KR20220021177A - Source-pitch continuous charge and reformed pitch continuous discharge of Pitch Reformer - Google Patents

Abstract

Pitch is the last remaining viscoelastic polymer after distilling fuel gas and fuel oil from coal or crude oil. When the volatile substances contained in the pitch are removed, the mechanical bonding strength (tensile modulus) is several dozen times that of iron, and the pitch is reformed as a precursor to obtain valuable industrial materials such as carbon fiber, carbon heat sink, carbon insulation foam material, etc. The conventional pitch reforming apparatus wastes a lot of energy and manpower because the pitch is filled in a reforming vessel, heated to a high temperature to remove volatile substances, and cooled to a constant temperature to be discharged and reformed by opening the vessel and refilling the raw material pitch. The specific gravity of pitch increases as volatiles are removed, and when heat is consumed to evaporate volatiles, the temperature rises only when a constant evaporation temperature is maintained, and all volatiles are removed. And when the pitch suddenly comes into contact with high temperatures, the volatile material is carbonized before evaporation and becomes a solid. Solidified carbon does not dissolve even at a temperature of 3000 degrees Celsius, nor does it dissolve in solvents such as toluene and quinoline. The present invention relates to a technology of a reforming means, which can significantly save energy and manpower by continuously injecting and continuously discharging the modified pitch by continuously injecting the raw pitch without opening a reforming container using the physical properties of the pitch, and a pitch continuous reforming device which implements the means.

Description

Continuous supply of raw pitch and continuous discharge of reformed pitch of a pitch reformer {Source-pitch continuous charge and reformed pitch continuous discharge of Pitch Reformer}

The precursor pitch is obtained by evaporating and removing volatile substances (Volatilization Material) from the raw pitch. The space where volatile substances contained in the raw material pitch are evaporated and removed must be a high-temperature, airtight space. As such, it relates to a technique for continuously injecting raw material pitch into a high-temperature airtight space to perform heat treatment reforming and continuously discharging the modified pitch.

Pitch is a precursor to industrial materials such as carbon fiber, carbon heat sink, and carbon insulating foam, and various volatile substances contained in the precursor pitch that affect the mechanical bonding strength, electrical conductivity, thermal conductivity, and density of these materials Evaporation temperature varies with pressure and ranges from 350°C to 440°C at atmospheric pressure.

In addition, when the pitch is suddenly exposed to high temperature, it becomes a solid that does not melt even at a high temperature of 3000℃ by coking before the volatile substances evaporate. It is also insoluble in strong solvents such as toluene and quinoline.

Therefore, the device for reforming pitch into a precursor must be controlled so that unstable fluctuations in temperature do not occur to minimize the generation of substances that do not dissolve in solvents such as toluene or quinoline, and also products manufactured using pitch as a precursor The heat treatment temperature should be changed according to the

And unlike metals, pitch does not expand in proportion to temperature, but rather decreases in volume as the temperature increases, so the specific gravity increases as the temperature increases.

It relates to an apparatus for implementing means and means for modifying the pitch into a precursor by using the physical properties of the pitch.

Conventionally, the raw material pitch for heat treatment is filled in a container in advance, the container lid is closed, and rubber or synthetic resin is placed between the container lid and the container body as an intervening material for airtightness.

Since the maximum operating temperature of rubber and synthetic resin is 300℃ or less, the temperature around the inclusions for airtightness of the upper opening/closing part should be 300℃ or less. should be heated to

Therefore, the container for evaporating volatile substances is lengthened up and down so that the upper airtight part and the lower heating part are separated by a certain distance, and in order to prevent the volatile substance vapor evaporated from the lower high temperature from condensing and falling in contact with the upper low temperature part, as shown in FIG. The volatile material vapor discharge pipe 114 is drawn into the evaporation vessel until it approaches the surface of the evaporating pitch solution, and a heater is placed on the outer circumferential surface of the discharge pipe to measure the temperature of the entire inner circumferential surface of the discharge pipe of the volatile substances contained in the pitch. By maintaining a temperature higher than the boiling point (Bubbling Point), the evaporated volatile material vapor came into contact with the low-temperature part of the upper part of the evaporation container and before condensing and falling, it was all discharged and separated through the high-temperature discharge pipe.

And the conventional pitch reformer opens the container for each reforming process, fills the raw material pitch inside the vessel, heats it to a high temperature, and heats it. When the heat treatment is completed, the airtight high temperature reforming atmosphere is destroyed and the reformed pitch is fluidized at a temperature (120). After cooling to -°C 150), the modified pitch was discharged, and the process of reforming by refilling the raw pitch was repeated. Therefore, a large amount of energy, time and manpower was wasted in each process.

In order to solve this conventional problem, the mass reduced as volatile substances are evaporated and removed without destroying the high-temperature, airtight reforming atmosphere in the reforming vessel and the raw material pitch as much as the mass emitted by reforming is sealed inside the vessel having a high-temperature reforming atmosphere. By using the characteristics of injecting raw material pitch into the furnace and the modified pitch increases in specific gravity as the temperature rises, the heat-treated pitch and the non-heat-treated pitch are automatically separated in the heat treatment container so that only the heat-treated pitch is discharged. It is a key technical task of the present invention to always maintain uniform properties of the precursor pitch.

