Method for operating mode of caprolactam production |
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IPC classes for russian patent Method for operating mode of caprolactam production (RU 2366651):
 
 Production area environmental control device / 2363031
Invention relates to instrument making and can be used to control production area environments. Proposed device comprises regulator unit, control unit, temperature pickup, noise and illumination pickups. It also includes transducers of signals generated by the temperature, noise and illumination pickups. It incorporates setters of maximum and minimum tolerable temperatures, maximum tolerable noise and maximum tolerable illumination. The device includes comparator for every aforesaid setter and logical elements for every aforesaid controlled parametre. It incorporates the 1st , 2nd, 3rd and 4th logical elements, read-only memories for all controlled parametres, shift registers and counters of all aforesaid parametres. In compliance with this invention, the proposed device additionally comprises I/O units, communication unit, satellite receiver unit, power supply monitor, power buffer, ADC, real-time clock unit, RAM, nonvolatile memory unit. It incorporates, further on, real-time clock storage battery, relative humidity pickup with amplifier, airflow speed pickup with amplifier, environment heat load intensity pickup with amplifier, carbon oxide concentration pickup with amplifier, sulfur oxide concentration pickup with amplifier, nitrogen oxide concentration pickup with amplifier, ozone concentration pickup with amplifier, town gas concentration pickup with amplifier, power supply voltage pickup with amplifier and power supply.
 Method for control of potassium chloride preparation / 2359909
Invention can be used in the process of potassium chloride preparation by the method of solution-crystallisation. The method for the control of the aforesaid process by the way of input water flow varying includes: 1) the adjustment of water flow fed into crystallisation alkali liquor depending on potassium chloride concentration in the liquor and water consumption for washing of crystallisation apparatus; 2) detection of the temperature, density and consumption of alkali liquor. The said measurements allow to determine the sodium chloride content in the alkali liquor. The crystallisation water consumption is calculated on the basis of the obtained data according to proposed equation; the calculated values are input as assignment to the system of water consumption control.
 Control of process of production of loose form of powdery choline chloride from its aqueous solution / 2356907
Invention is related to automation of technological processes and may be used in automation of process of production of loose form of powdery choline chloride from its aqueous solution. In method that provides for use of crushed and fractionated dry sugar beet pulp as active adsorbent, its mixing with previously heated aqueous solution of choline chloride, and then drying in vibration dryer by superheated steam of atmospheric pressure, separation of spent superheated steam flow into the main one, sent to vibration dryer with creation of recirculation circuit, and additional one sent for reheating of choline chloride prior to its supply for mixing, the novelty is the fact that superheating of atmospheric pressure steam is done with heating steam, at that heating steam is produced by means of steam generator with electric heating elements, feed pump and safety valve, heating steam condensate produced in this process after superheating and condensate produced during heating of aqueous solution of choline chloride is taken to condensate collector, and then in mode of closed circuit is supplied in steam generator, at that flow rate of crushed and fractionated dry pulp is measured, as well as aqueous solution of choline chloride coming for mixing, flow rate and temperature of superheated steam upstream vibration dryer, choline chloride temperature before and after its heating, pressure of choline chloride after heating, temperature and humidity of mixture of crushed and fractionated dry pulp and aqueous solution of choline chloride prior to supply for drying, amplitude and frequency of oscillations in gas-distributing grid of vibration dryer, flow rate and humidity of powdery choline chloride after drying, level of condensate in steam generator and pressure of heating steam, at that flow arte of dry sugar beet pulp after fractionation is used to set flow rate of heated choline chloride coming for mixing, and flow rate and humidity of prepared mixture of crushed and fractionated dry pulp and aqueous solution of choline chloride prior to supply for drying, flow rate and humidity of powdery choline chloride after drying are used to determine amount of evaporated moisture in vibration dryer, which is used to establish flow rate of superheated steam in the main circuit of recirculation, and its temperature is established by current value of temperature of mixture of crushed and fractionated dry pulp and aqueous solution of choline chloride by setting of specified capacity of steam generator affecting power of electric heating elements, at that in case condensate level in steam generator falls below specified value, condensate is supplied from condensate collector, and when pressure of steam in steam generator reaches upper limit value, steam pressure is released through safety valve, if flow rate of mixture of crushed and fractionated dry pulp and aqueous solution of choline chloride deviates prior to supply for drying to the side of increase from specified value, at first frequency is increased, and then amplitude of oscillations in gas-distributing grid of vibration dryer, if flow rate of mixture of crushed and fractionated dry pulp and aqueous solution of choline chloride deviates to the side of reduction from specified value, at first frequency is reduced, and then amplitude of oscillations in gas-distributing grid of vibration dryer, current values of temperature and flow rate of choline chloride prior to heating are used to set flow rate of spent superheated steam in additional recirculation circuit, at that temperature of choline chloride after heating is used to set specified pressure of choline chloride at the inlet to mixer.
 Method of controlling process of sylvinite ore dissolution / 2352385
Invention relates to technique of controlling processes of sylvinite ores dissolution and can be used in production of potassium chloride by dissolution-crystallisation method. Method of controlling processes of sylvinite ores dissolution includes regulation of ore supply depending on content of useful component in input flows, measuring ready solution temperature and determining sodium chloride content in solution by calculation method. Additionally determined are density, temperature and consumption of dissolving solution, content of sodium chloride in it is determined by content of useful component, density and temperature. Ore supply is calculated according to suggested equation and calculated value is given as task to system of weigher control.
