JP2001065800A - Pressurizing gas flow control method in pressure-feeding method for liquid raw material - Google Patents

Abstract

PROBLEM TO BE SOLVED: To stably feed liquid raw material stored under atmospheric pressure into a device such as a pressurized reactor while preventing fluctuation in flow rate caused by attachment in a valve and abrasion of a valve element, and to increase followability to pressure change of the device. SOLUTION: After filling cylinders with liquid raw material in a raw material tank 1, a raw material returning line 35 is purged by means of pressurizing gas, and then the pressurizing gas is filled in the cylinders to pressurize the raw material. On completing pressurizing the cylinders are communicated with the reactor 3 and then the pressurizing gas is fed into the cylinders, so that the pressurized material is pushed out to the reactor 3 in a volume flow comparable to a pressurizing gas flow rate. The remaining material in the cylinders is fed out by means of the pressurizing gas. These operation are repeated in order for a plural system of cylinders 30A, 30B to continuously feed the raw material in the reactor 3. At that time, an actual pressurizing gas flow rate corresponding to each cylinder is controlled to be equal to an automatically set pressurizing gas flow rate.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for pressurizing and supplying a liquid raw material (homogeneous liquid, emulsion, slurry, etc.) stored under atmospheric pressure into a pressurized reactor. The present invention relates to a pressure gas flow control method.

[0002]

2. Description of the Related Art Conventionally, as a liquid material pressurizing apparatus, as shown in FIG. 8, a pump 2 is provided near a material tank 1 (atmospheric pressure) according to the properties and head of the material. In general, a system in which the raw material pressurized by the pump 2 is supplied to the reactor 3 is used. In this case, the discharge flow rate of the pump 2 is usually set to be larger than the raw material supply amount required in the reactor 3. Generally, the flow rate of the raw material guided to the reactor 3 is adjusted by the flow control valve 4, and a part of the pump discharge amount is reduced by the pressure control valve 5 and returned to the raw material tank 1.

[0003]

However, when the raw material supply amount is extremely small, such as in a test device, the pump 2
Not only is difficult to select, but also the flow rate control valve 4 for controlling the flow rate becomes small, and in the case of a liquid raw material containing a solid content such as slurry, not only the solid content adheres to the valve port and the flow rate becomes unstable, but also It may cause troubles such as blockage.
In addition, the narrowed portion of the valve or the like is worn by the solid content, and it may be difficult to use it stably for a long time.

The present invention has been made in view of the above-mentioned circumstances, and has been developed in view of the fact that even when the supply amount of the raw material stored under the atmospheric pressure is extremely small, the flow rate fluctuation due to the deposits on the valve and the flow rate of the valve may be reduced. An object of the present invention is to provide a pressurized gas flow control method in a liquid raw material pressurized supply method capable of stably supplying the raw material into a pressurized reactor or the like while preventing body wear.

[0005]

According to the present invention, there is provided a raw material filling method in which a liquid raw material stored at atmospheric pressure in a raw material tank is circulated from a cylinder to a raw material tank via a raw material return line while filling the cylinder. After charging the raw material into the cylinder, the pressurizing gas is led to the raw material tank via the raw material return line, and the raw material return line purge for pushing out the raw material filled in the raw material return line to the raw material tank, and the pressurizing gas is discharged into the cylinder. When the pressure in the cylinder rises to approximately the same level as the pressure in the equipment, the cylinder and the equipment are brought into communication, and the gas for pressurization is further introduced into the cylinder. By supplying the material, the material pressurized in the cylinder is extruded from the cylinder to the equipment at a volume flow rate corresponding to the gas flow rate for pressurization. After the supply of raw materials to the cylinder is completed, the liquid raw material is continuously fed into the pressurized equipment by sequentially repeating in-cylinder purging of discharging the remaining raw material in the cylinder to the raw material tank by the pressurizing gas in multiple cylinders. Pressurizing gas flow control method in the pressurized liquid raw material supply method, wherein the raw material flow rate as mass flow rate is set to m and the raw material specific gravity is set to ρ in advance, and the actual pressurizing gas pressure P ₁ and each The cylinder pressure P ₂ is detected, the atmospheric pressure with respect to vacuum is set to P _{0 in the} same pressure unit as P ₁ and P _2, and the pressurizing gas flow rate V as the volume flow rate corresponding to each cylinder is set to

V = m / ρ × (P ₂ + P ₀ ) / (P ₁ + P ₀ ) and is set, and the actual pressurization gas flow rate V corresponding to each cylinder is set. The present invention relates to a pressurizing gas flow rate controlling method in a liquid raw material pressurizing and supplying method, characterized in that it is controlled to be equal to:

According to the above means, the following effects can be obtained.

The liquid raw material stored in the raw material tank under atmospheric pressure is filled into the cylinder while being circulated from the cylinder to the raw material tank via the raw material return line, and the raw material is filled, and the raw material is filled into the cylinder. After that, the pressurizing gas is led to the raw material tank via the raw material return line, the raw material filled in the raw material return line is pushed out to the raw material tank, the raw material return line is purged, and the pressurizing gas is introduced into the cylinder. By being sealed, the inside of the cylinder is pressurized and the cylinder is pressurized. When the pressure in the cylinder becomes substantially the same as the pressure in the device, the cylinder and the device are communicated with each other, and the pressurizing gas is further released. Is supplied into the cylinder, the raw material pressurized in the cylinder is pushed out from the cylinder to the equipment at a volume flow rate corresponding to the gas flow rate for pressurization, and the raw material is supplied. After the supply of the raw material from the cylinder to the equipment is completed, the raw material remaining in the cylinder is discharged to the raw material tank by the pressurizing gas, the purge in the cylinder is performed, and these operations are sequentially repeated in a plurality of cylinders, so that the continuous operation is performed. The raw material is supplied to the equipment.