The means to solve this technical problem is a solid at room temperature, and when the temperature is 100-130 ° C. by applying heat, it changes to a mesophase, and the pitch changed to a fluid solid (mesophase) is a raw material pitch injector 220 by earth gravity. As the screw flows into the evaporator and rotates, the pitch of the raw material is injected into the evaporation container and degassed, and when it is gradually heated and enters the evaporation container, the temperature and pressure match the pressure and temperature inside the evaporation container. The raw material pitch is injected into the evaporation container without affecting the pressure and temperature inside the evaporation container, and the raw material pitch injected into the evaporation container is stirred and mixed with the pitch under heat treatment, and the specific gravity increases as the volatile substances are removed by evaporation. do. So, the high-temperature pitch, which has increased specific gravity due to the removal of volatile substances, sinks downward by the earth's gravity.

The evaporation vessel for reforming the pitch using these properties of the pitch is lengthened up and down as shown in FIG. 3, and the pitch with increased specific gravity is ground down, and the temperature of the pitch with increased specific gravity also increases in proportion to the specific gravity, so it sinks If the temperature of the seated pitch is detected and the discharge flow rate is automatically adjusted according to the detected temperature and discharged, the reformed pitch and the non-reformed pitch can be automatically selected and discharged.

And without cooling the modified high-temperature pitch due to heat treatment, using the high-temperature heat-treated pitch as a raw material to directly supply the raw material pitch to an apparatus for manufacturing carbon fiber, carbon heat sink, and carbon foam is a solution to the problem of the present invention am.

As a solution to this problem, the raw material pitch is modified and the high-temperature precursor pitch is directly supplied to the manufacturing equipment using the pitch as a precursor, such as carbon fiber, carbon heat sink, and “carbon insulating foam”, so that a hermetic high-temperature atmosphere is created for every process. It does not consume the energy to form and the energy to heat the raw material pitch from room temperature and normal pressure to high temperature and high pressure, and has the effect of greatly saving the work process and manpower.

In addition, since the temperature and pressure inside the airtight container are arbitrarily adjusted, there is an effect that the physical properties of the product using the molecular crystal of the pitch as a precursor can be optimally improved.

Figure 1: Top development view of the evaporation vessel according to the invention
Figure 2: Bottom development view of the evaporation vessel according to the invention
Figure 3: Schematic diagram of an evaporation condensing device having a raw material injection device according to the invention.
Figure 4: Schematic diagram of an evaporation condensing device that is divided and connected according to evaporation temperature
Figure 5: The overall reformer configuration diagram
Figure 6: The entire piping of the reformer and control and measurement functions.
Figure 7 : Development view of high temperature fluid "automatic flow control valve"

The evaporation vessel of the device for carrying out the present invention is divided into an upper and a lower portion, and the upper airtight portion 203 and the lower heating portion are spaced apart from each other as in FIG. ), the heating element 201 is placed along the "outer peripheral surface of the lower heating part", and the heating element is wrapped with a "Ceramic Fiber Castable" that withstands high temperatures, then sintered and sintered on the outer peripheral surface of the "fibrous ceramic casting" Insulate with glass-wool.

Then, dig an O-ring groove in the flange at the upper end of the lower part that divides the evaporation vessel into upper and lower parts as shown in the “enlarged picture” of FIG. When (Fig. 2) is aligned and the clamp is tightened, an airtight evaporation space is formed as shown in Fig. 3 .

And the device for injecting the raw material pitch into the formed evaporation space is positioned so that the raw material pitch is injected into the area where the lower edge of the agitator wing is located as shown in FIG.

The raw material pitch injector 220 puts a hopper 210 for supplying a solid raw material pitch, puts a "raw material pitch preheater 211" under the hop, puts a "raw material pitch preheater 211" and an electric heater on the outer peripheral surface of the "raw material pitch preheater 211" By placing 212, the raw material pitch is melted at 100-130 ° C. and introduced into the raw material pitch injector 220, and the raw material pitch injector 220 is a cylindrical cylinder with a screw 223, an airtight device 222, and a screw driving motor 221. The raw material pitch is gradually heated as the screw driving motor is driven and the heating element 224 installed on the outer circumferential surface of the cylindrical cylinder is supplied with power and entered into the evaporation vessel inlet.

As the screw rotates, the raw material pitch closes while entering the evaporation vessel, and the non-condensing gas contained in the raw material pitch is discharged in the reverse direction according to the pressure difference in contact. diameter increases, and the “gap between screw and screw” becomes narrower, making the space into which the raw material pitch enters narrower.

And the discharge pipe for discharging the reformed pitch by evaporating and removing the volatile substances in the evaporation container is composed of a discharge pipe 230 and "discharge flow control valve 240", and according to the temperature sensed by the temperature sensor 231, " The discharge flow control valve 240" precisely controls the discharge amount.

