Method of regulating process streams during production of cyclohexane

FIELD: physics; control.

SUBSTANCE: invention relates to methods and devices for regulating processes and can be used in chemical industry during production of cyclohexane. The method of regulating streams in the production of cyclohexane comprises heat exchangers, condensers, hydrogen and benzene hydrogenation reactors, an end product cooler, a separator with benzene and hydrogen flow valves and sensors, temperature sensors in the hydrogenation reactors, level sensors in the end product cooler, connected to a controller. The method also comprises a benzene circulation loop with a pump, a container and a pressure sensor, collectors for distributing benzene and hydrogen to standby units, apparatus for removing trace impurities from benzene, a liquid cyclohexane pipe, shut-off valves, additional temperatures sensors in hydrogen and benzene hydrogenation reactors, and a pressure and residual gas flow sensor. Benzene and hydrogen are fed from the container with a pump and shut-off valves along the circulation loop to benzene and hydrogen distribution controllers. The initial mixture is heated and directed through heat exchangers and shut-off valves into the apparatus for removing trace impurities from benzene and into hydrogen and benzene hydrogenation reactors. The weighted average temperature of the mixture is determined and is regulated through supply of condensate.

EFFECT: wider range of application, increased output and quality of obtained cyclohexane.

2 cl, 2 dwg, 1 tbl

 

The present invention relates to devices and methods of regulation processes, and may find application in the chemical industry, for example in the manufacture of caprolactam.

A known method of separation of cyclohexane by distillation in two devices with capacitors, in which gases, water and part of the unreacted cyclohexane return to the column, and a concentrated fraction is used in the production of caprolactam (U.S. Pat. Of the Russian Federation No. 2226185, IPC SS 13/18, 27/28, 45/82, 29/18, 2000).

The disadvantage of this method is the limited scope, the lack of gas emissions during the processing of raw materials benzene and hydrogen.

The known method for obtaining a mixture of cyclohexane and benzene, followed by separation of the reaction products. To simplify the fuel mixture benzene, hydratious, using the hydrogen fed to the reactor (Ed. mon. No. 1833359, SS 45/32, 35/05, 1993).

The disadvantage is the low yield due to inaccurate dosing of benzene and hydrogen, as well as reduced productivity and neudovletvoritelnye quality products for sulphur soedineny.

The closest is a way of managing the process of obtaining intermediates caprolactam by hydrogenation, for example, benzene in the presence of a catalyst, the original mixture of benzene and vodorodozapravki in heat exchangers and sent to the hydrogenation reactor, regulate the temperature and the resulting cyclohexane is sent to the cooler-condenser and then for the production of caprolactam, and the residual gas is returned to the process. Management controller is used (U.S. Pat. Of the Russian Federation No. 2296741, CL. SS 35/08, SS 29/19, SS 49/309, SS 45/00, G05D 27/00, 2008).

Lack of control is the low quality of the benzene in the feed to the hydrogenation reactor, as it does not provide additional cleaning of the benzene from the trace. Not enough is controlled by the temperature in the hydrogenation reactor, which reduces the quality of the product. In addition, when returning the residual gases in the process does not take into account loss of cyclohexane, which reduces performance.

The task of the invention is the expansion of applications, improving productivity and quality of product.

The problem is solved in that way to control the flows in the production of cyclohexane containing heat exchangers, condensers, reactors for the hydrogenation of benzene and hydrogen, refrigerator finished product separator with sensors and valves expenses benzene and hydrogen, the temperature sensors in the hydrogenation reactor, the level sensor in the tank finished product connected with the controller further includes a circuit benzene with pump, tank and the sensor is m pressure the collectors of the distribution of benzene and hydrogen on reserve units, apparatus for removal of benzene from the trace, the pipeline of liquid cyclohexane, off valves-valve, additional temperature sensors in the reactor hydrogenation of benzene and hydrogen and the flow of residual gases and pressure, thus fed from the tank with the pump and the shutoff valve on the circuit benzene and hydrogen at the collectors of the distribution of benzene and hydrogen, the initial mixture is heated and directed through the heat exchangers and the selectors-valve apparatus for removal of benzene from trace contaminants in the reactor hydrogenation of benzene and hydrogen, determine the average temperature of the mixture and regulate its flow of condensate; received cyclohexane send in the fridge ready product, allocate the residual gases in the separator and sent considering the consumption of residual gas in the line of hydrogen on reserve units, and the liquid phase cyclohexane served by pipeline in the line of the finished product; and a specified ratio of benzene and hydrogen support using the controller's effect on the valve expenses benzene and hydrogen with a correction for the pressure of residual gases. In addition, the controller provides communication with upper level management.