As a result, even if the amount of raw material supplied is extremely small as in a test apparatus, the selection of a circulation pump becomes easy,
There is no need for a flow control valve to adjust the flow rate of the raw material, and even if the raw material contains solids such as slurry, the solids do not adhere to the valve port and impair the stability of the flow rate. No troubles such as the occurrence of troubles, and there is no fear that the throttled parts such as valves will be worn by solids, making it difficult to use them stably for a long time. Is supplied, and the flow of the raw material is always formed in any of the paths, and the path in which the flow needs to be stopped is purged with the pressurizing gas, so that the liquid raw material does not stay in each part of the pipe.

When the raw material pressurized in the cylinder is pushed out of the cylinder at a volume flow rate corresponding to the flow rate of the pressurizing gas from the cylinder to the equipment, the raw material flow rate as the mass flow rate is m and the raw material specific gravity is ρ. The actual gas pressure for pressurization P ₁ and each cylinder pressure P ₂ are detected, and the atmospheric pressure with respect to vacuum is set to P _{0 in the} same pressure unit as P ₁ and P _2. Pressurizing gas flow rate V as the corresponding volume flow rate is respectively

## EQU3 ## V = m / ρ × (P ₂ + P ₀ ) / (P ₁ + P ₀ ) is obtained and set, and the actual pressurization gas flow rate corresponding to each cylinder is set. V
Thus, even if the pressure of a device such as a reactor to which the raw material is supplied changes, the supply amount of the raw material is kept constant without changing, and the operator can control the equipment such as the reactor. It is not necessary to change the setting of the pressurizing gas flow rate V in accordance with the pressure change, and the operation is not complicated.

[0010]

Embodiments of the present invention will be described below with reference to the drawings.

FIG. 1 and FIG. 2 show an example of an apparatus for carrying out a method for pressurizing and supplying a liquid raw material according to the present invention. In FIG. 1 and FIG. I have.

In the illustrated example, a plurality of systems (two systems A and B in the illustrated example) are provided with cylinders 30A and 30B,
For each of the cylinders 30A and 30B, the liquid raw material stored in the raw material tank 1 (where a stirrer is installed as necessary) is supplied from the filling line 31 to the four-way valve V4 through the operation of the circulation pump 20. Filling line 32 provided with shut-off valve V5, four-way valve V3, filling / press-fitting lines 33A, 33B
And can be filled through

The cylinders 30A and 30B are connected to the filling / press-fitting lines 33A and 33B on the bottom surface, and connected to a pressurizing gas system 34 for introducing a pressurizing gas such as air or nitrogen to the top surface. A raw material return line 35 communicating with the raw material tank 1 is connected to a required position of the raw material tank 1. In the raw material return line 35, shutoff valves V2A and V2B and a restriction orifice 36 are provided.

The pressurizing gas system 34 is provided with a pressure control valve 39 and a pressure gauge 40 in the middle of a pressurizing gas line 38 extending from a pressure source 37 in which the pressurizing gas is stored. From line 38 to cylinder 30A,
Pressurizing gas lines 38A, 38 branching to and extending to 30B
In the middle of B, a configuration is provided in which manual open / close valves 44A, 44B, positive displacement flow meters 45A, 45B, and flow control valves V1A, V1B are provided. Here, the pressure 41 of the pressurizing gas detected by the pressure gauge 40 is a pressure controller 42
The opening command 43 is output to the pressure control valve 39 so as to be equal to a pressure set value preset in the pressure controller 42, and is detected by the positive displacement type flow meters 45A and 45B. Of pressurized gas 46
A and 46B are input to the flow controllers 47A and 47B, and the flow control valves V1A and V1 are set to be equal to the flow set values preset in the flow controllers 47A and 47B.
The opening degree commands 48A and 48B are output to B. Note that the pressure set value and the flow rate set value are manually set as appropriate by an operator, judging from operation conditions.

A press-in line 49 connected to the reactor 3 via the four-way valve V3 is connected to the filling / press-in line 33A, 33B. A manual opening / closing valve 51 for completely stopping the supply of the raw material when the operation is stopped is provided.

A circulating line 52 connected to the raw material tank 1 is connected to the filling line 31 via a four-way valve V4 so as to be able to shut off or switch to a communicating state. The connected in-cylinder purge material return line 53 is connected via a four-way valve V4 so that it can be shut off or switched to a communicating state. A restriction orifice 54 is provided in the middle of the circulation line 52, and the in-cylinder purge material return line 53 is provided. In the middle of the line 53, a shutoff valve V7 and a restriction orifice 55 are provided.

A purge gas system 56 for introducing a pressurizing gas such as air or nitrogen for purging is connected in the middle of the purge material return line 53 in the cylinder between the four-way valve V4 and the shut-off valve V7. is there.

The purging gas system 56 includes a pressure regulating valve 58, a pressure gauge 59, and a pressure regulating valve 58 in the middle of a purging gas line 57 extended from a pressure source 37 in which a pressurizing gas is stored.
It has a configuration in which a gas holder 63, a shutoff valve V6, and a check valve 64 are provided. Here, the pressure 60 of the pressurizing gas detected by the pressure gauge 59 is a pressure controller 61.
And an opening command 62 is output to the pressure control valve 58 so as to be equal to a pressure set value preset in the pressure controller 61. Note that the pressure set value is manually set as appropriate by an operator, judging from the driving situation.

The cylinders 30A and 30B are provided with pressure gauges 66A and 66B for detecting the pressures 65A and 65B in the cylinders 30A and 30B, respectively.
A pressure gauge 68 for detecting the pressure 67 in the reactor 3 is provided. Further, the pressures 65A and 65B in the cylinders 30A and 30B detected by the pressure gauges 66A and 66B and the mass flow meter 50 are detected. The flow rate 69 of the raw material supplied to the reactor 3 and the pressure 67 in the reactor 3 detected by the pressure gauge 68 are input, and based on these detected values, a sequence as shown in FIG. , Output opening / closing commands 70A and 70B to shutoff valves V2A and V2B, output position switching instruction 71 to four-way valve V3, output position switching instruction 72 to four-way valve V4, and output opening / closing instruction 73 to shutoff valve V5. And a control device 76 for outputting an open / close command 74 to the shutoff valve V6 and outputting an open / close command 75 to the shutoff valve V7.