The discharged pitch is discharged as a precursor of a material having a constant density, electrical conductivity, thermal conductivity, and bonding strength when the temperature sensed by the temperature sensor 231 always maintains a constant temperature, and the internal pressure of the container maintains a constant pressure .

So, in the upper part of the evaporation vessel, as shown in FIG. 1, a stirring device is installed in the center of the upper head plate 110, and several discharge pipes 114 are placed around the stirring device according to the size of the device, and at the upper end of the discharge pipe, a "steam outlet space ( 113)" and the volatile material vapor discharged through the discharge pipe is in contact with the upper low temperature of the "steam outflow space 113", so that the condensed solution does not flow into the evaporation vessel. Outflow space 113" to protrude higher than the floor.

And the discharge pipe 114 puts the heating element 115 along the outer circumferential surface, and after filling the circumference of the heating element with the insulating material 116, the exterior is sealed with a stainless steel plate that withstands high temperature.

And a temperature sensor 120 is placed at the upper end of the discharge pipe to sense the temperature of the exhaust steam, and the temperature detected by the temperature sensor 120 is supplied to the heating element 115 to keep it higher than the temperature of the steam evaporated inside the evaporation vessel. control the power In addition, the high-temperature volatile substance vapor evaporated from the raw material pitch does not condense even under high pressure so that it does not come into contact with the low-temperature part at the top. In order to fill the upper part of the evaporation container and prevent the vapor evaporated from the lower evaporation container from coming into contact with the upper low temperature part, a pipe 112 for injecting an inert gas and a valve are placed at the ends of the pipe line 112.

And a "rotation force detector 121" is placed between the output shaft of the "agitator driving motor 111" and the agitator blade driving shaft to measure the blade driving rotational force for stirring, and the measured rotational force increases in proportion to the rise in the liquid level of the stirred pitch solution. The signal of the rotational force immediately indicates the position of the pitch solution level rise. Therefore, it is possible to overcome the impossibility of having a pitch solution level detector inside the high-temperature and high-pressure evaporation vessel, and accurately detect the position of the pitch solution liquid level introduced therein.

As mentioned above, when pitch is suddenly exposed to high temperature, it is carbonized (coking) before volatile substances evaporate and becomes a solid that does not dissolve even at a high temperature of 3000°C and does not dissolve in strong solvents such as toluene or quinoline.

Since the evaporation temperature of the volatile substances contained in the pitch varies from 350 ° C to 440 ° C, the pitch solution heat-treated at high temperature is slightly out of the pressure difference.

When the raw material pitch preheater 210 is completely filled with the raw material pitch and the temperature is heated to 100-130°C by supplying power, the raw material pitch melts and becomes a fluid meso-phase and flows into the screw inlet of the raw material sebum injector, and the raw material pitch As the moving screw rotates the screw driving motor of the injector 220, the raw material pitch is injected along the screw blade toward the evaporation vessel 200, and the diameter of the screw drive shaft increases in proportion to the direction of the evaporation vessel, and the distance between the screw blade and the blade is It decreases toward the evaporation vessel. Therefore, as the raw material pitch rotates, the space in which the advancing raw material pitch stays is reduced, so the injected raw material pitch is closely adhered to form airtightness.

So, as shown in FIG. 5, the vacuum pump 500 is operated, and then the "non-condensed gas discharge ball valve 502" driven by air pressure is opened, so that the non-condensed gas in the evaporation condensing space of the device is discharged, so evaporation, condensation, and container With the pressure sensed by the "pressure transmitter (P)" that detects the internal pressure, the vacuum inside the container is confirmed, the "non-condensed gas discharge ball valve 502" valve is closed, and then the vacuum pump 500 is stopped.

When the screw driving motor 221 of the raw material pitch injector 220 is driven at a constant speed, power is supplied to the electric heater 225, and the power supplied at this time is at a temperature of 100-130° C. at which the raw material pitch can continuously maintain fluidity. The raw material to be injected reaches the entrance of the evaporation vessel equipped with the "injected raw material pitch temperature sense 226" and the raw material to be injected in contact with the "injected raw material pitch temperature sense 226" When the temperature of the pitch is sensed, the power is advanced to the heating element 201 so that the temperature sensed by the temperature sensor 202 in contact with the evaporation vessel heating element 201 is maintained at a constant temperature, and accordingly, the raw material pitch injected into the evaporation vessel It melts and fills the lower part of the evaporation container in a complete liquid phase, and even when the liquid level of the filled raw material pitch rises, the heat of the filled raw material pitch is not conducted to the temperature sensor located at the upper end of the temperature sensor 251. An insulating layer 252 that withstands high temperatures is placed.

So, when the raw material pitch liquid level reaches the upper end of the temperature sensor 251, the temperature of the liquid raw material pitch is sensed by the temperature sensing element at the upper end of the temperature sensor 251, and the agitator driving motor is operated according to the detected temperature signal. .

The rotational force detected by the "stirrer driving torque sensor 121" increases in proportion to the rise in the liquid level of the raw material pitch.

