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System of automatic temperature profile support in reactor

System of automatic temperature profile support in reactor
IPC classes for russian patent System of automatic temperature profile support in reactor (RU 2326424):
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Invention relates to the chemical industry, particularly to the automatic control systems and can be used for temperature support of the reaction mixture in chemical reactors. The system of automatic temperature profile support in the reactor with distributed constants in maleic anhydride production contains two control systems: cascade automatic control system (ACS) of coolant temperature control in the reactor and ACS of benzene-air mixture fed to the reactor where the correction signal is inleted according to reaction mixture temperature. The correction signal represents the sum of the signals about reaction mixture temperature in the measurement points positioned along the reactor height multiplied to the weight factor determined intuitively or from optimization problem solution. Then the correction signal is compared with assignment signal on the functional generator serving as algebraic adder. The invention allows to increase the temperature support accuracy in the reactor at maleic anhydride production.
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Invention relates to a method of producing maleic anhydride in a fluidised bed by oxidising material which contains C4 hydrocarbons with molecular oxygen or oxygen-containing gas in a reactor with a fluidised bed at reactor temperature 325-500°C in the presence of a catalyst capable of working in the fluidised bed, containing mixed oxides of vanadium and phosphorus, wherein the catalyst is prepared as follows: (a) preparation of a catalyst precursor containing mixed vanadium and phosphorus oxide; (b) packing the catalyst precursor; (c) crushing the catalyst precursor to particles whose average size is less than one micrometre in diametre; (d) moulding particles which are capable of working in the fluidised bed, with bulk density greater than or equal to 0.75 g/cm3 from the packed crushed catalyst precursor; and (e) annealing said particles in boiling conditions, where output of the maleic anhydride is increased by adding a compensating catalyst into the reactor with the fluidised bed, wherein said compensating catalyst contains alkyl ether of orthophosphoric acid of formula (RO)3P=O, where R is hydrogen or C1-C4 alkyl and at least one R is C1-C4 alkyl, where the compensating catalyst is prepared by saturating the catalyst obtained according to steps (a) to (e) with alkyl ether of orthophosphoric aid. The invention also discloses a method of improving operation of the mixed vanadium-phosphorus oxide catalyst for producing maleic anhydride from butane in a fluidised bed. The invention also relates to a catalyst capable of working in the fluidised bed, for producing maleic acid by oxidising material which contains C4 hydrocarbons.

FIELD: physics; operation.

SUBSTANCE: invention relates to the chemical industry, particularly to the automatic control systems and can be used for temperature support of the reaction mixture in chemical reactors. The system of automatic temperature profile support in the reactor with distributed constants in maleic anhydride production contains two control systems: cascade automatic control system (ACS) of coolant temperature control in the reactor and ACS of benzene-air mixture fed to the reactor where the correction signal is inleted according to reaction mixture temperature. The correction signal represents the sum of the signals about reaction mixture temperature in the measurement points positioned along the reactor height multiplied to the weight factor determined intuitively or from optimization problem solution. Then the correction signal is compared with assignment signal on the functional generator serving as algebraic adder. The invention allows to increase the temperature support accuracy in the reactor at maleic anhydride production.

EFFECT: increasing of the temperature support accuracy in the reactor.

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The invention relates to a system for automatic high-precision maintaining the temperature in the reactor at one or another of its coordinate (for example, the length or height), i.e. to the system automatic precision maintaining its temperature profile (fields). Such objects are called objects with distributed parameters (PPR).

While accurately maintaining the temperature profile as in statics and dynamics depends on the quality in the reactor product or intermediate, with attendant economic consequences.

Known reactors, in which the temperature of the reaction mixture is maintained at a predetermined value through a single billing system.

For example, in the semi-continuous reactor steps in the production of the PTS-60 (Voronezh-Tambov stabilizer) this is done by stabilizing the temperature in the reactor by the change of the flow of combusted natural gas in a furnace, in which the reactor, i.e. by changing the number of the heat carrier heating the reactor (see schedule production PTS-Novomoskovsk 60 JSC "Combine of organic synthesis" (COP)).