The cylinders 30A and 30B are connected to the reactor 3
Use a material that can withstand a pressure slightly higher than the pressure of the above, and increase the internal capacity for one cycle, the amount of raw material delivered per cylinder (the amount of supply per hour to the reactor 3 is 1/2 of one cycle) (E.g., capacity over time) (e.g., about 1.5 times the raw material delivery amount per cylinder per cylinder
About twice).

Next, the operation of the illustrated example will be described.

In the illustrated example, as shown in FIG. 2, the raw material filling, the raw material return line purge, the cylinder pressurization, the raw material supply, and the in-cylinder purge are sequentially performed in the A and B two-system cylinders 30A and 30B. By repeating, the raw material is continuously supplied into the reactor 3.

In the pressurizing gas system 34, the pressure 41 of the pressurizing gas detected by the pressure gauge 40 is input to the pressure controller 42 so that it becomes equal to the pressure set value preset in the pressure controller 42. Pressure control valve 39
The opening degree command 43 is output to the pressure type flow meter 45A, and the flow rate 46A of the pressurizing gas detected by the positive flow meter 45B.
46B is input to the flow controllers 47A and 47B,
The opening commands 48A, 48B are output to the flow control valves V1A, V1B so as to be equal to the flow setting values preset in the flow controllers 47A, 47B, whereby the preset pressure is applied to the cylinders 30A, 30B. A pressurizing gas having a pressure equal to the set value and a flow rate equal to the preset flow rate set value is constantly supplied.

The procedure for the cylinder A of the A system is roughly as follows.

A-Injection of raw material When the raw material of the A system is inserted, the shut-off valve V2A is opened by an opening / closing command 70A output from the control device 76, and the four-way valve V3 is filled by the position switching command 71 output from the control device 76. 32 and filling / press-fitting line 33
A is switched to a position for connecting A (connecting a → b), and the four-way valve V4 connects the filling line 31 and the filling line 32 according to the position switching command 72 output from the control device 76 (connecting a → b). ) Open / close command 7 which is switched to the position and output from the controller 76
3, the shutoff valve V5 is opened, whereby the raw material circulates at a relatively low pressure in the order of the raw material tank 1, the four-way valve V4, the shutoff valve V5, the four-way valve V3, the cylinder 30A, the shutoff valve V2A, and the raw material tank 1. The raw material is filled in the cylinder 30A.

A—Raw material return line purge When the raw material is filled in the cylinder 30A, the controller 76
Four-way valve V
4 is switched to a position for connecting the filling line 31 and the circulation line 52 (connecting a → c), and the shutoff valve V is output by an open / close command 73 output from the controller 76.
5 is closed, and the flow of the raw material is changed from the raw material tank 1 to the four-way valve V
4 → Switch to the system of raw material tank 1
The supply of the raw material to A is stopped. On the other hand, the flow control valve V1A
The pressurizing gas, which is supplied to the cylinder 30A in a constant amount through the cylinder 30A, is discharged to the raw material tank 1 through the shutoff valve V2A opened from the cylinder 30A. that time,
Since the pressurizing gas pushes out the raw material filled in the raw material return line 35, the raw material is removed from the inside of the raw material return line 35, and solid sedimentation can be prevented here.
At this time, although a pipeline from b to a of the four-way valve V3 is formed, the flow of the raw material does not occur because the shut-off valve V5 is closed.

A-Cylinder pressurization After the purge of the raw material return line 35 is completed, the control unit 76
The shut-off valve V2A is closed by the opening / closing command 70A output from the controller, and the pressurizing gas is confined in the cylinder 30A, so that the pressure in the cylinder 30A is increased at a speed corresponding to the supply amount of the pressurizing gas from the flow control valve V1A. Is done. When the pressure 65A in the cylinder 30A detected by the pressure gauge 66A becomes substantially the same as the pressure 67 in the reactor 3 detected by the pressure gauge 68, the four-way valve V3 is output by the position switching command 71 output from the control device 76. Is switched to a position that connects the filling / press-fitting line 33A and the press-fitting line 49 (connecting b → d), and the feed of the raw material from the pressurized cylinder 30A to the reactor 3 is started. As described above, the pressure gauge 66A is attached to the cylinder 30A, and the pressure 65A in the cylinder 30A detected by the pressure gauge 66A is measured by the pressure gauge 68.
If the setting is made such that the four-way valve V3 is switched when the pressure in the reactor 3 slightly becomes higher than the pressure 67 detected in the step 3, the reverse flow of the raw material from the reactor 3 or the pressure in the cylinder 30A is reduced. Although there is no concern about a temporary increase in the flow rate of the raw material due to the increase in the pressure, a simpler method is to determine the flow rate of the pressurizing gas and the space above the cylinder 30A (the volume of the portion not filled with the raw material). It is also possible to set the calculated pressurization time by a timer to switch the four-way valve V3.

A-Raw material supply After the pressurization in the cylinder 30A is completed, the raw material is pushed out from the cylinder 30A to the reactor 3 in accordance with the flow rate of the pressurizing gas supplied from the flow control valve V1A by switching the four-way valve V3. It is. When the raw material is sent from the cylinder 30A to the reactor 3, the pressure of the pressurizing gas is applied from the upstream side of the cylinder 30A, and the pressure in the reactor 3 is applied from the downstream side, and the flow rate of the pressurizing gas is zero. In this case, the raw material tends to stay in the cylinder 30A due to the balance between the two pressures, but if the pressurizing gas is supplied at a constant flow rate while the pressurizing gas is kept slightly higher than the pressure in the reactor 3. The raw material is delivered into the reactor 3 at a volume flow rate corresponding to the actual flow rate of the pressurizing gas (the actual volume flow rate under the pressure of the gas and the temperature).