Therefore, since the agitator rotational force sensed by the "stirrer driving torque sensor 121" is constantly maintained, the liquid level of the raw material pitch inside the evaporation container 200 can be maintained constant.

So, the frequency setting signal of the inverter that controls the rotation speed of the raw material pitch injector is selected as the frequency setting input signal of the inverter 311 through the "frequency setting signal selection relay", and the output signal of the "stirrer torque controller" is selected as the frequency setting input signal of the inverter 311. If the rotation speed of the raw material pitch injector is reduced and the rotational force of the stirrer is reduced, the rotation speed of the injector is controlled to increase, so that the liquid level of the raw material pitch inside the evaporation vessel can be maintained at a constant height.

And the volatile material vapor evaporated inside the evaporation vessel is filled in the condensation vessel 400 through the "discharge pipe 114", the "steam outlet space 113" and the pipe. So, the pressure inside the container rises, and the increased pressure is sensed by the "pressure transmitter (P)", and the coolant circulates according to the sensed pressure.

6, the pitch reforming apparatus of the present invention as described above

If it is represented as a component device, pipe, and “measurement and controller (instrument)” and explained sequentially according to its function in turn,

When the raw material pitch, which is solid at room temperature, fills the hop 210, the temperature signal detected by the temperature sensor T0 is input to the temperature indication controller (TIC0) located in the "driver operation panel 101". and the temperature indication controller TIC0 outputs a control signal so that the semiconductor power controller TPR0 located in the electrical and electronic control panel 102 heats the raw material pitch to 100-130° C. to the electric heater 212 to melt it.

The melted raw material pitch is introduced into the raw material pitch injector 220 and is injected according to the driving speed of the "raw material pitch injecting device 220" in which the driving speed is controlled because the inverter INV controls the power frequency supplied to the driving motor. The amount of raw material pitch is determined. And when the raw material pitch injection device is driven, the heater 224 located on the cylindrical outer surface of the raw material pitch injector transmits the temperature signal sensed by the temperature sensor 226 to the temperature indication controller TIC2 located on the “operator control panel 101”. is input, and the temperature indication controller TIC2 inputs a power control signal to the semiconductor power controller TPR1 located in the electrical and electronic control panel 102 so that the raw material pitch temperature into which the electric heater 224 is injected becomes the same temperature as the internal temperature of the evaporation vessel. Controls the power supplied to the heater (224).

When operating the equipment for the first time, set the frequency according to the "Initial raw material supply speed setting" in the inverter (INV) for speed control of the driving motor of the "raw material pitch supply device 220" installed on the operator's operation panel 101 and start the device. When the raw material pitch injection device is driven at a set speed, the raw material pitch is injected into the evaporator, and the temperature signal of the temperature sensor T2 that detects the injected raw material pitch temperature is the temperature located in the “operator operation panel 101”. The semiconductor power controller (TPR1) located in the electrical and electronic control panel 102 according to the output signal of the temperature indicating controller (TIC2) input to the instruction controller (TIC2) controls and supplies electric power to the electric heater of the pitch of the raw material injected into the evaporator. The temperature is controlled to maintain 300-350°C, which is the lowest evaporation temperature of volatile substances contained in the raw material pitch, inside the evaporation vessel.

In addition, the temperature signal sensed by the temperature sensor T3 that detects the surface temperature of the electric heater 201 installed on the outer peripheral surface of the evaporation vessel is input to the temperature indication program controller (TIPC1) installed in the “driver operation panel 101” The semiconductor power controller TPR2 located in the electronic control panel 102 controls the power supplied to the electric heater 201, and the temperature sensed by the temperature sensor T3 is the raw material pitch temperature (300-350° C.) injected through the raw material pitch injector. ), in consideration of the time required for the rise of the raw material pitch inside the evaporation container, the temperature rise pattern of the temperature indication program controller is set, and the temperature rises gradually according to the set program.

That is, the lowest temperature of evaporation among volatile substances contained in the raw material pitch is about 350°C.

In Fig. 6, the surface temperature of each evaporation vessel heating element 201 was set at 500, 510, and 520° C. in consideration of the evaporation temperature and the set pressure of the volatile substances contained in the raw material pitch in the three evaporation and condensing vessels. Set the temperature rise gradient according to time so that the temperature rises gradually.

The internal pressure of the evaporation vessel is sensed with the “pressure transmitter (P)” and the detected pressure signal is input to the pressure indication regulator (PIC1) located on the operator panel 101, and the atmospheric pressure is set to 0 atm in the pressure indication regulator (PIC1). and set to 1.5, 1, and 0.5 atm, respectively, and control the internal pressure of each condensing container by opening and closing the cooling water discharge solenoid valve according to the set pressure value.

