СПИСОК ИСПОЛЬЗОВАННЫХ ИСТОЧНИКОВ. 2. ГОСТ 12.1.005-88 Гигиенические требования к микроклимату производственных помещений
1. ГОСТ 12.0.003-74 “ССБТ. Опасные и вредные факторы. Классификация”.
2. ГОСТ 12.1.005-88 Гигиенические требования к микроклимату производственных помещений.
3. ГОСТ 12.1.004–76 и ГОСТ 12.1.010 – 76. Основы противопожарной защиты предприятий.
4. ГОСТ 50923-96 Дисплеи. Рабочее место оператора. Общие эргономические требования и требования к производственной среде. Методы измерения.
5. ГОСТ 12.2.032-78 Рабочее место при выполнении работ сидя. Общие эргономические требования.
6. СанПиН 2.2.2.542-96 “Гигиенические требования к ВДТ, ПЭВМ и организация работы”.
7. СанПин 2.2.4/2.1.8.562-96 Шум на рабочих местах, в помещениях жилых, общественных зданий и на территории жилой застройки.
8. СанПиН 2.2.548-96 Гигиенические требования к микроклимату производственных помещений.
9. СНиП 23-05-95 Естественное и искусственное освещение.
10. СН 512-78 Инструкция по проектированию зданий и помещений для электронно-вычислительных машин.
11. СН 245-71 Санитарные нормы проектирования промышленных предприятий.
12. Охрана окружающей среды /Под ред. С. В. Белова. – М.: Высш. шк., 1991 г.
13. Безопастность жизнедеятельности /Под ред. С. В. Белова. – М.: Высш. шк., 1999 г.
14. Проектирование систем автоматизации ТП. Справочное пособие/ Под общ. ред. Клюева А.С.-М.:Энергоиздат, 1990г.
15. Деменков Н.П. Разработка АСУ ТП на базе промышленных контроллеров и систем оперативного управления/ Приборы и системы управления, №3, 1998г.
16. Техническая документация по микропроцессорному контроллеру Delta V фирмы Emerson.
17. Технологический регламент управления синтезом катализатора.
18. Лекции по дисциплине «Автоматизированные системы управления».
Приложение 1. DESCRIPTION OF AUTOMATION OBJECT
Description of technology of synthesis of magnesium-bearing alloy
The technological process of synthesis magnesium-bearing alloy includes:
preparation for synthesis;
dispension of solutions of organomagnesium combination and tetraethoxycilane (TEOS) in a reactor in dibutyl ether medium (DEM);
heat treatment of a reaction mixture;
sluicing a hard product;
modifying a hard product by spirits and titan: serial processing by the solution of ethyl spirit and then by the solution of tetraethoxytitane (TEOT) in heptane;
sluicing magnesium-bearing alloy;
unloading the magnesium-bearing alloy from the reactor;
preparation for following synthesis.
Preparation for synthesis
The synthesis of magnesium-bearing alloy is carried out in the reactor (pos. Р-301) or in the reactor (pos. Р-302). The reactor (pos. Р-301) represents a vertical cylindrical device with a jacket for heating and cooling equipped with a propeller mixer. The reactor is equipped by two movable siphons (one with the filter, another without the filter) for pressing mother water and sluicing solutions in the mode of filtration or by decantation. Also the reactor is equipped with a device for sluicing of dibutyl ether, "shower", and a run-down box, and also equipped with reflective partitions (4 pieces) for the reduction of spraying and suppressing the funnel formed at the rotation of a mixer.
The reactor (pos. Р-302) represents a vertical cylindrical device with a jacket for thermostatting and is equipped similarly to the reactor (pos. Р-301), but it does not have the run-down box, and movable siphons are established on the same connecting pipe alternately.
For the maintenance in the jackets of reactors of the given temperature in devices a coolant is passed, which is diathermic oil that heats up or is cooled in the unit of thermostatting. The introduction of direct "hot" or "cold" oil in the jacket of the reactor (pos. Р-301 (Р-302)) is carried out by switching over into the corresponding position the three-way valve, established at the input in the jacket of the reactor, with the warning alarm of the position of the valve. And to each of these positions of the valve on an input in a jacket of reactor there corresponds the position of the three-way valve, established on an exit from the jacket of reactor that allows "hot" oil to return in "pos. Е-602/2", capacity for the storage of "hot" oil and "cold" oil to return in "pos. Е-602/1", capacity for the storage of "cold" oil.
Before the beginning of the synthesis of the magnesium-bearing alloy, the drained raw material arrives in corresponding capacities to the synthesis unit.