A-In-Cylinder Purging When the flow rate 69 of the raw material detected by the mass flow meter 50 reaches a predetermined amount in total after the supply of the raw material to the reactor 3 from the cylinder 30A is started, the output from the controller 76 is output. The four-way valve V3 makes the filling / press-fitting line 33A and the filling line 32 communicate with each other by the position switching command 71 (b →
a) to the cylinder 30
The flow path from A to the reactor 3 is shut off, the shutoff valve V5 is opened by an open / close command 73 output from the control device 76, and the four-way valve V4 is filled by the position switching command 72 output from the control device 76. The position is switched to a position where the line 32 communicates with the purge material return line 53 in the cylinder (connecting b → d), and the shutoff valve V7 is opened by an open / close command 75 output from the controller 76,
A line for discharging the raw material to the raw material tank 1 is created. Here, since the capacity of the cylinder 30A is set to be larger than the raw material supply amount in one cycle (flow rate per hour × time of one cycle), the raw material remaining in the cylinder 30A is discharged to the raw material tank 1 through a discharge line. That is, the filling / press-fitting line 33A, the filling line 32, and the purge material return line 53 in the cylinder.
And is released through. Since the pressurizing gas is constantly supplied to the cylinder 30A from the flow control valve V1A, all the raw materials remaining in the cylinder 30A are pushed out,
The inside of the cylinder 30A is temporarily emptied.

The same line as A- is created by switching the A-raw material refilling valve, and the above operation is repeated.

The procedure for the cylinder B of the B system is as follows.

B-Feeding of raw material When feeding raw material in the B system, the shut-off valve V2B is opened by an opening / closing command 70B output from the control device 76, and the four-way valve V3 is charged by the position switching command 71 output from the control device 76. 32 and filling / press-fitting line 33
B is switched to a position for connecting B (connecting a → c), and the four-way valve V4 connects the filling line 31 and the filling line 32 according to a position switching command 72 output from the control device 76 (connecting a → b). ) Open / close command 7 which is switched to the position and output from the controller 76
3, the shutoff valve V5 is opened, whereby the raw material circulates at a relatively low pressure in the order of the raw material tank 1, the four-way valve V4, the shutoff valve V5, the four-way valve V3, the cylinder 30B, the shutoff valve V2B, and the raw material tank 1. The raw material is filled in the cylinder 30B.

B—Raw material return line purge When the raw material is filled in the cylinder 30B, the controller 76
Four-way valve V
4 is switched to a position for connecting the filling line 31 and the circulation line 52 (connecting a → c), and the shutoff valve V is output by an open / close command 73 output from the controller 76.
5 is closed, and the flow of the raw material is changed from the raw material tank 1 to the four-way valve V
4 → Switch to the system of raw material tank 1
The supply of the raw material to B is stopped. On the other hand, the flow control valve V1B
The pressurizing gas constantly supplied to the cylinder 30B through the cylinder 30B is discharged to the raw material tank 1 through the shutoff valve V2B opened from the cylinder 30B. that time,
Since the pressurizing gas pushes out the raw material filled in the raw material return line 35, the raw material is removed from the inside of the raw material return line 35, and solid sedimentation can be prevented here.
At this time, although the pipeline from c to a of the four-way valve V3 is formed, the flow of the raw material does not occur because the shut-off valve V5 is closed.

B-Cylinder pressurization After the purging of the raw material return line 35 is completed, the controller 76
The shut-off valve V2B is closed by the opening / closing command 70B output from the cylinder and the pressurizing gas is confined in the cylinder 30B, so that the pressure in the cylinder 30B is increased at a speed corresponding to the supply amount of the pressurizing gas from the flow rate control valve V1B. Is done. When the pressure 65B in the cylinder 30B detected by the pressure gauge 66B becomes substantially the same as the pressure 67 in the reactor 3 detected by the pressure gauge 68, the four-way valve V3 is output by the position switching command 71 output from the control device 76. Is switched to a position that connects the filling / press-fitting line 33B and the press-fitting line 49 (connecting c → d), and the feed of the raw material from the pressurized cylinder 30B to the reactor 3 is started. The pressure gauge 66B is attached to the cylinder 30B as described above, and the pressure 65B in the cylinder 30B detected by the pressure gauge 66B is measured by the pressure gauge 68.
If the setting is made such that the four-way valve V3 is switched at the time when the pressure in the reactor 3 slightly becomes higher than the pressure 67 detected in the step 3, the reverse flow of the raw material from the reactor 3 or the pressure in the cylinder 30B is reduced. Although there is no concern about a temporary increase in the flow rate of the raw material due to the higher pressure, a simpler method is to determine the flow rate of the pressurizing gas and the space above the cylinder 30B (the volume of the portion not filled with the raw material). It is also possible to set the calculated pressurization time by a timer to switch the four-way valve V3.

B-Raw material supply After the pressurization in the cylinder 30B is completed, the raw material is pushed out of the cylinder 30B to the reactor 3 by switching the four-way valve V3 in accordance with the flow rate of the pressurizing gas supplied from the flow control valve V1B. It is. When the raw material is sent from the cylinder 30B to the reactor 3, the pressure of the pressurizing gas is applied from the upstream side of the cylinder 30B, and the pressure in the reactor 3 is applied from the downstream side, and the flow rate of the pressurizing gas is zero. In this case, the raw material tends to stay in the cylinder 30B due to the balance between the two pressures, but if the pressurizing gas is supplied at a constant flow rate while the pressurizing gas is kept slightly higher than the pressure in the reactor 3. The raw material is delivered into the reactor 3 at a volume flow rate corresponding to the actual flow rate of the pressurizing gas (the actual volume flow rate under the pressure of the gas and the temperature).