The raw material pitch injected into the evaporative condenser at the speed set in the “initial raw material supply rate setting” by the “raw material pitch injector 220” receives the heat from the lower heater 201 of the evaporative vessel and melts into a liquid and pools in the lower portion of the evaporator. It goes down and forms a liquid level, and the formed liquid level gradually rises according to the amount of the injected raw material pitch. And in order to detect that the rising liquid level rises to the bottom of the agitator blade, the temperature sensor 251 puts an insulating layer 252 that withstands high temperature on the outer peripheral surface of the sheath pipe to prevent heat from being conducted from the raw material pitch, and the temperature sense The temperature sensing element at the upper end of (251) is lengthened to the height of the lower part of the agitator blade, and placed in the center of the evaporation container through a flush bottom valve 250 that opens and closes in line with the bottom of the evaporation container. When in contact with this temperature sensing element, the lower end of the agitator blade comes into contact with the rising pitch solution level. Therefore, the high-temperature heat of the raw pitch solution is not conducted to the temperature sensing element before the liquid level of the raw pitch solution reaches the uppermost part where the "temperature sensing element" of the temperature sensor 251 is located from the lower part of the evaporation container. As soon as the temperature sensing element reaches the position, the temperature of the raw material pitch is sensed, and power is supplied to the agitator driving motor according to the sensed temperature signal, and the agitator blade rotates at a constant speed.

Therefore, the torque signal detected by the torque detector 121 installed between the agitator blade drive shaft and the motor drive shaft in proportion to the rise in the raw material pitch solution level increases in proportion to the rise in the raw material pitch liquid level, and the increasing torque signal is the rise in the raw material pitch liquid level. indicates the location.

The "turning force detection signal Tr" is input to the torque indication controller TrIC1 located on the driver's operation panel 101 and outputs a control signal output according to the value set in the torque indication controller TrIC1 "selection relay that PLC outputs" Since " is selectively connected to be input as an input signal that sets the output frequency of the inverter (INV) that controls the driving speed of the driving motor, the rotation speed of the raw material pitch injection motor 221 is the control output signal of the torque indication regulator (TrIC1). controlled and driven

That is, when the raw material pitch liquid level does not reach the set liquid level, the rotation speed of the raw material pitch injector increases, and when the raw material pitch liquid level reaches the set liquid level, the raw material pitch injector rotates decreases. Therefore, the raw material pitch inside the evaporation container always maintains a liquid level at a constant height, and is evaporated and removed according to the evaporation temperature of the volatile material contained in the raw material pitch, and the evaporated vapor is condensed in the condensation container 400 .

Since the specific gravity of the pitch from which the volatile substances are removed by evaporation in the evaporation container increases, it grinds down, and the volatile substances continue to evaporate by conducting heat from the electric heater at the bottom, so the specific gravity of the pitch increases at the same time. When the pitch temperature of a certain position reaches a certain level or more according to the pressure inside the evaporation vessel, all the volatile substances that can evaporate at the reached temperature are removed by evaporation, so it is the reached temperature.

In other words, the heat consumed for evaporating the volatile material is the heat of evaporation at a certain temperature, so the temperature cannot rise. However, the heat applied after all the volatile substances have evaporated causes the temperature to rise. Therefore, by observing the temperature rise of the pitch, it can be recognized that the evaporation of the volatile material is completed.

Therefore, it is possible to distinguish between the heat-treated pitch and the non-completed pitch by checking the two things: the ground down position and the temperature rise of the pitch due to the increase in specific gravity.

So, to separate and discharge the heat-treated pitch, as shown in FIG. 3, put the discharge pipe 230 for discharging at the ground position according to the increase in the specific gravity of the reformed pitch, and put the temperature sensor 231 at the outlet of the discharge pipe. When only the pitch at which the temperature sensed by the temperature sensor 231 reaches the set heat treatment completion temperature or more is discharged, the volatile substances that evaporate according to the temperature and pressure of the evaporation vessel are completely evaporated and only the removed pitch is discharged.

That is, the temperature signal detected by the temperature sensor T1 in FIG. 6 is input to the temperature indication controller TIC1 located on the driver's operation panel 101, and the temperature of the pitch on which the reforming is completed is set to the temperature indication controller TIC1. The control output signal that is output by comparing the temperature to be set with the set temperature is input to the "Valve Positioner 320", and the "Valve Positioner" is the "Automatic Flow Control Valve 240" according to the input signal. The degree of opening of

Therefore, only the pitch that is evaporated and removed according to the evaporation temperature of the volatile material in the evaporation container is determined and discharged according to the opening degree of the "automatic flow rate control valve 240".

Since the pitch is coking when suddenly in contact with high-temperature heat, the evaporation temperature of volatile substances contained in the raw pitch has a difference of about 90°C from 350°C to 440°C under atmospheric pressure. So, as shown in FIG. 5, the evaporation condensing vessel is divided into three with a difference of 30° C., the evaporation temperature is 350-380° C., 380-410° C., and 410-440° C. under atmospheric pressure according to the evaporation temperature.

And, as discussed above, the pitch heated to 350° C. or higher flows according to the pressure difference as a complete liquid. Therefore, if the pressure difference between the three evaporation and condensing vessels is 0.5 atm, it can be easily discharged.