 Automated method of controlling and managing process for preparing sugar syrup mixture for crystallisation by cooling / 2342438
Proposed automated method of controlling and managing the process of preparing sugar syrup mixture for crystallisation by cooling makes provisions for regulating the volumetric discharge of water entering the mixer and the level of sugar syrup in it. Regulating the level of the sugar syrup in the vertical mould is achieved by acting on the adjustable-frequency electric drive of the sugar syrup pump. Periodically using the lab the density of the ready sugar syrup is controlled at the exit from the mixer. The active electrical power which is used in the electric motor of the sugar syrup pump, the temperature and pressure differential of the sugar syrup mixture, coming from the mixer and water at the entrance of the mixer are all measured. The water-mass density is calculated by its temperature and the density of the sugar syrup mixture by its pressure differential. Afterwards the volume flow rate is worked out by the measured volume flow rate of water, by the estimated value of the density of water and sugar syrup mixture and by the density of ready sugar syrup measured in the laboratory. The dependency ratio of the active electric power from the volume rate of flow of the sugar syrup mixture and the differential in its pressure N=α1Q3 УΔPy+α2QyΔPy , where N - active electric power; QY - volume rate of flow of sugar syrup mixture entering the mixer; ΔPY - pressure differential of the sugar syrup mixture; α1, α2 - coefficients. The obtained plot is used for future calculations of volume rate of flow of sugar syrup mixture only with measured values of active electric power and pressure differential of the sugar syrup mixture. The current task of the regulator of the volumetric water discharge is determined on the basis of measured values of this output, estimated values of the density of sugar syrup mixture, water and volume rate of flow of the sugar syrup mixture, the determined value of density of ready sugar syrup mixture and the task of the regulator calculated in the previous control step. The solid content of the original sugar syrup mixture is controlled - by its temperature and density in the ready sugar syrup mixture. This invention makes it possible to reduce the loss of sugar from molasses due to a more qualitative stabilisation of the density of molasses on its exit from the mixer.
 Work environment remote control device / 2335795
Device contains control unit, temperature sensor, noise sensor and luminance sensor, temperature, noise and luminance signal converter per each sensor, boundary value generator per each controlled factor, comparator per each generator of maximum permissible values of measured temperature, noise, luminance, logic elements per each controlled factor, read-only storage per each controlled factor, shift registers, value counter of each controlled factor, control unit and generator. Besides, device contains relative humidity detector, air speed transducer and pulse number sensor, signal converters of relative humidity, air speed and pulsation factor per each sensor, boundary value generator per each additional controlled factor, comparator per each generator of each additional controlled factor, logic elements per each controlled factor, read-only storage per each controlled factor, shift registers, counter of maximum relative humidity, counter of minimum relative humidity, counter of air speeds, counter of pulsation factors.
 Work environment remote control device / 2335794
Device contains control unit, temperature sensor, noise sensor and luminance sensor, temperature, noise and luminance signal converter per each sensor, boundary value generator per each controlled factor, comparator per each generator of maximum permissible values of measured parameters, logic elements per each controlled factor, read-only storages per each controlled factor, four shift registers, counter of maximum temperature, counter of minimum temperature, noise counter, luminance, control unit and generator. Besides, device contains chemical sensor with converter, chemical concentration generator, logic element of maximum chemical concentrations, read-only storage of maximum chemical concentrations, shift register, counter of maximum chemical concentrations.
 Air humidity detector / 2332701
Invention can be applied for automated systems of microclimate control in closed warehouse space for improving accuracy of heat and humidity calculation in controlled variable air medium. Detector contains temperature sensor, relative humidity and atmospheric pressure detectors, temperature converter to air vapour pressure, and computing unit. Using of converter and atmospheric pressure detector allows for increased accuracy of humidity detection. Invention provides automated real-time humidity and increased accuracy of humidity detection.
 System of automatic temperature profile support in reactor / 2326424
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.
 System of engine fuel supply / 2325547
System of engine fuel supply consists of fuel tank wherein the following is installed: a level meter connected to the inlet of a "fuel-water" level regulator, and a control valve to flow out commodity water; the said valve is connected to a control outlet of the regulator. The level meter is made as two sensors of the fuel level, located in a portion of the lowest allowable fuel level mainly at opposite sides of the tank and one water level sensor located at the flow out level. The control valve is assembled so as to provide a positive feedback with the regulator upon receiving a signal on water presence and a negative feedback when there is no signal entry. At the moment of a positive feedback and water flow out the regulator is programmed to let out not more than 100 kg of fuel.