B—In-Cylinder Purge When the flow rate 69 of the raw material detected by the mass flow meter 50 reaches a predetermined amount in total after the supply of the raw material from the cylinder 30B to the reactor 3 is started, the output from the controller 76 is output. The four-way valve V3 makes the filling / press-fitting line 33B and the filling line 32 communicate with each other according to the position switching command 71 (c →
a) to the cylinder 30
The flow path from B to the reactor 3 is shut off, the shutoff valve V5 is opened by an open / close command 73 output from the control device 76, and the four-way valve V4 is filled by the position switching command 72 output from the control device 76. The position is switched to a position where the line 32 communicates with the purge material return line 53 in the cylinder (connecting b → d), and the shutoff valve V7 is opened by an open / close command 75 output from the controller 76,
A line for discharging the raw material to the raw material tank 1 is created. Here, since the capacity of the cylinder 30B is set to be larger than the raw material supply amount in one cycle (flow rate per hour × time of one cycle), the raw material remaining in the cylinder 30B is discharged to the raw material tank 1 by a discharge line. That is, the filling / press-fitting line 33B, the filling line 32, and the purge material return line 53 in the cylinder.
And is released through. Since the pressurizing gas is constantly supplied from the flow control valve V1B to the cylinder 30B, all the raw material remaining in the cylinder 30B is pushed out,
The inside of the cylinder 30B is temporarily emptied.

By switching the B-raw material refilling valve, the same line as B- is made, and the above operation is repeated.

As shown in FIG. 2, while the raw material is being supplied in the A system, the purge in the cylinder, the filling of the raw material, the purge of the raw material return line, and the cylinder pressure are sequentially performed in the B system. While the raw material is being supplied in the system, the purge in the cylinder, the filling of the raw material, the purge of the raw material return line, and the pressure increase in the cylinder are sequentially performed in the system A, whereby the raw material is continuously supplied into the reactor 3. Is done.

Also, when the raw material filling is started in the B system while the raw material is being supplied in the A system,
As shown in FIG. 2, since the shut-off valve V6 is opened in a state where the shut-off valve V7 is opened, the pressurized gas from the purge gas system 56 allows the in-cylinder purge material return line 5 to be opened.
After that, the shut-off valve V7 is closed in a state where the four-way valve V4 is switched to the position for connecting the in-cylinder purge material return line 53 and the circulation line 52 (connecting d → c). Therefore, the pressurizing gas from the purge gas system 56 is supplied from the purge material return line 53 in the cylinder to the circulation line 52 via the four-way valve V4.
And the circulation line 52 is purged. Similarly, when the raw material feeding is started in the system A while the raw material is being supplied in the system B, as shown in FIG. 2, the shut-off valve V6 is opened with the shut-off valve V7 opened. Therefore, the purge material return line 53 in the cylinder is purged by the pressurizing gas from the purge gas system 56, and thereafter, the four-way valve V4 connects the purge material return line 53 in the cylinder with the circulation line 52. (D →
c), the shut-off valve V7 is closed, and the pressurizing gas from the purge gas system 56 is supplied with the purge material return line 53 in the cylinder.
The liquid is guided from the side to the circulation line 52 via the four-way valve V4, and the circulation line 52 is purged.

In the case of the illustrated example, the closed cylinder 30
After filling the raw materials in A and 30B, pressurizing gas (air,
Nitrogen or the like) and pressurize the raw material into the pressurized reactor 3, so that a stable raw material supply can be performed without being affected by the characteristics of the circulation pump 20 as a rotating device.

Also, no valves or the like for controlling the flow rate are provided in the flow path of the raw material, and the flow rate of the raw material is controlled indirectly by pressurizing the cylinders 30A and 30B filled with the raw material with a pressurizing gas. Fluctuations in flow rate and blockage troubles occurring in the control valve can be avoided.

Further, in the case where the raw material is a settling slurry or the like, if the raw material is temporarily stored in the closed cylinders 30A and 30B, the solid content of the raw material may settle during that time. In the illustrated example, since the following measures are taken, a stable supply is ensured. Filling of the cylinders 30A and 30B with the raw material is performed through the entire amount of the discharge from the circulation pump 20 (particularly, a high head is not required), so that the raw material does not stay in the cylinders 30A and 30B for a long time. By providing two systems of cylinders 30A and 30B and switching between them in a short period of time, the liquid flow in the cylinders 30A and 30B is temporarily settled for a short time in the process of supplying the raw material to the reactor 3. Since the material does not settle for a long time, sedimentation of the solid content of the raw material is prevented. In the piping system through which the raw material flows, the flow is constantly maintained by the switching operation, or even when the flow stops, the liquid remains in the piping in a stationary state because it is purged by the pressurizing gas such as nitrogen. Never.

As a result, even if the supply amount of the raw material is extremely small as in a test apparatus or the like, the selection of the circulation pump 20 becomes easy, and the flow control valve 4 for controlling the flow rate of the raw material is not required. Even in the case of a liquid raw material containing a solid content, the solid content does not adhere to the valve port and does not impair the stability of the flow rate. The raw material can be stably supplied into the pressurized reactor 3 without the fear of being worn out by solids and making it difficult to use the raw material stably for a long time. By purging with a gas for pressurizing the path where the flow is formed and the flow must be stopped, the liquid raw material does not stay in each part of the pipe.

In this way, even if the supply amount of the liquid raw material stored under the atmospheric pressure is extremely small, it is possible to prevent the flow rate fluctuation and the wear of the valve body due to the deposit on the valve while preventing the valve raw material from being worn. A stable feed can be supplied into the pressurized reactor 3, the flow of the raw material can be constantly performed in one of the routes, and the flow in which the flow needs to be stopped is purged with a pressurizing gas, so that the liquid raw material can be supplied to each part of the pipe. Can be prevented from staying.

FIGS. 3 and 4 show another example of an apparatus for carrying out the pressurized liquid material supply method according to the present invention.
1 and 2 denote the same parts, and the basic configuration is the same as that shown in FIGS. 1 and 2. However, the features of the illustrated example are as follows. As shown in FIG. 3, the units including the cylinders 30A and 30B and the piping system surrounded by the imaginary line are designated as NO. 1 unit and the N
O. NO. 1 having exactly the same configuration as one unit. 2 units, the raw material tank 1 and the circulation pump 20 As shown in FIG. 4, NO.
Regarding the switching timing of the raw material supply in one unit of the A system and the B system, NO. The point is that the switching timing of the raw material supply in the two units A system and B system is shifted by 1/4 cycle.