Pitch is a viscoelastic polymer at room temperature, and hydrocarbons coexist in the form of various molecular bonds. Therefore, the pitch is not constant in evaporation pressure and temperature. Therefore, the electric heater that supplies the evaporation heat has a temperature sensor 202 that senses the surface temperature of the heating element as shown in FIG. 3, senses the surface temperature of the heating element as shown in FIG. ) is input to the temperature indication controller (TIC3) located in ) and according to the temperature set in the temperature indication controller (TIC3), a control signal is input as a signal to control the output power of the semiconductor power controller (TPR2) located in the electrical and electronic control panel 102 . Therefore, the heating element always maintains the temperature set in the temperature indication controller (TIC3). If 500℃ is set in the temperature indicator controller (TIC3), the surface temperature of the heating element is always maintained at 500℃. However, if the evaporation temperature of the volatile substances contained in the raw material pitch inside the evaporation vessel is 350 °C from the 500 °C heating element, the heat of the heating element is transferred to the raw material pitch with a temperature difference of 150 °C to evaporate the volatile substances and vaporize the volatile substances increases the pressure inside the container, and the pressure transmitter (P), which detects the increased pressure By outputting a control signal according to the set pressure and the pressure signal detected by the “pressure transmitter (P)”, the solenoid valve that discharges the cooling water to the condensing vessel is opened and closed, so the pressure inside the evaporative condensing vessel is maintained at the set pressure.

At this time, if the set pressure of 1.5 atm is not maintained even though the cooling water does not flow through the condenser, the set temperature of the “heating element surface temperature indicating controller (TIC3)” is raised. ) to lower the set temperature. In this way, the temperature of each heating element is determined according to the internal pressure maintenance of each evaporation and condensation vessel.

As described above, since the types of various volatile substances constituting the pitch are diverse, the evaporation temperature of the volatile substances cannot be defined. Therefore, the temperature of the heating element according to the evaporation pressure of the evaporated steam is not set in advance, but the temperature of the electric heater of each evaporation vessel is not set in advance. In accordance with the order in which raw material pitch is injected and discharged, 1.5, 1, and 0.5 atm are set in advance, and the surface temperature of the heating element of the electric heater is set accordingly. The evaporation temperature of the material is lower than the evaporation temperature of the volatile material evaporated in the "evaporation and condensation tank set at 1 atmosphere", and thus, condensed materials can be obtained sequentially in the order of the evaporation temperature of the volatile material being lower.

And the second and third evaporative and condensing tanks describe the means of maintaining a constant level of the raw material pitch solution. In the first evaporative and condensing tank, the heat-treated pitch increases in specific gravity, so it sinks to a certain height and reaches a constant temperature. Discharge is divided into the heat-treated pitch and the non-heat-treated pitch. Therefore, the discharged pitch flows into the second evaporative and condensing tank through the automatic flow control valve as a liquid fluid. Even at this time, the level of the inflow pitch is maintained by maintaining the liquid level and rising according to the liquid level maintenance procedure described above. The control signal that is input to the torque indication regulator (TrIC1) and is output by comparing the value set in the torque indication regulator (TrIC1) with the input torque signal is input to the "Valve Positioner 320" and "valve opening degree" The "controller" determines the opening degree of the "automatic flow control valve 240" according to the input signal, and controls the discharged flow rate accordingly, so that the liquid level of the solution is always maintained at a constant height.

That is, when the maintained liquid level is lower than the set liquid level, the flow rate discharged through the flow control valve is lowered, and when the maintained liquid level is higher than the set liquid level, the flow rate discharged through the flow control valve is increased.

The third evaporative condenser maintains the liquid level of the solution constant in the same procedure as the second evaporative condenser.

The "evaporated volatile matter vapor condenser 400" puts the "space 402 in which non-condensing gas collects" as shown in FIG. 3 at the top of the "Shell and Tube condenser 400", and It consists of a space temperature sensor (T5), a back pressure regulator (404), a bypass valve (405), and a discharge valve (401).

All the vapors from which the volatile substances contained in the pitch are evaporated are condensed and liquefied in the "cell-and-tube condenser 400, but the non-condensing gas such as air injected through the raw pitch injector is lighter than the condensed gas, so non-condensing at the top of the condenser 400 When the non-condensing gas accumulates in the space where the gas accumulates and the non-condensable gas increases and fills the entire space where the non-condensable gas accumulates, the temperature of the high-temperature condensed gas is not conducted and the temperature sensed by the temperature sensor (T5) decreases. is input to the temperature indication controller (TIC5) located on the operator's operation panel 101, and the temperature indication controller (TIC5) closes the discharge valve 401 when the set temperature and the temperature sensed by the temperature sensor T5 are lower than the set temperature. At the same time, the valve 503 is opened, and the non-condensable gas in the space in which the non-condensable gas is accumulated is discharged to the atmosphere through the hood and filled with high-temperature steam, so that the valves 401 and 503 are closed.

And when the cooling water supply is stopped or the pressure inside the container rises due to equipment failure, the relief valve opens and high-pressure steam is discharged. The pressure indication controller (PIC1) located in the “operator operation panel 101”, where It sounds and indicates the part where the safety valve has been activated.