 A method for production of epsilon-caprolactam / 2240312
The invention relates to a method of obtaining
 -caprolactam rearrangement cyclohexasiloxane with a solid acid catalyst in the gas phase
The method of producing caprolactam / 2125556
 The reactor for the production of caprolactam by beckmann rearrangement of cyclohexasiloxane / 2005536
The invention relates to chemical technology and can be used in the manufacture of caprolactam
 Method for operating mode of caprolactam production / 2366651
Invention refers to the method for operating mode of caprolactam production from benzene carried out in the plant with one process line including the stations of benzene hydrogenation with hydrogen, cyclohexane oxidation with oxygen, cyclohexanone rectification, oximation, cyclohexanone oxim rearrangement to caprolactam, neutralisation of the reaction mixture with ammonia and mixing of caprolactam. The said stations are connected with pumps, pipelines with sensors and valves for consumption control of benzene, hydrogen, cyclohexanone, hydroxylamine sulphate and oleum, sensor of acid value and pH-metre of caprolactam. The said line contains additionally the second process line of caprolactam production from phenol including the stations of phenol hydrogenation with hydrogen, dehydrogenation of cyclohexanol with circulation circuit including: pump - station of cyclohexanol dehydrogenation - station of cyclohexanone rectification - pump, station of cyclohexanone rectification, oximation with hydroxylamine sulphate, rearrangement of cyclohexanon oxim to caprolactam and neutralisation of the reaction mixture with ammonia connected by pumps and pipelines with sensors and valves for control of benzene, hydrogen, cyclohexanone, hydroxylamine sulphate and oleum consumption, sensor of acid value and pH-metre of caprolactam and contains the device of benzene-phenol ratio connected with stations of benzene and phenol hydrogenation, oxidation and dehydrogenation; device of cyclohexanone distribution to the oximation stations connected with rectification stations and (through the cyclohexanone mixing tank) with the oximation stations; device of crystalline caprolactam switch-over to liquid caprolactam connected with caprolactam mixer, concentrator of crystalline caprolactam and tank of liquid caprolactam. The total caprolactam capacity, benzene-phenol ratio, cyclohexanone distribution to oximation stations, shipping of crystalline and liquid caprolactam to customers are set up; the consumption of benzene, phenol, hydrogen, cyclohexanone, hydroxylamine sulphate and oleum are corrected with corresponding valves.
Method of purifying ε-caprolactam / 2427570
Invention relates to an improved method of purifying crude ε-caprolactam obtained from cyclohexanone oxime via gas phase Beckmann rearrangement, comprising a step for crystallisation of ε-caprolactam from the solution of crude ε-caprolactam in ether or halogenated hydrocarbon, a step for washing the crystalline ε-caprolactam obtained from the crystallisation step with a solvent and a step for hydrogenation of the crystalline ε-caprolactam through contact with hydrogen in the presence of a hydrogenation catalyst.
 Method of controlling drying of cyclohexanone oxime / 2465265
Method of controlling drying of cyclohexanone oxime from an oximation step, involving further use of a separator with a phase separating device, having pipes for collecting ammonium sulphate and cyclohexanone oxime with collectors, wherein the outlet of the ammonium sulphate collector is connected to the first inlet of the ammonium sulphate collector of the first drying step, and the outlet of the cyclohexanone oxime collector is connected to the inlet of the separator of the first step with a flow sensor and a valve, the first outlet of which is connected to the second inlet of the ammonium sulphate collector of the first step, and the second outlet is connected to the cyclohexanone oxime collector of the first step, which is connected by a pipe to a pump and a vortex mixer to which ammonium sulphate is also fed, with a flow sensor and a valve, hydroxylamine sulphate with a valve and ammonia with a flow sensor and a valve, installed in front of a heat exchanger, after which medium pH and temperature sensors are installed, and the outlet of the vortex mixer is connected to the inlet of the separator of the second drying step with a phase separating device, having pipes for collecting ammonium sulphate and cyclohexanone oxime with collectors; the outlet of the ammonium sulphate collector is connected to the inlet of the ammonium sulphate collector of the second step with a pump, and the outlet of the cyclohexanone oxime collector is connected to the inlet of the cyclohexanone oxime collector of the second step with pressure and temperature sensors, connected to a filter and a pump for feeding cyclohexanone oxime for regrouping; control is carried out by setting flow rate of cyclohexanone oxime for drying, ammonium sulphate into the first and second drying steps, pH of the medium, concentration of residual cyclohexanone in cyclohexanone oxime and valves for feeding cyclohexanone oxime, ammonium sulphate to the first and second drying steps, ammonia and hydroxylaminesulphate are actuated, respectively.
 Method for automated oils mixing management, said oils being manufactured from oil product, by means of forming mixing timetables in real time / 2246984
Method is based on use of computer system, including an optimizer, tables for selection of goal function, block for determination of optimization method. Database for recording inputted information and received results is used as well as block for importing data concerning initial state of reservoir fleet and mixing task. Graphic user interface is used to indicate and alter current data during creation of timetable, parameters for optimizer adjustment and indication of textual and graphical system reports. Block for controlling trustworthiness of initial data for forming the best timetable, block for generation of optimization task matrix and block for interpretation of results of optimization task solution are used. Data concerning amount of components, admixtures and product oils in all mixing reservoirs at the moment of beginning of timetable creation, concerning planned tasks for readiness of product oils at certain time moment in accordance to shipment graph, concerning mixing receipts and certification time for each oil, concerning mixing time and readjustment of mixing reservoir during transfer from one oil type to another, concerning speed of feeding of each component and admixture from appropriate reservoirs, concerning configuration of area of mixing and amount of mixing reservoirs are all transferred to computer system from data import block. After check of physical possibility, linear programming matrix is generated for use by optimizer, which automatically selects an optimization method for determination of the best timetable, which is interpreted in form of series of mixing of given product oils, beginning and ending time for each mixing, transfer of each component and admixture from appropriate reservoirs for mixing of each oil, beginning and ending time for feeding of prepared oil directly after mixing and certification into appropriate product reservoir, time of switching feeding of component after filling of one component reservoir to another by results interpretation block.