The raw material supply capacity of each unit is about 約 of that in the example shown in FIG. 1, and the total is substantially equal to the raw material supply capacity in the example shown in FIG.

Note that the controller 76 sends the NO. A command or NO. Output to each valve of the two units. The illustration of the pressure in the cylinder input from the two unit pressure gauges to the control device 76 is omitted.

By doing so, the NO. 1 unit of A
At the time of switching the material supply between the system and the B system, the NO.
Raw material supply or raw material filling in two units of the A system or the B system is continuously performed. here,
In the case of the example shown in FIG. 1, the flow of the raw material stops momentarily during the switching operation of the four-way valve V3, so that the discharge flow rate of the circulation pump 20 and the supply amount to the reactor 3 fluctuate. Although it may affect the operation of the reactor 3,
As shown in FIGS. 3 and 4, while one unit is performing the switching operation, the other unit continues to supply the raw material or feed the raw material into the cylinder at a constant rate, thereby reducing the fluctuation of the raw material flow rate by about half. It becomes possible to reduce.

When it is necessary to further reduce the fluctuation of the flow rate of the raw material, it can be dealt with by appropriately increasing the number of units.

FIGS. 5 and 6 show still another example of the apparatus for carrying out the method of pressurizing and supplying a liquid raw material according to the present invention. In the figure, portions denoted by the same reference numerals as those in FIGS. 1 and 2 are shown. Represent the same thing, and the basic configuration is the same as that shown in FIG. 1 and FIG. 2, but the feature of this illustrated example is that FIG.
As shown in the figure, a unit including the cylinders 30A and 30B surrounded by phantom lines and a piping system (however, the purge gas system 56 including the four-way valve V4, the shutoff valve V5, and the shutoff valve V6 in the example of FIG. 1, and the restriction orifice 54) Including circulation line 52
And the in-cylinder purging material return line 53 including the shut-off valve V7 and the restriction orifice 55 are eliminated, and the press-fit line 4 between the four-way valve V3 and the mass flow meter 50 is replaced.
9, a shutoff valve V8 and a three-way valve V9 are provided
No. 9 is connected to a raw material return line 78 for in-cylinder purging which is connected to the raw material tank 1 and is provided with a restricting orifice 77 in the middle thereof. No. 1 unit. N having exactly the same configuration as one unit
O. Two units are juxtaposed, and in the case of the above-described example (see FIGS.
As shown in FIG. 6, the material supply process, which was a cycle, was shortened to 1/4 cycle. In the case of the above-described example (see FIGS. 1 to 4), each of the A and B systems had a 1/4 cycle. 1/2 of the process of loading the raw material, which was a cycle
NO. Material supply in one unit A system, NO. Material supply in B unit of 2 units, NO. Raw material supply in one unit B system,
NO. The raw material supply in the two units of the system A is sequentially repeated, so that the raw material is continuously supplied into the reactor 3.

It is to be noted that the control device 76 issues a NO. A command or NO. Output to each valve of the two units. The illustration of the pressure in the cylinder input from the two unit pressure gauges to the control device 76 is omitted.

In the case of the example shown in FIGS. At the time of loading raw material in one unit A system, shut-off valve V
In the state where 2A is opened and the four-way valve V3 is switched from the position a to the position b, the raw material circulates at a relatively low pressure in the order of the raw material tank 1, the four-way valve V3, the cylinder 30A, the shutoff valve V2A, and the raw material tank 1. Then, the cylinder 30A is filled with the raw material, and at the time of the raw material return line purge, the four-way valve V3 is switched to the position of b → d, a → c and the shutoff valve V8 is closed, and the flow of the raw material is changed to the raw material tank 1 → The system is switched to the four-way valve V3 → the cylinder 30B → the shutoff valve V2B → the system of the raw material tank 1 (the system in which the raw material is inserted into the B system), and the supply of the raw material to the cylinder 30A is stopped. The pressurizing gas supplied to the cylinder 30A is discharged to the raw material tank 1 through the shut-off valve V2A opened from the cylinder 30A, and when the cylinder is pressurized. The shut-off valve V2A is closed, by confining the pressurizing gas in the cylinder 30A,
The inside of the cylinder 30A is pressurized at a speed corresponding to the supply amount of the pressurizing gas from the flow control valve V1A, and at the time of supplying the raw material, the shut-off valve V8 is opened with the four-way valve V3 switched from the position b to d. Further, the three-way valve V9 is switched from the position a to the b, and the raw material is pushed out from the cylinder 30A to the reactor 3 in accordance with the flow rate of the pressurizing gas supplied from the flow control valve V1A. Is switched from a to c position and cylinder 3
The line from 0A to the reactor 3 is shut off, and a line for discharging the raw material to the raw material tank 1 is formed.
The raw material remaining in A is transferred from the flow control valve V1A to the cylinder 3
With the pressurizing gas constantly supplied to 0A, all the gas is pushed out to the raw material tank 1 through the in-cylinder purging raw material return line 78, and the inside of the cylinder 30A is temporarily emptied. Is performed, and the above operation is repeated.