100: upper end plate
101: driver operation panel 102: electric and electronic control panel
111: agitator driving motor 112: inert gas supply pipe
113: steam discharge space 114: steam discharge pipe
115: heating element 116: insulating material
117: agitator drive shaft 118: agitator blades
119: tightening bracket 120: temperature sensor
121: torque sensor
200: evaporation vessel according to the invention
201: evaporation vessel heating element 202: heating element temperature sensor
210: Hopper
211: heating element for raw material pitch preheating 212: raw material pitch preheater
220: raw material pitch injector
221: raw material pitch injector driving motor 222: sealing
223: screw blade 224: screw shaft
225: raw material pitch injection device heating element 226: injected raw material pitch
temperature sensor
230: heat treatment completed pitch discharge pipe
231: heat-treated pitch temperature sense
240: automatic flow control valve
250: flush bottom valve (Flush Bottom Valve)
251: heat-treated pitch temperature sense
300: evaporative condenser
310: agitator driving torque control device 311: inverter
312: frequency setting signal selection relay
320: heat treatment completed pitch discharge control device
321: heat-treated pitch temperature sensor
400: condensate recovery device
401: non-condensed gas discharge valve 402: non-condensing gas space
403: non-condensed gas storage tank temperature sense
404: safety valve (Relief Valve) 405: bypass valve
500: vacuum pump
501 : filter
502: automatic ball valve operated by pneumatic pressure
503 : ""
T0: Temperature sensing (preheating temperature sensing) TIC0: Temperature indicating controller (preheating temperature)
TPR0: semiconductor power controller (preheater)
T1: Temperature sense (exhaust pitch temperature) TIC1: Temperature indication controller (exhaust pitch temperature)
S: solenoid
T2: Temperature sense (Incoming raw material pitch temperature) TIC2: Temperature indicating controller (Incoming raw material pitch)
T3: Temperature sense (heating element for evaporation) TIC3: Temperature indication controller (heating element for evaporation)
TPR2: semiconductor power controller (heating element for evaporation)
T4: temperature sense (exhaust steam temperature) TIC4: semiconductor power controller (exhaust steam)
T5: Temperature sense (non-condensing gas) TIC5: Semiconductor power controller (non-condensing gas)
P : Pressure transmitter (evaporative condensing vessel) PIC1 : Pressure indicating regulator (evaporative condenser)
Tr : torque sensor (stirrer drive) TrIC : torque indicator controller (stirrer drive)
700: automatic flow control valve
701: valve body 702: spring for fixing valve seat
703: toilet seat fixing screw 704: valve connector
705: Airtight Device 706: Positioner
707 : Valve Actuator

Claims (6)