 Method for automatic controlling of continuous malting process / 2248390
Method involves providing continuous malting process in rotating drum; measuring and stabilizing temperature of malt by changing air flow rate for cooling of grain under germination procedure; additionally measuring malt moisture content and regulating it depending on changing of malt moisture content as compared to set values by changing water supply for grain moistening during germination process; also, regulating water supply for cooling air and correcting changing of air flow rate for cooling of grain under germination process depending on changed temperature of malt as compared to set values.
Method of automatically governing biotechnological process / 2248399
Invention concerns governing periodical air-intake biotechnological process carried out in bioreactor. Method comprises measuring oxygen content in effluent gas, working volume of culture medium, concentration of biomass, and concentration of intermediate product of its vital activity. Measured parameters allow specific oxygen consumption rate and velocity of intermediate product concentration change to be determined to enable regulation of feeding air used in aeration, supplying nutritional medium, and agitating culture medium. Moreover, temperature of culture medium, temperature of supplied and withdrawn cooling agent, and consumption of the latter are measured to use these parameters for determining biomass heat release rate and velocity of intermediate product amount change. The two latter parameters enable regulation of feeding air used in aeration and supplying nutritional medium. The following characteristics are thus improved: elevating power by 8.1%, maltase activity by 7.9% and resistance by 7.4%.
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FIELD: chemistry. SUBSTANCE: invention refers to the method for operating mode of caprolactam production from benzene carried out in the plant with one process line including the stations of benzene hydrogenation with hydrogen, cyclohexane oxidation with oxygen, cyclohexanone rectification, oximation, cyclohexanone oxim rearrangement to caprolactam, neutralisation of the reaction mixture with ammonia and mixing of caprolactam. The said stations are connected with pumps, pipelines with sensors and valves for consumption control of benzene, hydrogen, cyclohexanone, hydroxylamine sulphate and oleum, sensor of acid value and pH-metre of caprolactam. The said line contains additionally the second process line of caprolactam production from phenol including the stations of phenol hydrogenation with hydrogen, dehydrogenation of cyclohexanol with circulation circuit including: pump - station of cyclohexanol dehydrogenation - station of cyclohexanone rectification - pump, station of cyclohexanone rectification, oximation with hydroxylamine sulphate, rearrangement of cyclohexanon oxim to caprolactam and neutralisation of the reaction mixture with ammonia connected by pumps and pipelines with sensors and valves for control of benzene, hydrogen, cyclohexanone, hydroxylamine sulphate and oleum consumption, sensor of acid value and pH-metre of caprolactam and contains the device of benzene-phenol ratio connected with stations of benzene and phenol hydrogenation, oxidation and dehydrogenation; device of cyclohexanone distribution to the oximation stations connected with rectification stations and (through the cyclohexanone mixing tank) with the oximation stations; device of crystalline caprolactam switch-over to liquid caprolactam connected with caprolactam mixer, concentrator of crystalline caprolactam and tank of liquid caprolactam. The total caprolactam capacity, benzene-phenol ratio, cyclohexanone distribution to oximation stations, shipping of crystalline and liquid caprolactam to customers are set up; the consumption of benzene, phenol, hydrogen, cyclohexanone, hydroxylamine sulphate and oleum are corrected with corresponding valves. EFFECT: enhancing of productivity and caprolactam quality. 9 cl, 1 ex, 1 tbl, 3 dwg
The present invention relates to methods of producing caprolactam and may find application in the processing of benzene, phenol, cyclohexane, cyclohexanol, cyclohexanone, followed by aksamitowana, isomerization cyclohexasiloxane and shipment of caprolactam to the consumer. A known method of controlling the process of obtaining caprolactam, which regulate the pH value of the reaction medium in the reactor with the correction of the flow rate of the rearrangement product. To enhance the yield of caprolactam measure the concentration of ammonium sulfate and acidity rearrange and adjust the flow of ammonia and gaseous ammonia in the reactor. (Ed. mon. No. 1648946, 07D 201, G05D 27/00 from 24.05.89,) Lack of control is a limited opportunity to improve performance by caprolactam. Known industrial method of producing caprolactam with the processing of cyclohexanone to caprolactam. Feedstock benzene is subjected to hydrogenation, oxidation, distillation, and then cyclohexanone sent to oxymorphine. Received cyclohexanone sent to isomerization to rearrange and then share in the sump organic layer (lactam oil) and an inorganic layer (ammonium sulfate) and sent to the catalytic Converter for the purification of caprolactam alkali or extraction of organic Rast is Oriflame. (Ed. by V. Ovchinnikov and Rusinskogo VP "caprolactam", M.: Chemistry, 1977, chapters 2, 3, 9.) The disadvantages of production is low and the quality of caprolactam and low performance when using only the scheme of one benzene. The closest is a way of managing the process of obtaining caprolactam, including distillation columns, obtaining cyclohexane oxidation of benzene and direction of cyclohexanone-rectified to install oxymorphine, reactors regrouping and neutralisation and then to install the isolation and purification of