In the case of NO. When the raw material is inserted in the B system of one unit, in a state where the shut-off valve V2B is opened and the four-way valve V3 is switched from the position a to the position c, the raw material tank 1 → the four-way valve V3 → the cylinder 30B → the shut-off valve V2
The raw material circulates at a relatively low pressure in the order of B → raw material tank 1 to fill the cylinder 30B with the raw material, and at the time of the raw material return line purge, the four-way valve V3 is switched to the positions of c → d, a → b, and The shutoff valve V8 is closed, and the flow of the raw material is changed from the raw material tank 1 to the four-way valve V3 to the cylinder 30A.
The system is switched from the shutoff valve V2A to the system of the raw material tank 1 (a system in which the raw material is inserted into the A system), and the supply of the raw material to the cylinder 30B is stopped. Pressurized gas is supplied to the shut-off valve V2B opened from the cylinder 30B.
Is released to the raw material tank 1 and when the cylinder is pressurized, the shut-off valve V2B is closed and the pressurizing gas is
0B, the inside of the cylinder 30B is pressurized at a speed corresponding to the supply amount of the pressurizing gas from the flow control valve V1B, and the four-way valve V3 is switched from the position c to the position d during the supply of the raw material. The shut-off valve V8 is opened and the three-way valve V9 is switched from the position a to the position b,
According to the flow rate of the gas for pressurization supplied from the flow control valve V1B, the raw material is extruded from the cylinder 30B to the reactor 3,
At the time of purging in the cylinder, the three-way valve V9 is switched from the position a to the position c, the flow path from the cylinder 30B to the reactor 3 is cut off, and a line for discharging the raw material to the raw material tank 1 is formed. The raw material left in
By the pressurizing gas constantly supplied from the flow control valve V1B to the cylinder 30B, all the gas is pushed out to the raw material tank 1 via the raw material return line 78 for purging in the cylinder, and the inside of the cylinder 30B is temporarily emptied, Thereafter, the raw material is laid again, and the above operation is repeated.

NO. The same operation as described above is repeated for the two-unit A and B systems.
O. Material supply in one unit A system, NO. Material supply in B unit of 2 units, NO. Material supply in one unit B system, NO. The raw material supply in the two units of the A system is sequentially repeated, and the raw material is continuously supplied into the reactor 3. In the example shown in FIGS. 5 and 6, when the material return line purge, cylinder pressure increase, or in-cylinder purge is performed in one system, the material is stuck in one of the other systems, and the circulation is performed. Pump 20
The flow of the raw material by the raw material tank 1
Since there is no circulation line 52 in the example of FIG. 1, there is no problem.

When the sedimentation of the solid content of the liquid material is extremely large, sedimentation in the process of supplying the raw material, in which the flow of the raw material in the cylinder is the slowest, becomes a problem. By doing so, the process of supplying the raw material per cylinder can be reduced to half of the case of the above-described example (see FIGS. 1 to 4), and the effect of suppressing the sedimentation of the solid content in the raw material can be reduced. Be expected. NO. 1 unit and N
O. By switching the two units of the four-way valve V3 with slightly shifting each, the supply of the raw material can be performed without interruption.

FIG. 7 shows an example of an apparatus for carrying out the pressurizing gas flow control method in the liquid raw material pressurizing and supplying method according to the present invention. In the drawing, the same reference numerals as those in FIG. 1 denote the same parts. The basic configuration is the same as that shown in FIG. 1, but the feature of this illustrated example is that the pressure controller 42 and the flow controllers 47A and 47B shown in FIG.
And the pressure controller 61, and as shown in FIG.
A pressure 41 of the pressurizing gas detected by the pressure control valve 39,
The flow rates 46A and 46B of the pressurizing gas detected by the positive displacement flow meters 45A and 45B and the pressure 60 of the pressurizing gas detected by the pressure gauge 59 are input to the control device 76,
In the controller 76, the raw material flow rate as the mass flow rate is set to m
[Kg / h] and the specific gravity of the raw material is preset as ρ [kg / m ³ ], and the actual pressure 41 of the pressurizing gas detected by the pressure gauge 40 (P ₁ [MPa] (gauge pressure))
) And actual pressures 65A, 65B in the cylinders 30A, 30B detected by the pressure gauges 66A, 66B (respectively P ₂ [MPa] (gauge pressure)).
The pressurizing gas flow rate V [m ³ / h] as the volume flow rate corresponding to each cylinder 30A, 30B is respectively

V = m / ρ × (P ₂ + P ₀ ) / (P ₁ + P ₀ ) (where P ₀ is obtained from the atmospheric pressure (with respect to vacuum) expressed in the same pressure unit as P ₁ and P ₂ ) So that the actual pressurized gas flow rate detected by the positive displacement flow meters 45A and 45B is equal to the set pressurized gas flow rate V.
It is configured to output the opening degree commands 48A and 48B to the flow rate control valves V1A and 1B to perform control.

When the pressure in the reactor 3 is P ₃ ,

P ₁ > P ₂ > P ₃ and

P ₁ = P ₃ + α (where α = approximately 0.05 to 0.2 [MPa]).

In the example shown in FIG. 1, when the pressure of the reactor 3 to which the raw material is supplied is constant, the pressure gas system 3
Since the setting of the pressure and flow rate of the pressurizing gas in Step 4 is constant, the movement of the pressure control valve 39 and the flow rate control valves V1A and 1B is small, and the operation of the pressurizing gas system 34 is stable. When starting and stopping are performed at short intervals as in a test apparatus or when the pressure of the reactor 3 changes frequently, when the pressure of the reactor 3 decreases, the pressurizing gas having the same flow rate is supplied to the cylinder 30A. , 30B, while the flow rate of the raw material supplied to the reactor 3 increases, when the pressure of the reactor 3 increases, the pressurizing gas having the same flow rate is supplied to the cylinders 30A, 3B.
Even if it is put in 0B, the flow rate of the raw material supplied to the reactor 3 decreases, and the raw material supply amount changes. Therefore, it is necessary for an operator to change the setting according to the change, and the operation may be complicated. There is.

However, according to the example shown in FIG. 7, the raw material pressurized in the cylinders 30A and 30B is supplied at a volume flow rate corresponding to the flow rate of the pressurizing gas.
When extruding from B into the reactor 3, the raw material flow rate as mass flow rate is set to m and the raw material specific gravity is set to ρ, and the actual pressurizing gas pressure P ₁ and each cylinder pressure P ₂ are Are detected, and the atmospheric pressure with respect to the vacuum is P ₁ , P ₂
Is set to P _{0 in the} same pressure unit as that of each cylinder 30A, 30
The pressurizing gas flow rate V as the volume flow rate corresponding to B is

V = m / ρ × (P ₂ + P ₀ ) / (P ₁ + P ₀ ), which is set and the actual pressurizing gas flow rate corresponding to each cylinder 30A, 30B is set. The pressure is controlled to be equal to the pressure gas flow rate V. Thus, even if the pressure of the reactor 3 to which the raw material is supplied changes, the raw material supply amount is kept constant without changing, and the operator It is not necessary to change the setting of the pressurizing gas flow rate V in accordance with the pressure change, and the operation is not complicated.