Research of processes of production of caprolactam showed that the La quality, it is necessary to clean the original products (for example, benzene), using the contours of the circulation, the apparatus for removing trace contaminants. The residual gas (hydrogen) can be used in the process of returning it back. It is also necessary to more accurately regulate the temperature in the reactor (the increase in the number of points in the reactor). To improve performance, use the headers on the load distribution with the appropriate equipment and to increase the accuracy of adjustment of the parameters to use controllers in the management process with the selection of the zones of regulation by temperature and pressure and improve the accuracy of controlling the ratios of benzene and hydrogen with a correction for the pressure of the residual gases.

The essence of the invention is illustrated by drawings, which shows a schematic diagram of control in the production of cyclohexane. The diagram (figure 1) includes units 1-15. 1 - capacity for benzene; 2 - pump benzene units; 3 - manifold distribution of benzene units; 4 - manifold hydrogen distribution on the units; 5 - heat exchanger heating benzene and hydrogen; 6 - heat exchanger heating the mixture; 7 - apparatus for removal of benzene from trace contaminants; 8 - hydrogenation reactor (primary); 9 - hydrogenation reactor (auxiliary); 10, 11 - capacitors; 12 - refrigerator finished product; 13 - separator. For the circulation of the reagents used shall be: 14 - circuit benzene (capacity 1 - pump 2 - capacity : 1 pipelines); 15 - pipeline liquid cyclohexane;

16 - gauge pressure of benzene; 17, 18 - loop benzene (sensor 17, the valve 18); 19 shutoff valve; 20, 21 - loop hydrogen; 22, 23 - off valves-valve; 24-33 - temperature sensors in reatore 8; 34-43 - temperature sensors in the reactor 9; 44 - a level sensor in the refrigerator 12; 45 - flow sensor residual gas (hydrogen) at the outlet of the separator 13; 46 - the gauge of pressure of residual gases; 47 - controller (figure 2)connected to the sensor input 16, 17, 20, 24-33, 34-43, 44, 45, 46, and outputs the valves 18, 21. Electrical connection of sensors and valves conventionally not shown. The level sensors and the valve in the capacitors 10, 11 are conventionally not shown. In addition, the controller 47 provides communication with upper level management to transfer production, consumption norms for cyclohexane and other parameters.

The method is carried out for 4 units with capacity up to 5 t/h of benzene and hydrogen. The drawing shows one process scheme (3 units conventionally not shown).

Ask expenditure:

- benzene - 4 t/h; hydrogen 260 t/h (65 t/t); the level of diluent in the device 7 - 0,66; the concentration of trace contaminants in the apparatus 7 to within 0.00001 wt.%. Zone control temperature in the heat exchangers 5, 6 - 125-160C; zone regulation of the temperature in the PE Torah hydrogenation 8, 9 - 240-250C; maximum values in the hydrogenation reactor 8, 9 - of 0.45 t/h, flagged and, if necessary, blocked; zone regulation of the pressure in the hydrogenation reactor 8, 9 and 1.5-2 MPa; zone regulation of the pressure in the separator 13 is 0.4-0.7 MPa and the level in the refrigerator for 12 - 25-35 wt.% with minimum alarm level - 24 wt.%. Control of hydrogen in the residual gases - 0.05 m3; control pressure alarm before the pump 2 is 0.2 MPa.