In a continuous reactor in the production of oxalic acid from ethylene glycol (see regulation for production of oxalic acid from the same plant - KOS) this is done by stabilizing the temperature in the reactor by changing the supply temperatures is enta shirt ("bath") reactor.

And in the first and second cases, the temperature in the reactor is measured only at one point. It is considered that due to the stirring reaction mixture temperature at all points of the reactor will be the same and equal to the temperature measured, i.e. the reactor in this case is the object with lumped parameters.

Similar schemes maintain the temperature in the reactor, i.e. its support by creating a single ASR can be found, for example, in the books:

1. Automatic control in the chemical industry. Ed. Agudama. - M.: Chemistry, 1987. S-132.

2. Sinski F. automatic control of chemical processes. - M.: Chemistry, 1974. S.

When small volumes of the reaction mixture at a sufficiently vigorous stirring the same parameters inside the reactor well run, that is, indeed, in these cases, the reactor can be mistaken for the object with lumped parameters and can be used to maintain the temperature inside the reactor single billing system.

When the requirements that provide the same parameters inside the reactor, the temperature values at a single regulation at different points of the reactor are different, which can lead to poor product quality. While trying to find such a point set and a temperature sensor in the reactor, which as much as possible to ensure the best management of the process at this point.

Insufficient quality of regulation, even if the condition on the concentration parameters of the reactor may, for example, due to the large inertsionnosti temperature measurement. In this case, to improve the quality of resorting to the creation of complex control systems, such as cascading billing system, by introducing an additional inner loop temperature control in the "Bane" of the reactor and introducing corrective signal for the temperature of the external circuit is the temperature inside the reactor, or combined systems, or systems with automatic change of settings (see, for example, the system of temperature regulation in the books:

1. Manusov E.B. Control and regulation of technological processes of paint and varnish industries. M.: Khimiya, 1977. P.50-57.

2. Automatic control in the chemical industry. Ed. Agudama. - M.: Chemistry, 1987. P.132-133).

At the same time, there are reactors with a marked rassredotochivshey parameters, for example, the height of the reactor. They should clearly be attributed to the objects with distributed parameters (PPR). Such objects include, for example, the reactor in the production of maleic anhydride (MA) JSC "Combine of organic synthesis" (KOS) whenmost, for which a new system of automatic maintenance of temperature profile.

Production MA at JSC Novomoskovsk KOS is based on a continuous vapor-phase catalytic oxidation of benzene with oxygen in the reactor (contact phone) on a stationary catalyst (see Moldovan BV, Kernos UD Maleic anhydride and maleic acid. L.: Chemistry, 1976. - 88 C.). At the exit of the reactor get maleina-air mixture (MVS) with a certain amount of maleic anhydride, which then allocate desublimate, distillation and subsequent crystallization.

The main reaction for the catalytic oxidation of benzene in MA is with great heat:

Schematic of the reactor and the existing regulatory systems shown in figure 1, showing: 1 - reactor (contact); 2 - steam generator; 3 - stirrer; 4, 5, respectively, flow regulators benzene and condensate; 6 - ratio controller benzene-air; 7 - temperature controller; 8 - meter temperature - thermocouple; 9 - temperature control devices salts (6 pieces); 10 - temperature control devices benzole-air mixture (10 PCs). Letter designations devices 4-10 taken in accordance with GOST 21.404-85 "denote the conditional instrumentation and automation in the schema.

For removal of heat of reaction in astronom space circulates the molten salt, the heat from which, in turn, is due to complete evaporation of the condensate in the steam generator 2, embedded in the Central part of the contact device and forming together the bath reactor.

The temperature in the bath varies from 280 to 325°and is not less than 3-6 points along the height of the contact apparatus. In the Central part of the apparatus, the flow of salts is directed upward, which is provided by a propeller stirrer 3, surrounded by the above-mentioned steam generator, and the external side from top to bottom due to gravity flow (see figure 1).