A calculated quantity of heptane is given by the pressure of nitrogen through the pipe of overpressing into a container (pos. М-311), representing a vertical cylindrical device with capacity 0,35 m3. Also in a jacket is passed "hot" oil for heating heptane before introduction sluicing of magnesium-bearing alloy in the reactor (pos. Р-301 (Р-302)). The introducnion of heptane from "pos. М-311" for the further conducting technological process is carried out through the bottom connecting pipe on the pipeline.
A calculated quantity of dibutyl ether is given by the pressure of nitrogen through the pipe of overpressing into a container (pos. М-313), representing the vertical cylindrical device with capacity 0,35 m3. The introduction of an aether from "pos. М-313" for the further conducting technological process is carried out through the bottom connecting pipe on the pipeline.
A calculated quantity of chlorbenzene is given by the pressure of nitrogen through the pipe of overpressing into a container (pos. М-312), representing a vertical cylindrical device with capacity 0,4 m3. The introduction of chlorbenzene from "pos. М-312" for the further conducting technological process is done through the bottom connecting pipe on the pipeline.
A calculated quantity of organomagnesium combination is given by the pressure of nitrogen through the pipe of overpressing into a container (pos. М-314), representing a vertical cylindrical device with capacity 0,25 м3. The introduction of organomagnesium combination from "pos. М-314" for the further conducting on of the technological process is done through the bottom connecting pipe on the pipeline.
The solution of TEOS in dibutyl ether is prepared in capacity (pos. М-315), representing a vertical cylindrical device with a mixer and capacity 0,15 m3. For the preparation of solution of TEOS into a container (pos. М-315) alternatively are loaded calculated quantities of dibutyl ether and TEOS.
Composite TEOS and DEM is mixed for not less than 5 minutes.
The introduction of the solution TEOS in dibutyl ether from "pos. М-315" for the further conduction of technological process is done through the bottom connecting pipe on the pipeline.
Before the synthesis the reactor (pos. Р-301 (Р-302)) is washed out by dibutyl ether through "shower" which in necessary quantities is given from "pos. М-313", or from "pos. Е-103/2", or through the pump (pos. Н-103). The mass fraction of moisture in dibutyl ether which should be no more than 5 ppm is controlled in advance. In the reactor (pos. Р-301) through "shower" dibutyl ether in number of 500 liter is given, into the reactor (pos. Р-302) - 130 liter. Then the mixer is switched on a reactor is thermoestablished at temperature (70-80) оС. Washing is carried out not less than 20 minutes and then the temperature in the reactor is reduced to less than 40 оС. The DEM is unloaded by the pressure of nitrogen in "pos. Е-306" through the reactor bottom through the cutoff valve (pos. HSA-306), where it is stored for the preparation of the next synthesis and is used repeatedly for reactor washing. The introduction of DEM from capacity (pos. Е-306) is carried out through the counter (pos. FQIRSAH-306/1) with the automatic closing of a cutoff valve (pos. HSA-306/1). The capacity (pos. Е-306) represents the vertical cylindrical device with capacity 1 м3, equipped with the index of level of type "Klinger".
After the reactor washing, there is possibility of the removal of the sedimentation of the catalyst from "pos. Е-306" through the pump (pos. Н-305) in the collection-container of mother waters (pos. Е-307) is provided, it is possible to have the recycling of dibutyl ether from "pos. Е-306" through the pump (pos. Н-305) with return to (pos. Е-306).
The pump (pos. Н-305) works in two operating modes:
1. "Work with pos. Е-306"
recycling dibutyl ether with return to "pos. Е-306";
clearing "pos. Е-306" from DEM with the sedimentation of the magnesium-bearing alloy in "pos. Е-307";
2. "Work with pos. Е-307"
recycling mother waters with return to "pos. Е-307";
clearing "pos. Е-306" from DEM with the sedimentation of the magnesium-bearing alloy in "pos. Е-307";
clearing "pos. Е-307" on external installation.
After washing, the reactor (pos. Р-301 (Р-302)) is ventilated by nitrogen during 5 minutes. In the reactor, which has been washed out by dibutyl ether and cleaned out by nitrogen, from capacity (pos. М-313) a certain calculated quantity of DEM is given then pressure of nitrogen is dumped to 0 МPascal and ventilation is finished. The system of temperature’s regulation is switched on and the reactor is thermoestablished at the included mixer, at the adjusted temperature (5-35) оС during (20-30) minutes.
From the container (pos. М-313) in the miniamalgamator (pos. МС-301 (МС-302)) dibutyl ether is given before the liquid appearance in the run-down box (pos. FS-301, FS-302 (FS-305, FS-306)), then the cutoff armature between miniamalgamator and run-down box is closed to avoid uncontrollable ingress of solutions in the miniamalgamator.