caprolactam. Cyclohexanone-rectified adjust change of temperature regimes in the columns, and the acidity of the rearranged product regulate the flow of oleum (U.S. Pat. Of the Russian Federation No. 2043340 from 10.09.95,, C07D 201/04, G05 27/00). The disadvantages are the low productivity of the installation and the quality of the caprolactam to trace when using as a monomer benzene. Besides, not considering the total load, the load distribution monomers for the first and second lines is not taken into account the burden of caprolactam consumers. The task of the invention is to increase productivity and improve the quality of caprolactam, as well as the expansion of the scope. The problem is solved in that way in the management of the production of caprolactam from benzene, held in the installation process line including units hydrogenation of benzene with hydrogen distillation of cyclohexanone, oxymorphine hydroxylaminopurine, rearrangement cyclohexasiloxane in caprolactam, neitralizatsii ammonia and a mixture of caprolactam, which are interconnected pumps, pipelines with sensors and valves for adjusting benzene, hydrogen, cyclohexanone, has synthesis, oleum, sensor indicator acidity and pH meter caprolactam, the installation further comprises a second production line for the production of caprolactam from phenol, including units hydrogenation of phenol by hydrogen in the dehydrogenation of cyclohexanol with a circuit, comprising: a pump unit dehydrogenation of cyclohexanol unit rectification of cyclohexanone - pump, the rectification unit cyclohexanone oxymorphine hydroxylaminsulphate, rearrangement cyclohexasiloxane in caprolactam and neutralize ammonia, interconnected pumps and pipelines with sensors and valves expenses phenol, hydrogen, has synthesis, oleum, sensors measure of the acidity and pH meter caprolactam, and also contains a device ratio benzene-phenol, United pipe with blocks hydrogenation of phenol, block oxidation and components the dehydrogenation; the distribution device cyclohexanone units oxymorphine, United pipe with blocks rectification and through the tank mixture of cyclohexanone with blocks of oxymorphine; a switching device of the crystalline caprolactam liquid caprolactam, United pipeline with mixer caprolactam and hub crystalline caprolactam and capacity of liquid caprolactam, ask your overall workload caprolactam, the ratio of benzene-phenol in the hydrogenation reactor, the distribution of cyclohexanone units oxymorphine, shipment crystalline and liquid caprolactam to the consumer and are adjusting accordingly the cost of benzene, phenol, hydrogen units hydrogenation, oxidation, dehydrogenation and rectification, the cost of cyclohexanone has synthesis on the power oxymorphine, oleum on the block rearrangement impact on the corresponding valve. In addition, the hydrogenation of benzene with hydrogen is carried out in two serially connected reactors and adjust the process temperature in the range of 160-230°C and pressure up to 0.8 MPa with recirculation otdelochnih gases. Hydrogenation of phenol with hydrogen is carried out in two serially connected reactors and adjust the process temperature in the range of 150-180°C. and a pressure of 0.75 MPa with recirculation otdelochnih gases. Ocil is of cyclohexane is carried out in two blocks of four reactors and adjust the process temperature in the range of 145-160°C and a pressure of 0.75 MPa. Dehydrogenation of cyclohexanol is carried out in five reactors and adjust the process temperature in the range of 370-450°C and pressure up to 0,065 MPa. Rectification of cyclohexanol and cyclohexanone is carried out in two reactors for the production of cyclohexanone-rectified and adjust the process temperature in the range of 120-140°C and pressure up to 0.25 MPa and a ratio of circulation to 20-30. Oxymorphine cyclohexanone by hydroxylaminsulphate conducted in countercurrent system with the faucets in the two reactors at a temperature of 55-80°C and a pressure of 0.1 MPa. Regrouping cyclohexasiloxane in caprolactam is carried out in the reactor at a temperature of 90-110°C and a pressure of 0.1 MPa and correct filing of oleum depending on acidity. Neutralization of sulfate caprolactam is carried out in the reactor ammonia water to 15 wt.% when applying ammonium sulfate and pH of 4.5 to 5.7 and adjust consumption has synthesis at 50°C and a pressure of 0.1 MPa, and the purification of caprolactam produced from trichloroethylene and alkali. Performance caprolactam is up to 180 t/year. Studies of caprolactam showed that to increase performance and quality targets need to use semi-monomers, benzene and phenol with their features. At the stage of hydrogenation of benzene with the floor is the group of cyclohexane and subsequent oxidation, the rectification and direction of cyclohexanone to oxymorphine and regrouping problems with purification of benzene from thiophene and other trace contaminants that affect the quality of the caprolactam. In addition, there are problems associated with losses in the waste by alkaline water and acidic water caprolactam production, which also reduces the performance of the installation. At the stage of hydrogenation of phenol with getting cyclohexanol, dehydration, distillation and direction of cyclohexanone to oxymorphine and the rearrangement does not have problems associated with the quality of the trace (e.g., cyclohexene)improves the performance of the installation. It should be noted that the phenol at a price more expensive than benzene, so the semi - benzene and phenol - should you file to install in a particular ratio with regard to the supply of benzene and phenol, with technological preparation lines for processing of caprolactam and having regard to the shipment of caprolactam to the consumer. Production control is proposed a method of oxidizing a method of obtaining caprolactam from benzene and the scheme of obtaining caprolactam by phenolic scheme to improve performance with improved properties caprolactam. The essence of the invention is illustrated by drawings, which shows a schematic CX the mA management caprolactam. Figure 1 provides a diagram of the production, figure 2 controllers for process control and figure 3 - block diagram of the device. 