In order to evaporate and remove the volatile substances contained in the pitch, the evaporation container 200 is heated as shown in FIG. 3 and the condensation recovery container 400 is airtightly connected to one of the two containers for cooling, and the raw material pitch is injected. Since the injector 220 is operated, the raw material pitch is injected into the evaporation vessel in a state where the injected raw material pitch is closely adhered and airtight is maintained, and the injected raw material pitch is heated in the evaporation vessel to evaporate the volatile substances contained in the raw material pitch, and The evaporated vapor is cooled and condensed in the connected condensing recovery unit, so it is separated and removed from the raw material pitch.
At this time, the heat applied to the raw material pitch from the evaporation container is absorbed as evaporation heat for evaporating the volatile material, so that the temperature of the pitch does not rise and the temperature of the pitch rises only after all the volatile materials have evaporated. In addition, the specific gravity of the pitch removed by evaporation of all volatile materials is higher than the specific gravity of the pitch in which all volatile materials are not evaporated and removed.
Using the physical properties of the pitch, the evaporation vessel is lengthened up and down in order to distinguish the pitch from which all volatile substances are evaporated and the pitch from which all volatile substances are not evaporated, and a stirrer blade at the top stirs the raw material pitch to remove volatile substances. It is placed as a space to evaporate, and a space is placed under the space where the pitch with increased specific gravity is ground down by evaporation and removal of volatile substances. The pitch ground down is raised in temperature close to the temperature of the heating source.
And since the solids contained in the pitch have a heavier specific gravity than the pitch from which all volatile substances are evaporated and removed, the discharge pipe 230 for discharging the reformed pitch to sink further to the bottom and separate from the bottom of the container at a certain height By placing a temperature sensor 231 at the front end of the discharge pipe inside the evaporation container, the temperature sensed by the temperature sensor 231 is discharged by adjusting the opening degree of the “automatic flow control valve 240” so that only the pitch above a certain temperature is discharged. The discharged pitch is a reforming means that can be reformed in a state in which all volatile substances are removed by evaporation and even solid substances that are not soluble in toluene and quinoline are separated and removed. The raw material pitch injection device for continuously injecting raw material pitch according to the amount of reforming and discharged from the inside of the high-temperature and high-pressure evaporation vessel implementing the reforming means of claim 1 is a preheater 210, a raw material pitch injector 220, and a heating element 224. , consisting of a temperature sense 226 and
While the raw material pitch is injected, it is pressurized to maintain airtightness and heated, and the raw material pitch temperature at the moment it is heated and injected into the evaporation vessel is controlled to match the internal pressure and temperature of the evaporation vessel, so it has no effect on the temperature and pressure inside the evaporation vessel Raw material pitch injection device that injects the raw material pitch into the evaporating vessel without causing When the volatile substances contained in the raw material pitch are removed by evaporation in the high-temperature and high-pressure airtight evaporation vessel 200 implementing the reforming means of claim 1, at the same time, the molecular crystal structure is improved and the specific gravity increases.
So, unlike other materials, pitch has a low coefficient of expansion with respect to heat, and its specific gravity increases as the temperature increases. Using the physical properties of this pitch, a stirring space is placed in the upper part of the evaporation vessel 200 as shown in FIG. 3 in order to discharge the pitch for which the heat treatment is not completed and the pitch for which the heat treatment is completed by specific gravity and temperature, and discharge it, and below the stirring space A space where the pitch of which the specific gravity has been modified and increased is replaced, and the discharge pipe 230 is placed at a certain height from the bottom of the space where the pitch is ground, and a temperature sense 231 is placed at the front end of the discharge pipe 230, and the discharge pipe A "flow automatic control valve 240" is placed at the end.
So, when the reforming is completed and the specific gravity increases, the pitch is ground down, and if the pitch ground down maintains a constant temperature, the pitch that has been heat-treated and the pitch that has not been heat-treated are automatically divided according to the physical properties of the pitch, and the pitch that has been heat-treated "Pitch exhaust device of pitch reforming means" that discharges only The mass of the volatile material that is evaporated and removed in the high-temperature and high-pressure evaporator 200 implementing the reforming means of claim 1 and the mass discharged through the discharging device discussed in “Claim 3” after the heat treatment is completed are the two masses A raw material pitch preheater 210, a raw material pitch injector 220, a temperature sense ( 226), evaporation vessel heating element 201, heating element temperature sense 202, evaporation vessel internal temperature sense 251, insulating insulating layer 252, stirring rotation force detector 121, stirring rotation force control device 310, inverter ( 311), "inverter input signal selection relay 312", and "injector driving motor 221"
When the raw material sebum is filled in the raw material pitch preheater 210 and the device is operated, the raw material pitch melts at 100-130° C. in the raw material pitch preheater 210 and changes to a meso-phase between liquid and solid, and the raw material by earth gravity It flows into the inlet of the pitch injector 220, and at this time, the "inverter input signal selection relay 312" is connected to the "raw material injection speed setting" side, and the raw material pitch injector driving motor is driven according to the "raw material injection speed setting" so that the raw material pitch evaporates It is injected into the container 200 .
The raw material pitch injected into the evaporation container is melted into a liquid phase, and the raw material pitch liquid level rises from the bottom of the evaporation container 200 . And in order to prevent the high temperature heat of the raw material pitch from being conducted to the temperature sensor 251 according to the rising liquid level, the outer peripheral surface of the temperature sensor 251 is wrapped with a heat insulating layer 252 that withstands high temperature and closed with a stainless steel plate to be airtight do.
When the rising raw material pitch liquid level reaches the portion where the uppermost temperature sensing element of the temperature sensor 251 is located, the temperature sensing element at the top of the temperature sense 251 detects the raw material pitch temperature of the liquid level, and the detected temperature signal operates the stirrer And as the stirrer operates, the amount of change in the rotational force detected by the "stirring rotational force sensor 11" coincides with the amount of change in the raw material pitch liquid level.
So, when the "agitator torque sensor 121" maintains a constant rotational force, the "inverter input signal selection relay 312" selects the output signal of the stirring drive driving torque indicating regulator (TrIC) to be connected to the inverter input signal.
Therefore, the control output of the rotational force indicating regulator (TrIC) decreases the driving rotational speed of the raw material pitch injector when the rotational force increases, and controls to increase the raw material injector driving rotational speed when the rotational force decreases to maintain a constant rotational force at all times. It is possible to maintain a constant height of the liquid level of the raw material pitch inside the evaporation container without a separate liquid level detector inside the high-temperature evaporation container.
A means to overcome the atmosphere in which a separate “liquid level detector” cannot be placed inside the evaporation vessel filled with the airtight, high-temperature, and pitch black viscoelastic material, and to maintain the liquid level of the pitch solution inside the evaporation vessel at a constant height. In order to implement the means of claim 4, a rotational force sensor 121 is placed between the agitator blade drive shaft and the stirring mechanism motor as shown in FIG. "Liquid level detection device" that detects the liquid level of the pitch solution inside the evaporation vessel filled with airtight, high temperature, and viscoelastic pitch using Since an insulating layer 252 that blocks heat transfer is placed on the outer peripheral surface of the sheath pipe of the temperature sensor 251 implementing the means of claim 4 as in FIG. "Pitch solution level reaching recognition device" that prevents the transfer to the sensing element and allows the heat of the solution to be conducted to the temperature sensing element as soon as the liquid level of the solution comes into contact with the temperature sensing element, so that it is possible to accurately recognize the position of the liquid level of the raw material pitch

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