given signal converter, by signal converter three multiple spots are shown that electrical signal conversion that thermopairs obtain becomes temperature value to feed back to Controlling System and shows, adjusts the catalytic gas phase oxidation processing condition according to temperature value shown on the screen for the operator on the screen of Controlling System.
2, the monitoring method of the hot-spot temperature of gas-phase catalytic oxidation reaction in the pyromellitic acid anhydride according to claim 1 preparation is characterized in that described trilateral is meant on the cross section of gas-phase catalyst oxidation reactor the position distribution with three summits of equilateral triangle on distributing.
3, in the pyromellitic acid anhydride according to claim 1 preparation the monitoring method of hot-spot temperature of gas-phase catalytic oxidation reaction, it is characterized in that described multiple spot shows that thermopair is meant that the temperature sense zone has five temperature sensitive member, spacing between five temperature sensitive member is 2cm, and wherein: first multiple spot shows that a temperature sensitive member of the top in five temperature sensitive member of thermopair is 15cm from the distance of reaction tubes beds upper surface; The distance of a temperature sensitive member an of temperature sensitive member of the top in five temperature sensitive member of second multiple spot demonstration thermopair the top in five temperature sensitive member of first multiple spot demonstration thermopair is 12cm; The distance of a temperature sensitive member an of temperature sensitive member of the top in five temperature sensitive member of the 3rd multiple spot demonstration thermopair the top in five temperature sensitive member of first multiple spot demonstration thermopair is 24cm.
4, in the pyromellitic acid anhydride according to claim 3 preparation the monitoring method of hot-spot temperature of gas-phase catalytic oxidation reaction, it is characterized in that described temperature sensitive member is a temperature sensor.
5, in the pyromellitic acid anhydride according to claim 1 preparation the monitoring method of hot-spot temperature of gas-phase catalytic oxidation reaction, it is characterized in that the temperature in the described gas-phase catalyst oxidation reactor is the hot(test)-spot temperature of gas-phase catalyst oxidation reactor.
6, in the pyromellitic acid anhydride according to claim 5 preparation the monitoring method of hot-spot temperature of gas-phase catalytic oxidation reaction, it is characterized in that described hot(test)-spot temperature is the top temperature of the reaction zone of gas-phase catalyst oxidation reactor.
7, in the pyromellitic acid anhydride according to claim 1 preparation the monitoring method of hot-spot temperature of gas-phase catalytic oxidation reaction, it is characterized in that described Controlling System is the distributed control system that includes computer, communication network, automatic control equipment at least based on microprocessor.
8, in the pyromellitic acid anhydride according to claim 1 preparation the monitoring method of hot-spot temperature of gas-phase catalytic oxidation reaction, it is characterized in that described catalytic gas phase oxidation processing condition are meant by durol Fixed Bed Gas Phase catalyzed oxidation and prepare air speed, load, temperature of molten salt and hot(test)-spot temperature in the pyromellitic acid anhydride process.
9, in the pyromellitic acid anhydride according to claim 8 preparation the monitoring method of hot-spot temperature of gas-phase catalytic oxidation reaction, it is characterized in that described air speed is 4800～5200L/hL, described load is 65～70g/hL, described temperature of molten salt is 380～390 ℃, and described hot(test)-spot temperature is 435～445 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107930557A (en) * | 2017-12-05 | 2018-04-20 | 江南大学 | A kind of chemical process production capacity optimal control method and device |
| CN108698006A (en) * | 2016-03-03 | 2018-10-23 | 埃克森美孚研究工程公司 | The abnormal temperature of fixed bed reactors detects |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101324788B (en) * | 2008-07-16 | 2010-06-23 | 大连理工大学 | Method for supervising programmed temperature configuration of catalyze micro-reaction apparatus |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108698006A (en) * | 2016-03-03 | 2018-10-23 | 埃克森美孚研究工程公司 | The abnormal temperature of fixed bed reactors detects |
| CN107930557A (en) * | 2017-12-05 | 2018-04-20 | 江南大学 | A kind of chemical process production capacity optimal control method and device |
| CN107930557B (en) * | 2017-12-05 | 2020-05-19 | 江南大学 | Chemical process capacity optimization control method and device |
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