The pipeline on which dispensing of organomagnesium combination is executed, is filled with a dispensing component before its appearance in the run-down box (pos. FS-302 (FS-306)).
The pipeline on which the dispensing of solution TEOS is executed, is filled by dispensing component before its appearance in a run-down box (pos. FS-301 (FS-305)).
Stop valve after run-down box is closed.
After filling in miniamalgamator and pipelines, in a jacket (pos. МС-301 (МС-302)) and the heat exchanger (pos. Т-301 (Т-302)) the coolant is given and the temperature (5-10) оС is reached.
The miniamalgamator (pos. МС-301 (МС-302)) represents a vertical device with capacity 0,000085 m3 with a mixing device which having the possibility of regulation of the number of turns of a shaft from 150 to 1000 turn/minute. The device is supplied by a jacket for cooling. The control of work of a mixer (pos. HСSA-301/1м (HСSA-302/1м)) is provided.
The heat exchanger (pos. Т-301 (Т-302)) is the vertical cylindrical device with two coils. The surface of heat exchange for organomagnesium combination is 0,41 m2, while the surface of heat exchange for TEOS is 0,23 m2.
Stage of dispensing
Mixers in the reactor (pos. Р-301 (Р-302)) and the miniamalgamator (pos. МС-301 (МС-302)) are switched on and a necessary speed of mixing is established. The stop valve is opened on the pipelines, which feed reagents in miniamalgamator and a line, connecting miniamalgamator with the reactor. Dosing pumps (pos. G-301, G302) are switched on and the dispensing of solutions organomagnesium combination (from pos. М-314) and TEOS (from pos. М-315) is executed. The correlation of flow organomagnesium combination to TEOS should be equal 2:1.
Depending on the modification of the received magnesium-bearing alloy, the duration of dispensing time changes from 2 to 12 hours and more. The time of preliminary mixing in the miniamalgamator is from 8 to 60 seconds. It is defined by the capacity of the miniamalgamator and the speed of dispensing the components. The speed of dispensing the solutions МОС and TEOS during synthesis is kept to be a constant, as well as keeping the established correlation of volume speeds.
During the dosing of components in the reactor (pos. Р301 (Р-302)) the constant temperature of (35-40) оС is held.
In the process of dispensing the speed of mixing in the reactor increases (1,5-2) times. The quantity of turns of the engine of the mixer (pos. HCSA-301m (HCSA -302m)) is regulated automatically by means of the frequency converter (pos. LIRCSAHL-301 (LIRCSAHL-302)) depending on the change of liquid level in the reactor.
Stage of heat treatment
After the dispensing termination, the heat treatment of the reactionary mix in the reactor (pos. Р-301 (Р-302)) is executed on a following mode:
the reactionary mix is kept during 0,5 hour at the temperature of dispensing (35-40) оС;
the temperature is evenly raised from that of dispensing (35−40) оС to (60-70) оС during (0,5-2) hours;
endurance at (60-70) оС during (1-2) hours.
Stage of washing
Upon the termination of the heat treatment, the mixing in the reactor (pos. Р-301 (Р-302)) is stopped (the mixer is stopped) and the sedimentation of the mixture in the reactor is executed during (45-60) minutes.
The liquid phase is deleted from the reactor in the collection of mother waters (pos. Е-307), representing a vertical cylindrical device with capacity 6,3 m3.
The removal of the liquid phase from the reactor (pos. Р-301 (Р-302)) is executed step by step, at gradual immersion of a mobile siphon up to appearance of the suspension of the magnesium-bearing alloy in the run-down box (pos. FS-303 (FS-307)).
The possibility of removal of mother waters from "pos. Р-301 (Р-302)" is provided by means of a mobile siphon with a filter. In this case the sediment of suspension of the magnesium-bearing alloy is not executed, the reactor mixer is switched off, and the mobile siphon falls to the bottom a reactor. After that the mother waters are moved through the filter, which has been built in the siphon by the pressure of nitrogen in "pos. Е-307". The control of the process of the moving is executed in accordance with the run-down box (pos. FS-304).