The top of the reactor 1 into the tube space, filled with a catalyst, served benzole-air mixture (BVS). Thus, the inner part of the reactor consists of a direct-flow shell-and-tube heat exchanger with 9142 tubes with a diameter of 30×1.8 mm and a length of 3500 mm In the catalyst bed height up to 3150 mm, the temperature of the reaction mixture varies from 200 to 480°C. the Last measured 10 thermocouples installed in a spiral at a depth of from 100 to 3000 mm In the operation position of thermocouple is adapted to better control the temperature distribution in the catalyst layer, and at least two thermocouples installed in the zone "hot spot".

The desired temperature profile, from the accurate maintenance of which depends on the product yield of the reaction is AI, provided by regulation of the ratio of benzene to air in BVS and temperature "baths" by changing the supply of condensate to the steam generator.

At the present time (see regulation for production of maleic anhydride KOS, Novomoskovsk, 1987) maintaining the temperature profile in the reactor are at a temperature of "hot spots", i.e. the point with the highest temperature of the reaction mixture at the height of the reactor, the component of order 480°C. In all other points along the height of the reactor temperature is controlled and its value by 10 points total order: 200°s at a height of 100 mm; 300° - under 265 mm; 400° - at 430 mm; 460° - at 600 mm; 400° - if 800 mm; 370° - if 1000 mm; 350° - at 1400 mm; 340° - at 1800 mm; 325° - at 2300 mm and 310° - at 2900 mm Thus, the "hot spot" is somewhere between the 3rd and 4th points of temperature measurement, and profile control is conducted on the 4-th point by building ASR ratio benzole-air mixture (BVS)fed to the reactor, the change in the amount of supplied air regulator 6 (FFC) (see figure 1) for a given "host" expense benzene (flow regulator benzene 4 (FC)) and by setting the ratio depending on the temperature of the "hot spots" (the dotted line to the regulator 6 (FFC) from the 4th point of the temperature profile MVS).

To maintain the profile also use the second system is to him - system cascade temperature control "baths". As the refrigerant used salt (in the reactor, they are loaded preset number (mass)), giving, in turn, the heat of reaction for the condensation of the steam generator, located at the centerline (in the middle) of the reactor, turning it into steam. The temperature of the salts according to the height of the reactor remains relatively constant (varying from 250°at the entrance to approximately 325°With output). This allows us to use to maintain the profile of salts cascading billing system 3 point temperature profile (only temperature profile of the refrigerant measured by the devices 9 in 6 points: 1-I am at a height of 100 mm; 2-I - 430 mm; 3-I - 800 mm; 4-I - 1400 mm; 5-I - 2300 mm and 6-I - 2910 mm), using information from thermocouple 8 controller 7 (TC) external circuit ACP. As the inner loop of the cascade billing temperature salt is used, the flow control condensate (see figure 1) regulation 5 (FC).

During operation it was discovered that when using these two standard systems of regulation of the quality management process (due to the complexity of chemical reactions and the complexity of the process) low and even worse than that which can be achieved through manual control by intuition apparatchiks. In addition, it supported manually ratio BVS status is made about 1:35÷ 1:40 (1 part of benzene, the rest is air), which is far from possible lower limit of 1:28 and below (up to the lower explosive limit of 1:24), which is the maximum content of MA (about 74%) in the MAM.

Thus, the application of the known systems described above, i.e. the creation of a single ASR ratio BVS with correction for the temperature of a hot spot in the reactor (prototype) together with cascading billing temperature of the refrigerant in the "bath" does not give the desired effect. Moreover, the low quality of the product (malaina-air mixture (MVS) of a given concentration and a given quality at the outlet of the reactor) results in failure of the single ASR temperature of the "hot spot" and hand the management of the process by maintaining the ratio of BVS (so the line job ratio controller 6 (FFC) at a temperature of 4-th point of the profile MVS shown in figure 1 by the dotted line) on the intuition of the operator.

The purpose of this invention is the creation of automatic control systems, providing the MAM of a given concentration and a given stability in automatic mode, i.e. systems that can provide a predetermined temperature profile along the height of the reactor as in statics and dynamics.