Enter the current information in the controller 47 from sensors 16, 17, 20, 24-33, 34-43, 44, 45, 46. Serves the benzene and hydrogen in a ratio, which vary depending on the pressure of the residual gases. Circulate benzene by circuit 14 (capacity 1 - pump 2 - capacity 1). The selectors 19 and 23 is closed at this time. After circulation of the selectors 19 and 23 open and together with the hydrogen serves mixture in the tube of the heat exchanger 5. Heat the mixture to 120C and sent to the heat exchanger 6, where it is heated to a temperature of 125-160C and then the mixture through a shut-off valve 22 serves in the apt. 7 for benzene purification from sulfur and other compounds. The device is filled with a catalyst to 0.66 (by volume), which when worn replace with a new one. After cleaning through the selectors 22 and 23, the mixture is sent to the primary and secondary hydrogenation reactor 8, 9. If benzene is supplied cleaned, the flow of the mixture is directed along the contour of the WMD pipeline (the selectors 22 and 23 are closed) in the reactor 8, 9. The reaction of hydrogenation is exothermic and takes place with evolution of heat.

The capacitors 10 and 11 serve to remove heat. The temperature in the reactors 8 and 9 is measured at 10 points along the height, which increases the accuracy of the measurement and the average value (depends on the load on the hydrogenation reactor 8, 9), adjust the flow of condensate (regulation capacitors 10, 11 are level - level sensors, valves conventionally not marked).

The resulting cyclohexane send in the fridge ready product 12, which control the level of information of the sensor 44 and then the cyclohexane guide for the production of caprolactam. The residual gas after the refrigerator 12 is directed into the separator 13 where the selected liquid cyclohexane through the pipeline 15 is directed in the line of the main pipeline after the refrigerator 12, and the residual gas is sent to other units. The ratio of benzene and hydrogen correct, also the pressure of residual gases.

Example

Consider a numerical example for a single unit. The benzene from the tank 1 by the pump 2 according to the sensor 17 at a rate of 4 t/h with pressure to 0.80 MPa (according to the sensor 16) is directed to the circulation circuit 14 (capacity 1 - pump 2 - capacity 1). Then mixed with hydrogen (according to the sensor 20) and serves in the amount of 260 t/h ratio (4/260=0,015 UNED) at a pressure of mod is cnyh gases 0.5 MPa (according to the sensor 46) and is directed to the heat exchanger 5, heat (steam heating) to 124C, and then into the heat exchanger 6.

The mixture is heated to 150C and sent to the device 7, where the purification of benzene from sulfur compounds on the catalyst filling apparatus to 0.66 by volume, and at a temperature of 150C and a pressure of 1.8 MPa bring the contents of trace contaminants to within 0.00001 wt.% (lab results). The mixture is then served in the annulus hydrogenation reactor 8. Forming a steam-water mixture is hydrated with the formation of cyclohexane, determine the weighted average temperature (sensor information 24-33) the height of the reactor T=/T1+T2+..T10/10=240C (load 4 t/h with constant coefficients at temperatures equal to one) and adjust the flow of condensate into the condenser 10 (loops conventionally not shown) to bring the temperature to the set value is 245. For a more complete conversion of benzene vapor-liquid mixture is sent into the reactor 9 (charging type). Determine a weighted average temperature of 10 points (on sensor information 34-43)equal to 249C, and regulate its flow of condensate level in the condenser 11. Increased temperature in the reactor 9 says about the poisoning of the catalyst in the reactor 8, so the total conversion of benzene to cyclohexane occurs in the reactor 9. Received the product in the amount of 5.2 t/h to send in holodilny the 12 level, 30 wt.% (measured by sensor 44). Residual gas in the amount of 2000 m3(according to information from sensor 45) is sent to the separator 13 for separating cyclohexane from the residual gas. Selected cyclohexane in the amount of 0.03 t (according to the laboratory analysis) sent through the pipeline 15 to the output of the refrigerator 12 in the main line. Residual gas in the amount of 1500 m3allocated to units 1-3, or when the hydrogen content is less than 0.05 m3discharged into the atmosphere. The system pressure hydrogenation is governed by the sensor 46 and is supported at 1.6 MPa (zone regulation 1.5 to 2 MPa) and shall be adjusted by the ratio of the benzene and hydrogen at a flow of hydrogen through the loop 20, 21.