However, in the case where the parameter of the reactor 3 which is an external factor as viewed from the apparatus of the present example, which affects the operation of the apparatus of the present example, there is a possibility that the stability of control may be impaired. It is desirable that the setting of the pressurizing gas flow rate V can be easily switched between automatic and manual in the controller 76.

As described above, in the control device 76,
The pressurizing gas flow rate V as a volume flow rate corresponding to each of the cylinders 30A and 30B is automatically set, and the actual pressurizing gas flow rate detected by the positive displacement flow meters 45A and 45B is set. So that
It is needless to say that the configuration in which the opening degree commands 48A and 48B are output to the flow rate control valves V1A and 1B and control is performed can be applied to the examples shown in FIGS.

Thus, in the case of the example shown in FIG. 7, as in the case of the above-described example, the liquid raw material stored under the atmospheric pressure can be used even when the raw material supply amount is extremely small.
It is necessary to stably supply the raw material into the pressurized reactor 3 while preventing the flow rate fluctuation and the abrasion of the valve body due to the deposits on the valve, and it is necessary to allow the flow of the raw material at any time and to stop the flow. By purging the passage with a gas for pressurization, the liquid raw material can be prevented from staying in each part of the pipe, and the followability to the pressure change of the reactor 3 can be improved.

The method of controlling the gas flow rate for pressurization in the method for pressurizing and supplying a liquid raw material of the present invention is not limited to the above-described example, but is applicable not only to the reactor but also to various pressurized devices. Needless to say, various changes can be made without departing from the spirit of the present invention.

[0064]

As described above, according to the pressurizing gas flow control method in the liquid raw material pressurizing supply method of the present invention, the liquid raw material stored under the atmospheric pressure can be supplied with an extremely small amount of raw material. Even in such a case, it is possible to stably supply the raw material to a pressurized reactor or the like while preventing the flow rate fluctuation and the abrasion of the valve body due to the deposits on the valve, and always feed the raw material through any route. By purging with a gas for pressurizing the path where the flow is possible and the flow needs to be stopped, it is possible to prevent the liquid raw material from remaining in each part of the piping, and to further improve the followability to the pressure change of the equipment. An excellent effect that can be achieved can be achieved.

[Brief description of the drawings]

FIG. 1 is an overall schematic configuration diagram of an example of an apparatus for performing a liquid raw material pressurizing supply method which is a base of the present invention.

FIG. 2 is a sequence diagram showing each process during operation in the example shown in FIG. 1 and the opening / closing or position of each valve.

FIG. 3 is an overall schematic configuration view of another example of an apparatus for performing a liquid raw material pressurizing supply method which is a base of the present invention.

FIG. 4 is a schematic sequence diagram showing each process during operation in the example shown in FIG.

FIG. 5 is an overall schematic configuration diagram of still another example of an apparatus for performing a liquid raw material pressurizing supply method which is a base of the present invention.

FIG. 6 is a sequence diagram showing each process at the time of operation in the example shown in FIG. 5, and the opening / closing or position of each valve.

FIG. 7 is an overall schematic configuration diagram of an example of an apparatus for performing a pressurizing gas flow rate control method in the liquid raw material pressurizing supply method of the present invention.

FIG. 8 is an overall schematic configuration diagram of a conventional example.

[Explanation of symbols]

 Reference Signs List 1 raw material tank 3 reactor (equipment) 20 circulation pump 30A cylinder 30B cylinder 31 filling line 32 filling line 33A filling / press-fitting line 33B filling / press-in line 34 pressurizing gas system 35 raw material return line 49 press-in line 76 control device V1A flow rate control Valve V1B Flow control valve V2A Shut-off valve V2B Shut-off valve V3 Four-way valve V4 Four-way valve V5 Shut-off valve V6 Shut-off valve V7 Shut-off valve V8 Shut-off valve V9 Three-way valve

Claims (1)

[Claims] 1. A raw material filling method in which a liquid raw material stored in a raw material tank under atmospheric pressure is circulated from a cylinder to a raw material tank via a raw material return line while filling the cylinder, and after the raw material is filled in the cylinder. The pressurizing gas is guided to the raw material tank through the raw material return line, and the raw material return line is purged to push out the raw material filled in the raw material return line to the raw material tank. When the pressure in the cylinder rises to approximately the same pressure as the pressure in the equipment, the cylinder and the equipment are brought into communication with each other, and the gas for pressurization is further supplied into the cylinder. Feeding the pressurized raw material from the cylinder to the equipment at a volume flow rate commensurate with the gas flow rate for pressurization, and after completing the raw material supply from the cylinder to the equipment, By repeatedly repeating in-cylinder purging of the raw material remaining in the cylinder to the raw material tank with a pressurizing gas in a plurality of cylinders, the liquid raw material is continuously pressed into the pressurized equipment. a pressurizing gas flow rate control method in the pressure supply method, the material flow as the mass flow rate and m and the material density is preset as [rho, the actual pressurization gas pressure P ₁ and the cylinder pressure P ₂ and the detection And the pressure of the atmosphere on the vacuum is P ₁ ,
Let P _{0 be the} same pressure unit as P _2, and the pressurizing gas flow rate V as the volume flow rate corresponding to each cylinder is given by: V = m / ρ × (P ₂ + P ₀ ) / (P ₁ + P ₀ ) Pressurizing gas flow rate control in a liquid raw material pressurizing and supplying method, wherein the pressurizing gas flow rate is set so as to obtain an actual pressurizing gas flow rate corresponding to each cylinder so as to be equal to the set pressurizing gas flow rate V. Method.