For this purpose it is offered instead of a single ASR ratio BVS-corrected temperature "hot spots" in re chore to enter into this single ASR ratio correction signal from the system optimal collect measurement data about the temperature profile along the height of the reactor.

The last signal is generated as follows (see figure 2). Figure 2 adopted the same conventions as in figure 1, with additional designations: 11, 12, 13 - functional signal Converter temperatures, meaning the conversion of which is explained in the inscription above the Converter. Full Kifunctional transducers 11 (10 PCs) shows that the signal of the temperature with the temperature control devices 10 (TI) damnaged on this ratio, and the symbol Σ - that the signals included in the corresponding Converter 12, 13, algebraically summed in them, giving the resulting signal I, the transducer 12 or ΔI - 13. The latter is a signal correction for the ratio controller 5 (FFC) BVS. In turn, it is formed on the Converter 13 (TY), acting as a comparison element, i.e. by comparing the signal I input from the Converter 12 (TY), with the reference signaland receiving the resulting signal. In turn, the I signal is a signal equal to:

where Tisignal proportional to the temperature value in the i-th measurement point of the temperature over the height of the reactor is given by the temperature control devices 10 (TI), ki- damnosus the th coefficient of the i-th transducer 11 (0≤ ki≤1), and their value is determined in such a way as to give the maximum value of the I signal, i.e. based on the solution of optimization problem:

where → read as "should", / - "subject", Ω - the constraints imposed on the solution of the problem (beyond the signal change Tithe limits of variation of the parameters of the transfer functions of Withe limits of variation of values of Kiand others). The resulting solution of this optimization problem, the weighting coefficients Toitake into account the dynamics of change in temperature, as the optimization criteria I values of Tiwill depend on the parameters of the transfer functions of Wiby respective temperature channels (i) depending on the control actions (U) the ratio of the BVS (UC) and its quantity (UQ), which is reflected in (1) showing the dependence of Tias a function ofandi.e. Ti(,). The solution of the optimization problem (1), we obtain the optimal values of the weighting coefficients Kithat is usually indicated by an asterisk, i.e. Toi*making a system for collecting measurement information about the temperature optimum.

In some cases, instead of finding wholesale the normal values For i* by solving the optimization problem (1) their values are chosen intuitive way, which makes the optimal system for collecting measurement information in intuitive, and the control system - in an intuitive control system (see the Posts SHE My brain. - M.: Sinteg, 2001. - 164 S.).

Note also that in the particular case of the reference signalmay be zero. Then as a corrective signal not used signal ΔI, and the signal I.

System temperature profile by introducing a correction in the ACP ratio BVS signal system optimal collect measurement data about the temperature profile of the reaction mixture at the height of the reactor shown in figure 2, was simulated on the computer by MATLAB in the SIMULINK system.

The simulation showed the stability of the temperature profile as in statics and in dynamics in comparison with its maintenance by the existing system - the system changes the ratio BVS temperature "hot spots" (see figure 1). This suggests the possibility of reducing the ratio of BVS towards the lower limit, i.e. to the possibility of maintaining it level 1:28 that, in turn, will significantly increase the content of the MA output MVS from the reactor.

Currently, the authors are engaged in the issue outside the rhenium of the proposed system on the reactor in the production of maleic anhydride KOS-based modules LOLICON-TM and multi-channel device MIP-S.

1. The system of automatic maintenance of temperature profile in the reactor with distributed parameters in the production of maleic anhydride by creating two control systems - cascade automatic regulation system (ASR) refrigerant temperature in the reactor and ASR ratio benzole-air mixture fed to the reactor, with the introduction of a correction signal according to the temperature of the reaction mixture, characterized in that as a correction signal using the signal generated as the sum of the signals of the temperature of the reaction mixture at the measurement points of the temperature over the height of the reactor, multiplied by weighting factors determined intuitively or as a result of solving optimization problems, and then compared with the reference signal on functional Converter that performs the function of the algebraic adder.

2. The system of automatic maintenance of temperature profile in the reactor with distributed parameters in the production of maleic anhydride according to claim 1, characterized in that in the particular case of the reference signal on the functional Converter may be zero.

 

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