1 - pump benzene with sensor 2 and the valve 3; 4 - block hydrogenation of benzene (two reactor temperature sensors, condensers for heat dissipation is conventionally not shown); the sensor and the valve on the supply of hydrogen 4-a and 4-b; 5 - device ratio benzene-phenol"includes valve 6, 7, 8, 9 (adjustable gate valve, cut off) and 10, 11 (back gate); 12 - block benzene oxidation with oxygen (air), connected to a pipeline with a valve 8 (supply line air conditional not shown); a 13 - block rectification of obesidade (flow from block oxidation); 14 - pump phenol with sensor 15 and the valve 16; the sensor and the valve on the supply of hydrogen 15-a, 15-b; 17 - block hydrogenation of phenol, connected by pipeline with valve 9; 18 - unit dehydrogenation of cyclohexanol (see one of the five reactors); 19 - the rectification unit (stream from the dehydrogenation unit); the circuit including the pump 20, the pump 20 to the dehydrogenation unit 18 unit rectification 19 - pump 20", connected by pipelines; 21 - distribution device cyclohexanone units oxymorphine (first and second line), including valve 22, 23 and the backup valve 24, 25, United pipelines with capacity of mixing cyclohexanone 26, blocks rectification 1 and 19 with sensor total consumption of cyclohexanone 27; 28 - the first unit oxymorphine (three reactor reciclada reagents) with flow sensors cyclohexanone 29 and valve 30; 31 - second unit oxymorphine with the flow sensor 32 and valve 33; 34 is a block for hydroxylamine sulfate production with the flow sensor 35 and valve 36 to the first block of oxymorphine 28 and the flow sensor 37 and valve 38 to the second unit oxymorphine 31; 39 - the first block rearrangement (reactor with a refrigerator, a temperature sensor, a valve on the supply of alkali, trichloroethylene are conventionally not numbered) with a flow sensor oleum 40, valve 41 and the sensor acidity 42 (when the output of the sensor 42 acidity is determined by laboratory method); 43 - second unit rearrange the flow of oleum 44, valve 45 and the sensor acidity 46; 47 the first reactor neutralization pH meter 48 (sump separation lactam oil from ammonium sulfate not shown); 49 - second reactor neutralization pH meter 50; pumps caprolactam 51, 52 in the mixer caprolactam 53; 54 - switching device of crystalline caprolactam liquid caprolactam, including 55 in the hub of the crystalline caprolactam (to send caprolactam in plastic bags); 56 - capacity liquid caprolactam (to send caprolactam in tanks); 57 - supply of caprolactam to the consumer (Tsereteli), 58 - the supply of crystalline caprolactam; 59 - the supply of liquid caprolactam; 60 - the microcontrollers are connected with the inputs of the sensors 2, 4, 15, 15-a, 27, 29, 32, 35, 37, 40, 44, 42, 48, 46, 50 and outputs of the valves 3, 4-b, 16, 15-b, 30, 33, 36, 38, 41, 45, forming the loops. When the controllers manage the processes of obtaining caprolactam is carried out by the operator manually. The control mode upon receipt of the caprolactam is as follows. - set the overall load on caprolactam, - set the ratio of benzene and phenol in the reactor hydrogenation; - specify the distribution of cyclohexanone along the lines of oxymorphine (first and second line); - ask the shipment of crystalline and liquid caprolactam consumers; - adjust the cost of benzene and phenol and operational parameters on the blocks hydrogenation, oxidation, dehydrogenation and rectification; - adjust the costs and operational parameters of cyclohexanone and has synthesis on line oxymorphine; - adjust the cost of oleum, alkali and trichloroethylene and operational parameters at the stage of isomerization and conversion cyclohexasiloxane in blocks rearrangements in caprolactam; - adjust the cost of crystalline and liquid caprolactam for the consumer. The mass ratio of the benzene-phenol, the distribution of cyclohexanone on Lin the pits of oxymorphine and shipment of caprolactam consumer support within 70:30 and 65:35%; 55:45 and 60:40% and 40:60 and 50:50%, respectively. Consider the numerical examples of the preparation of caprolactam. Example Specify the total load (controller 60) 20 t/h and distributed in a mass ratio of 15 t/h of benzene and 5 t/h of phenol using device 5 (valves 6, 7, 8, 9 are open, the valves 10, 11 are closed). The pump 1 through the control loop 2, 3 serves heated benzene in the amount of 15 t/h and hydrogen 60 kg/t (path 2A, 3A) to the hydrogenation unit 4 into the tube space. Depending on the feed coal or petroleum benzene set temperature of 160°C, which is adjustable depending on the concentration of sulfur trace (temperature sensors, condensers for heat dissipation, the selectors to limit values for benzene and hydrogen is conventionally not shown). Next cyclohexane serves to block the oxidation of 12 (depicted one reactor, other reactor not shown), which is served by pipeline oxygen in the air. The main oxidation product is cyclohexanone-oxidat. An important parameter is the stay of the mixture in the reactor and the temperature. The output product - oxidat contains cyclohexanol and other impurities, which remove the temperature control in the range of 180-200°C or residence time in the reactor when the load changes. To reduce losses at the stage of oxidation of the corrected temperature of the process is up to 190°C. Further oxidat directed to the rectification unit 13, 19 (together with the thread of the block 18) to obtain cyclohexanone rectified. The pump 14 through the control loop 15, 