Then quadruple washing of the magnesium-bearing alloy is executed at temperature (50−60) оС. For this purpose in "pos. М-311" the necessary quantity of drained heptane is accepted. "Hot" oil is moved to the jacket (pos. М-311) and the heptane is warmed up to temperature (50-60) оС. The warmed heptane is moved into the reactor through the bottom (pos. М-311). The reactor mixer is switched on, the temperature (50−60) оС is established and sluising during 20 minutes is executed. Then mixing is stopped, the sedimentation is executed during (30-40) minutes, and then the decanting of the washing solution takes place through a mobile siphon, through a run-down box (pos. FS-303 (FS-307)) in "pos. Е-303". The possibility of removal of the washing solution from the reactor is provided through a mobile siphon with a filter. In this case the sedimentation of the suspension of the magnesium-bearing alloy is not executed, the reactor mixer is switched off, and the mobile siphon falls on the bottom of the reactor. After that mother waters through the filter, which has been built in the siphon, are moved by the pressure of nitrogen in "pos. Е-303".
The washing operation repeats three more times. The washing solution after the first and second washing goes in "pos. Е-303", and after the third and fourth washings - in "pos. Е-304/1" and is used as the washing solution of the first and second washing for the next synthesis of the magnesium-bearing alloy. The washing solution comes back into the reactor by the pipeline through the counter (pos. FQIRSAH-304) with a task possibility of giving the necessary quantity of a solvent with automatic closing cutoff valve (pos. HSA-304) at the achievement of the adjusted quantity on symbolic circuit ASU TP.
In case of using the returned washing solutions as solvent for the first and second washing, for the third and fourth washing pure solvent from "pos. М-311" or from "pos. Е-101/2" is used.
The possibility of a ventilating by nitrogen the pipeline of introduction of returnable washing solutions through bypass (pos. FQIRSAH-304, HSA-304) in "pos. Е-303, Е-304/1, Е-304/2" is provided.
The collection-container of washing solutions (pos. Е-303) represents a vertical cylindrical device capacity with 1 m3, intended for gathering the washing solution after the first and second washing of the magnesium-bearing alloy.
Possibility of clearing of washing solutions (pos. Е-303) in collection-containerthrough the pump (pos. Н-304) is provided on external installation, and also it is possible to have a recycle of the washing solution from "pos. Е-303" through the pump (pos. Н-304) with return to "pos. Е-303".
The collection-container of washing solutions (pos. Е-304/1) represents a vertical cylindrical device with capacity 1 m3, intended for gathering of washing solution after the third and fourth washing of the magnesium-bearing alloy with the following return to "pos. Р-301 (Р-302)" as a solvent for the first and second washings of the magnesium-bearing alloy of the next synthesis.
There is a possibility of clearing the washing solutions (pos. Е-304/1) in collection-container through the pump (pos. Н-304) on the external installation, and also it is possible to recycle the washing solution from "pos. Е-304/1" through the pump (pos. Н-304) with return to "pos. Е-304/1".
The pump (pos. Н-304) works in three modes:
1. "Work with pos. Е-303":
recycle of a washing solution with return to "pos. Е-303";
return of a washing solution to the reactor (pos. Р-301 (Р-302));
clearing "pos. Е-303" on external installation.
2. "Work with pos. Е-304/1":
recycle of a washing solution with return to "pos. Е-304/1";
return of a washing solution to the reactor (pos. Р-301 (Р-302));
clearing "pos. Е-304/1" on external installation.
3. "Work with pos. Е-304/2":
recycle of a washing solution with return to "pos. Е-304/2";
return of a washing solution to the reactor (pos. Р-301 (Р-302));
clearing "pos. Е-304/2" on external installation.
Stage of activation
The activation stage is done for the preparation of the activated magnesium-bearing alloy.
In a laboratory of department 502, ethyl spirit is absolutised, and airtight calculated quantities of ethyl spirit are loaded under nitrogen into a portable container (pos. Х-301) preliminary ventilated by nitrogen, and representing a portable vertical vessel with capacity 0,002 m3. The container is equipped by a stationary siphon and connecting pipe with a stop valve for connecting through a flexible hose the pipelines of ventilationand nitrogen.
The reactor (pos. Р-302 (Р-402)) is used in the synthesis of the magnesium-bearing alloy in "pos. Р-301 (Р-302)" for the preparation of ethanol and TEOS solutions and dispensing activating solutions in the reactor with the magnesium-bearing alloy through the pump (pos. Н-303).
In the reactor (pos. Р-302 (Р-402)) is given the calculated quantity of heptane from "pos. М-311" or a returnable washing solution from "pos. Е-304/1". The ethanol from "pos. Х-301" is passed over through a flexible hose by nitrogen in "pos. Р-302 (Р-402)"; the mixer is switched on, and the mix is mixed for not less than 5 minutes.