Thus, feeding benzene and hydrogen units hydrogenation at a corresponding upgrading equipment, improving performance cyclohexane. Cleaning the benzene from the concentration of improving the quality of benzene and accordingly improve the quality in the production of caprolactam.

Adjusting the benzene and hydrogen in a certain ratio and highlighting areas of regulation of pressure and temperature hydrogenation using a controller, increase the yield of cyclohexane. Returning cyclohexane and the residual gas in the hydrogenation process, improving performance is on the cyclohexane, that saves raw materials and energy resources and increase management efficiency in the production of caprolactam. The table below shows the results of industrial tests of the method.

Table
Indicesthe proposed methodthe placeholder
1. Regulation of the ratio of benzene/hydrogen, Rel. ed0,0010,01
2. Regulation
the reactor temperature1,41,8
hydrogenation,C
3. Regulation
pressure, MPa0,0020,004
4. Content concentration
sulfur compounds0,0000090,0001
in benzene after cleaning, wt.%
5. Loss of cyclohexane, % Rel.4,310
6. Increase productivity
for cyclohexane, % Rel.20-

The implementation of the method is planned in 2008 in Togliatti JSC "KuibyshevAzot". The economic effect from the introduction of 7 million rubles per year.

1. The method of regulation of flows in the production of cyclohexane containing heat exchangers, condensers, reactors for the hydrogenation of benzene and hydrogen, refrigerator finished product separator with sensors and valves expenses benzene and hydrogen, the temperature sensors in the hydrogenation reactor, the level sensors in the fridge ready product connected to the controller, characterized in that it further comprises a circuit benzene with pump, tank and pressure sensor, the collectors of the distribution of hydrogen on the benzene backup units, apparatus for removal of benzene from the trace, the pipeline of liquid cyclohexane, off valves-valves, additional temperature sensors in the reactors gidrirovanie the benzene and hydrogen and the flow sensor residual gases and pressure, thus fed from the tank with the pump and cut off the valves on the circuit benzene and hydrogen at the collectors of the distribution of benzene and hydrogen, the initial mixture is heated and directed through the heat exchangers and off valves-the valves in the apparatus for removal of benzene from trace contaminants in the reactor hydrogenation of benzene and hydrogen, determine the average temperature of the mixture and regulate its flow of condensate from cyclohexane send in the fridge ready product, allocate the residual gases in the separator and sent considering the consumption of residual gas in the line of the hydrogen reserve units, and the liquid phase cyclohexane served by pipeline liquid cyclohexane and output it in the fridge ready product, with a given ratio benzene/hydrogen support impact on valves expenses benzene and hydrogen with a correction for the pressure of the residual gases.

2. The method according to claim 1, wherein the controller provides communication with upper level management.



 

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24 cl, 4 dwg

FIELD: physics; control.

SUBSTANCE: invention relates to methods and devices for regulating processes and can be used in chemical industry during production of cyclohexane. The method of regulating streams in the production of cyclohexane comprises heat exchangers, condensers, hydrogen and benzene hydrogenation reactors, an end product cooler, a separator with benzene and hydrogen flow valves and sensors, temperature sensors in the hydrogenation reactors, level sensors in the end product cooler, connected to a controller. The method also comprises a benzene circulation loop with a pump, a container and a pressure sensor, collectors for distributing benzene and hydrogen to standby units, apparatus for removing trace impurities from benzene, a liquid cyclohexane pipe, shut-off valves, additional temperatures sensors in hydrogen and benzene hydrogenation reactors, and a pressure and residual gas flow sensor. Benzene and hydrogen are fed from the container with a pump and shut-off valves along the circulation loop to benzene and hydrogen distribution controllers. The initial mixture is heated and directed through heat exchangers and shut-off valves into the apparatus for removing trace impurities from benzene and into hydrogen and benzene hydrogenation reactors. The weighted average temperature of the mixture is determined and is regulated through supply of condensate.

EFFECT: wider range of application, increased output and quality of obtained cyclohexane.

2 cl, 2 dwg, 1 tbl

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