16 serves heated phenol in an amount of 5 t/h and hydrogen 60 kg/g (contour 15-a, 15-b) to the hydrogenation unit 17 (shown one reactor hydrogenation) in the pipe space (condensers, evaporators, temperature sensors and pressure of steam, the selectors for the limiting values of phenol conventionally not shown). The set temperature of 175°C. to increase the reaction rate, the selectivity of the process and to exclude cyclohexane, water, cyclohexane and other impurities. Received heated cyclohexanol sent to the dehydrogenation unit 18 (shown one reactor, heat exchangers, refrigerators not shown). The dehydration occurs at a temperature of 400°C and a pressure of 0.7 MPa. For cleaning cyclohexanol (anon) and other impurities produced by the circulation of pump 20 to the dehydrogenation unit 18 unit rectification 19 pump 20 with a multiplicity of 20-30. Then the mixture flows from the blocks 12 and 18) served on blocks rectification 13, 19 to remove impurities (esters, acids, cyclohexanol and cyclohexanone). Threads cyclohexanone-rectified with the rectification unit 13, 19 control on laboratory data and sent to the distribution device cyclohexanone (anon) 21 (valves 22 and 23 are opened, and the vent is whether 24, 25 closed) and through the stirring tank 26 and rashtchy 27 - units oxymorphine. On the first line serves 55% wt. and on the second line of 45% (10,7 t/h, of 8.95 t/h). Routed through the control loop 29,30 anon in the amount of 10.7 t/h on the unit oxymorphine 28, which also served ammonia water in the amount of 2.34 t/h (loop not shown) and hydroxyanisole (GUS) from the block 34 through the control loop 35, 36 of 44 t/h Reaction oxymorphine is carried out in two stages. The first stage creates excess anon, and at the second stage, excess gas with recirculation of the reactants. An important parameter is the pH environment of the reagents, which is maintained in the range of 4.5 to 5.8 with gaseous ammonia. Depending on the concentration of moisture more than 0.2% of the specified 4,5% additionally served on the second stage gas. Distillation of anon and water, oparka of ammonium sulfate and the drying cyclohexasiloxane (oxime) removing the ammonium sulfate, which is returned to production, not shown. Then the oxime through mechanical cleaning filters in the amount of 11.7 t/h (composition for 95.3 wt.% the oxime, and 4.5% water and 0.2% anon) is sent to the isomerization of the oxime to caprolactam at block 39. Two-stage rearrangement is carried out in an environment of oleum (23 wt.%), supplied through the control loop 40, 41. The reaction is carried out at a temperature of 100°C and atmospheric pressure (recirculate the mixture, refrigerators, shut-off valve not shown). An important parameter is the mixing ratio of the oxime-oleum", the temperature and output of the pH (up to 60 wt.%), determined by the sensor 42, or on the testimony of the laboratory analysis. Depending on the indications acidity adjusting the flow of oleum to improve the quality of caprolactam by optical density. For example, to 0.25 t/h when the pH value of 57 wt.%. Next sulphate caprolactam is neutralized in the reactor 47, which serves ammonia water in an amount of 5.1 t/h and pH control environment based on the sensor readings 48 (the pH is maintained within 59-61 wt.%) In the settling tank top organic layer contains a lactam oil (60-70 wt.% caprolactam) and 38-42% of ammonium sulfate, which is returned to production on oxymorphine and in the workshop production of crystalline ammonium sulfate. The mixture is then directed to the extraction with trichloroethylene (TAE) to 8 kg/h and alkali to 0.14 kg/t to improve the quality of caprolactam (stage conventionally not shown). The resulting caprolactam in the amount of 11.7 t/h to send the pump 51 into the container 53. Similar processes occur when applying anon on the second line of oxymorphine (45% of the specified load - 8,95 t/h) in blocks 31, 34, 43, 49 using circuits 32 and 33; 37 and 38; 44 and 45; and sensor acidity 46 and pH IU the RA 50. The device 21 is in the same position as when connecting the first line oxymorphine. The resulting caprolactam in the amount of 9.9 tons/h pump 52 is directed into the container 53, where it is stirred and send in the amount of 21.6 t/h on device 54 switching crystalline caprolactam liquid caprolactam. The distribution of caprolactam depends on the consumer. When storing caprolactam less than 15 days from the tank 56 is directed caprolactam in the number 8,64 t for transportation in tanks (valves 57, 59 are opened, and the valve 58 is closed). When storing caprolactam more than 15 days sent caprolactam in the hub of the crystalline caprolactam 55 (valves 57 and 58 are opened, and the valve 59 is closed). The hub represents the capacity of the drum where it is cooled to a temperature of 60°C and in the form of crystals comes packaged in polyethylene bags to the consumer in the amount of 12,96 so Thus, combining the methods of oxidative method of obtaining caprolactam from benzene and the method of obtaining caprolactam by phenolic scheme and adjusting modes at the stage of hydrogenation of benzene and oxidation during the hydrogenation of phenol, dehydrogenation of cyclohexanol, followed by distillation, as well as reducing the concentration of water at the stage of oxymorphine with subsequent correction for submitting oleum on the stage of rearrangement achieve p is increasing its productivity with the desired properties of caprolactam. This increase performance up to 20%, reduce loss of caprolactam to 10% and reduce the amount of microtraces ready caprolactam. The table below shows the indicators of the quality of caprolactam and performance modes for the load 22 t/h, when the mass ratio of the benzene-phenol 70:30%, the load distribution along the line of oxymorphine 55:45% and shipment to the customer 40:60%.