After executing the third washing of the magnesium-bearing alloy in a reactor (pos. Р-301 (Р-302)) the additional portion of heptane from "pos. М-311" or a returnable washing solution from "pos. Е-304/2" is loaded. The system of temperature regulation is turned on and the reactor contents, while being mixed, are thermoestablished at temperature (10-15) оС during 0,5 hour. Then while mixing the suspension of the magnesium-bearing alloy in the reactor (pos. Р-301 (Р-302)) from "pos. Р-302 (Р-402)" through a diaphragm dosing pump (pos. Н-303) the ethanol solution is given. Dispensing is executed at a constant temperature during 1 hour. After the dispensing termination, the suspension of the magnesium-bearing alloy is carried out at (10-15) оС during 0,5 hour.
In the laboratory of department 502 airtight under nitrogen in the portable container (pos. Х-302), preliminary is ventilated by nitrogen, calculated quantities of TEOT are loaded.
The container (pos. Х-302) represents a portable vertical vessel with capacity 0,007 m3, equipped a stationary siphon and a connecting pipe with a stop valve for connection through a flexible hose of pipelines ventilation and nitrogen.
In the reactor (pos. Р-302 (Р-402)) a calculated quantity of heptane is passed from "pos. М-311" or a returnable washing solution from "pos. Е-304/2". After the washing solution from "pos. Е-304/2" has been sent, the pipeline of the returnable washing solution is ventilated by nitrogen from the reactor (pos. Р-301 (Р-302, Р-402)) through bypass (pos. FQIRSAH-304, HSA-304) in "pos. Е-304/2".
TEOT from "pos. Х-301" through a flexible hose is pressed over by nitrogen in reactor (pos. Р-302 (Р-402)), the mixer is switched on, and the mix is mixed for not less than 10 minutes.
While mixing the suspension of the magnesium-bearing alloy in the reactor (pos. Р-301 (Р-302)) from the reactor (pos. Р-302 (Р-402)) through a diaphragm dosing pump the solution of TEOT is given. Dispensing is executed at the constant temperature (10-15) оС during 1 hour.
After the termination of dispensing the solution TEOT, the even raising of temperature, 0,3 оС in a minute, is executed in the reactor (pos. Р-301 (Р-302)) from (10-15) оС to 30 оС during 1 hour.
Further, the reactionary mix is maintained during 2 hours at 30 оС.
Then with the switched-off mixer is executed, the sedimentation of the magnesium-bearing alloy during (30-40) minutes. After the sedimentation of the suspension of the magnesium-bearing alloy and decanting the liquid phase from the reactor (pos. Р-301 (Р-302)) into collection-container (pos. Е-303), the magnesium-bearing alloy is washed once by heptane at 30 оС (for the washing there is used pure heptane from "pos. Е-311"). After the sedimentation of suspension the washing solution is deleted in the collection (pos. Е-304/2), also is used repeatedly for the preparation of the suspension of the magnesium-bearing alloy for activation in "pos. Р-301 (Р-302)" and preparations of activating solutions in "pos. Р-302 (Р-402)".
The possibility of removal of washing solutions from "pos. Р-301 (Р-302)" is provided through a mobile siphon a filter. In this case the sedimentation of the suspension of the magnesium-bearing alloy is not executed, the reactor mixer is switched off and the mobile siphon falls to the bottom of the reactor. After that the washing solution through a filter, which has been built in a siphon is pressed over by nitrogen in "pos. Е-303" or in "pos. Е-304/2".
The collection-container of washing solutions (pos. Е-304/2) represents a vertical cylindrical device with capacity 1 m3, intended for gathering the washing solution after washing of the activated magnesium-bearing alloy with the following return to "pos. Р-301 (Р-302, Р-402)" as a solvent for the preparation of activation solutions and preparation of suspension of the magnesium-bearing alloy at the stage of activation of the next synthesis.
The possibility of clearing of "pos. Е-304/2" through the pump (pos. Н-304) in collection-container of washing solutions on external installation is provided, and also it is possible to have the recycle of the washing solution from "pos. Е-304/2" through the pump (pos. Н-304) with return to "pos. Е-304/2".
With the synthesis of the activated magnesium-bearing alloy, only the third washing at the stage of synthesis of the magnesium-bearing alloy is used again (through the container (pos. Е-304/1) it goes on the first washing of the magnesium-bearing alloy in the next synthesis). Washing of the activated magnesium-bearing alloy is used again in the next synthesis, which is gathered in the container (pos. Е-304/2) and is used for the preparation of suspension of the magnesium-bearing alloy in the reactor (pos. Р-301 (Р-302)) at the stage of activation and preparation of ethanol and TEOT solutions in "pos. Р-302 (Р-402)".
Washing with pure heptane "pos. Е-303, Е-304/1, Е-304/2" is provided as a variation.