As can be seen from the table, superior quality indicators and increased plant capacity. The economic effect is up to 30 million rubles per year. The method introduced in 2007 JSC "KuibyshevAzot". 1. The method of controlling the manufacture of caprolactam from benzene, held in installation with one production line, including units hydrogenation of benzene with hydrogen, the oxidation of cyclohexane with oxygen, the rectification of cyclohexanone, oxymorphine hydroxylaminopurine, rearrangement cyclohexasiloxane in caprolactam, neutralization of ammonia and a mixture of caprolactam, which are interconnected pumps, pipelines with sensors and valves for adjusting benzene, hydrogen, cyclohexanone, has synthesis, is the Jum, sensor acidity and pH meter caprolactam, wherein the installation further comprises a second production line for the production of caprolactam from phenol, including units hydrogenation of phenol by hydrogen in the dehydrogenation of cyclohexanol with a circuit, comprising: a pump unit dehydrogenation of cyclohexanol unit rectification of cyclohexanone - pump, the rectification unit cyclohexanone oxymorphine hydroxylaminsulphate, rearrangement cyclohexasiloxane in caprolactam and neutralize ammonia, interconnected pumps and pipelines with sensors and valves expenses phenol, hydrogen, has synthesis, oleum, sensors measure of the acidity and pH meter caprolactam, and also contains a device ratio benzene-phenol, United pipe with blocks hydrogenation of benzene and phenol, block oxidation and dehydrogenation unit; a distribution device cyclohexanone units oxymorphine, United pipe with blocks rectification and through the tank mixture of cyclohexanone with blocks of oxymorphine; a switching device of the crystalline caprolactam liquid caprolactam, United pipeline with mixer caprolactam and hub crystalline caprolactam and capacity liquid caprolactam is, ask your overall workload caprolactam, the ratio of benzene-phenol in the hydrogenation reactor, the distribution of cyclohexanone units oxymorphine, shipment crystalline and liquid caprolactam to the consumer and are adjusting accordingly the cost of benzene, phenol, hydrogen units hydrogenation, oxidation, dehydrogenation and rectification, the cost of cyclohexanone has synthesis on the power oxymorphine, oleum on the block rearrangement impact on the corresponding valve. 2. The method according to claim 1, characterized in that the hydrogenation of benzene with hydrogen is carried out in two serially connected reactors and adjust the process temperature in the range of 160-230°C and a pressure of 0.8 MPa with recirculation otdelochnih gases. 3. The method according to claim 1, characterized in that the hydrogenation of phenol with hydrogen is carried out in two serially connected reactors and adjust the process temperature in the range of 150-180°C. and a pressure of 0.75 MPa with recirculation otdelochnih gases. 4. The method according to claim 1, characterized in that the oxidation of cyclohexane with oxygen is carried out in two blocks of four reactors and adjust the process temperature in the range of 145-160°C and a pressure of 0.75 MPa. 5. The method according to claim 1, characterized in that the dehydrogenation of cyclohexanol is carried out in five reactors and adjust the process temperature in the range of the Ohe 370-450°C and pressure up to 0,065 MPa. 6. The method according to claim 1, characterized in that the rectification of cyclohexanol and cyclohexanone is carried out in two reactors for the production of cyclohexanone - rectified and adjust the process temperature in the range of 120-140°C and pressure up to 0.25 MPa and a ratio of circulation to 20-30. 7. The method according to claim 1, characterized in that oxymorphine cyclohexanone by hydroxylaminsulphate conducted in countercurrent system with the faucets in the two reactors at a temperature of 55-80°C and a pressure of 0.1 MPa. 8. The method according to claim 1, characterized in that the rearrangement cyclohexasiloxane in caprolactam is carried out in the reactor at a temperature of 90-110°C and a pressure of 0.1 MPa and correct filing of oleum depending on acidity. 9. The method according to claim 1, characterized in that the neutralization of the sulfate caprolactam is carried out in the reactor ammonia water to 15 wt.% at a temperature of 50°C and a pressure of 0.1 MPa.
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